BY-NC-ND 3.0 license Open Access Published by De Gruyter May 26, 2017

Analytical methods for the determination of some selected 4-quinolone antibacterials

Fathallah Belal, Nahed El-Enany and Mary E.K. Wahba

Abstract

A comprehensive review with 337 references for the analysis of some selected 4-quinolone drugs belonging to the first and second generations since 2006 up till now is presented. This group includes nalidixic acid, oxolinic acid, piromidic acid, pipemidic acid and rosoxacin from the first generation and enoxacin, fleroxacin, nadifloxacin, pefloxacin and rufloxacin from the second generation. The review covers most of the methods described for the analysis of these drugs, either per se, in dosage forms, biological fluids, environmental samples, cosmetics, animal tissues and feed-premix samples.

Introduction

4-Quinolones comprise a large and expanding group of synthetic antibacterial agents. The first drug of this class, nalidixic acid (NDA) was discovered in 1962 and was a modification of a compound isolated during the production of the antimalarial drug, chloroquine (Lesher et al. 1962), and was later approved for clinical use in 1965. However, its antibacterial spectrum of activity was restricted to the Enterobacteriaceae, and due to the limited absorption and distribution of the drug, it was effective solely for the treatment of urinary tract infections. A major advance occurred during the 1980s with the discovery that a fluorine atom at 6-position of the basic quinolone nucleus and a piperazine substitution at the 7-position were found to enhance the quinolone antibacterial activity and to increase the extent of oral absorption and distribution (Ball 2000).

Drugs possessing this fluorine atom are known as the fluoroquinolones (FQs). The first FQ approved for use in clinical medicine was norfloxacin, followed shortly thereafter by ciprofloxacin in the mid-1980s. Poor oral bioavailability and tissue distribution with limited spectrum of activity were associated with the first generation drugs (Sweetman 2009).

Structural changes in the second generation FQs increased their oral bioavailability and systemic distribution, and broadened their spectrum of activity (Lesher et al. 1962). The favorable characteristics of the second generation drugs were maintained by the third generation FQs while exhibiting increased activity against Gram-positive bacteria, anaerobes and mycobacteria. Moreover, these compounds also exhibited excellent oral bioavailability and were associated with a prolonged terminal elimination half-life (Ball 2000). Lower central nervous system toxicities are another advantage of this group. Pharmacological actions and pharmacokinetics of FQs have been reviewed by many researchers (Schentag 2000, Martinez et al. 2006).

Physicochemical properties of FQs

The amphoteric property of FQs is a result of the modification in the quinolone core structure by inserting a fluorine atom at position C-6 and a piperazinyl or piperazine derivative group (R) at C-7.

Such chemical structure enhances their water solubility and provides them with a strong capability to form stable 1:1 complexes with several cations (e.g. magnesium, calcium, aluminum, iron and zinc) (Turiel et al. 2006, Sukul and Spiteller 2007). Although FQs show resistance to hydrolysis and heat, they seem to be highly photosensitive. Irradiation with UV radiation in water leads to de-fluorination and/or oxidative degradation of the amine side chain (Freccero et al. 2008, Sturini et al. 2010a).

Literature survey of FQs

Many reviews were published in the literature dealing with the pharmacology of FQs (Schentag 2000, Martinez et al. 2006). The determination of FQs in solid environmental matrices (Speltini et al. 2011) was also reported. Recent analytical techniques (Samanidou et al. 2005a,b) used for the determination of FQs in pharmaceuticals and samples of biological origin were also reviewed. A review concerned with analytical methods for the determination of the third and fourth generation FQs in biological matrices and pharmaceutical formulations by liquid chromatography was recently reported (Sousa et al. 2012); therefore, the authors in this work were concerned with earlier generations. Another review on the separation methods for the determination of some FQs was published (Saleh et al. 2013). Moreover, the spectrophotometric methods for the determination of FQs were also reviewed (Kaura et al. 2008).

Although many recent reviews covered the analytical methods for the determination of FQs, many drugs of the first and second generations were not reviewed since 2005, namely, NDA, oxolinic acid (OXA), piromidic acid, pipemidic acid (PIA) and rosoxacin (ROX) from the first generation and enoxacin (ENX), fleroxacin (FRX), nadifloxacin (NFX), pefloxacin (PFX) and rufloxacin (RFX) from the second generation, since 2006 up till now. The structural formulae of the selected drugs are listed in Table 1.

Table 1:

Chemical structure of the selected 4-quinolones.

NameStructural formulaAbbreviation
Nalidixic acid
NDA
Oxolinic acid
OXA
Piromidic acid
PMA
Pipemidic acid
PIA
Rosoxacin
ROX
Enoxacin
ENX
Fleroxacin
FRX
Nadifloxacin
NFX
Pefloxacin
PFX
Rufloxacin
RFX

Official and compendial methods of analysis

NDA is the subject of monographs in both the British Pharmacopoeia (2009) and the United States Pharmacopoeia (2007). Spectrophotometric measurement of its alkaline solution at 334 nm is described in BP, while the USP used non-aqueous titration with lithium methoxide as a titrant for its assay in pure form, and high performance liquid chromatography (HPLC) with UV detection at 254 nm for its quantitation in tablets and oral suspensions.

OXA, PIA and PFX are official drugs in the BP (The British Pharmacopoeia 2009), which recommends a non-aqueous potentiometric titration method using tetrabutyl ammonium hydroxide or perchloric acid as titrant for PIA and PFX for their determination.

Reported methods of analysis

Spectroscopic methods

UV-VIS spectrophotometry

Estimation of NDA in pharmaceutical formulations by UV spectrometry (Maheshwari et al. 2006), and the study of its complexation equilibria with proton and metal ions in aqueous organic mixtures, was carried out (Gandhi and Sekhon 2007). A eutectic liquid obtained by triturating phenol crystals and metformin hydrochloride in a 4:1 ratio on weight basis was employed to extract NDA from fine powder of tablets. Distilled water was used for dilution purpose to carry out spectrophotometric estimation at 330 nm without utilizing any organic solvent (Maheshwari et al. 2015).

The interaction of cobalt (II) with OXA in the absence or presence of the Lewis bases 2,2′-bipyridine, 2,2′-bipyridylamine, 1,10-phenanthroline, pyridine or 4-benzylpyridine resulted in the formation of a series of mononuclear complexes which were characterized with physicochemical and spectroscopic techniques (Irgi et al. 2015). The hydrophilic ionic liquids and potassium hydrogen phosphate formation of an aqueous two-phase system for the determination of OXA was investigated (Yan et al. 2009).

Regarding ROX, a selective spectrophotometric method for its determination was carried out based on the reaction with alkaline sodium nitroprusside forming a red chromogen measured at 455 nm (Askal et al. 2008). Another report described the formation of yellow-colored water-soluble ion-pair complexes with 2% (w/v) β-naphthol in sulfuric acid at room temperature (Darwish et al. 2006).

A spectrophotometric titration method in a wide range of pH was utilized for the estimation of complex-formation equilibrium between ENX and Al(III), Fe(III), Cu(II) and Zn(II) ions (Urbaniak and Kokot 2013). Another method has been established for the assay of ENX using sodium 1,2-naphthoquinone-4-sulfonate as a derivatizing chromogenic reagent (Wu et al. 2010). ENX was also assayed based on an association complex formation with Al (III) and erythrosine (Yamaguchi et al. 2009). Moreover, ENX and ciprofloxacin were determined simultaneously using a simulated system based on a partial least-squares method (Ajuan 2008). On the other hand, the determination of ENX and PFX based on charge transfer reaction with alizarin red in ethanol-water medium or phosphate buffer was also postulated (Li and Zhang 2008, Zhang and Lin 2009).

Regarding the analysis of FRX, one report concerned with the determination of its content in powder for injection with chrome azurol was described (Quan et al. 2009).

A multi-wavelength method for simultaneous estimation of NFX and ibuprofen in formulated hydro-gel preparations was presented (Kalantre and Pishwikar 2012). Another report suggested three UV methods for the estimation of NFX in pharmaceutical dosage forms by measuring its absorbance at 296.5 nm (method A), or measure its first-order derivative spectra at 278 nm (method B), or measuring the area under curve in the wavelength range (method C) (Kulkarni et al. 2010).

A simple zero-order UV spectrophotometric method for the estimation of PFX in bulk and tablet formulation was developed. Single point standardization was used for quantitative estimation of the drug and absorbance was determined at 288 nm using methanol as a solvent system (Raghunath et al. 2015). Based on the charge transfer reaction between PFX and chloranilic acid in methanol, a spectrophotometric method was established for the determination of PFX in pharmaceuticals (Pang et al. 2013). PFX was also quantified based on oxidation with cerium (IV) in the presence of perchloric acid and subsequent measurement of the excess Ce (IV) by its reaction with p-dimethylaminobenzaldehyde to give a colored product measured at 470 nm (Adegoke et al. 2010). PFX was estimated in pharmaceutical bulk and tablet dosage forms using UV detection at 277.5 nm in a 100 mm HCl medium (Misra et al. 2008). It was also determined in pharmaceutical formulations using three different salts of iron. These methods are based on the formation of complexes with ferric nitrate, ferric chloride or iron ammonium citrate in which the carboxylic group of PFX undergoes complexion with iron (Siddiqui et al. 2010).

The simultaneous determination of PFX and its structurally similar metabolite, norfloxacin, was described based on the monitoring of a kinetic spectrophotometric reaction of the two analytes with potassium permanganate as an oxidant, and measurement of the reaction process following the absorbance decrease of potassium permanganate at 526 nm (Ni et al. 2008).

Analytical studies were carried out to evaluate the use of N-bromosuccinimide (NBS) as an analytical reagent for the spectrophotometric assay of PFX. The procedures involved the reaction of the studied drug with NBS and subsequent measurement of the excess NBS by its reaction with phenylenediamine to give a violet-colored product that was measured spectrophotometrically at 530 nm (Askal et al. 2007). Another spectrophotometric method was described for the assay of PFX in bulk drug and in tablets. The described method was based on ion-pair formation with bromophenol blue dye at pH 5.2 followed by extraction and measurement of the dye absorbance at 590 nm (Basavaiah et al. 2007). Finally, the influence of Al3+ on the absorption characteristics of PFX had been studied where the absorbance of the Al3+-PFX complex was measured at 275 nm (Zhang et al. 2006b).

Spectrofluorimetric methods

Several spectrofluorimetric methods for the determination of FQs were recorded. The use of lanthanide ions in some of such methods was mentioned in the literature for the assay of OXA, NDA, PIA, ENX and PFX; this could be summarized as follows.

The influence of the nature of micellar surfactant solutions on the sensitized fluorescence of mixed ligand chelates Tb3+-1,10-phenanthroline-OXA and Tb3+-1,10-phenanthroline-NDA was studied (Smirnova and Nevryueva 2010). On the other hand, a time-resolved fluorescence analytical method was developed using a Eu3+ ion as a fluorescent probe for the quantitation of PIA (Liu et al. 2008b), where intra-molecular energy transfer occurs in the europium complex with PIA and the characteristics fluorescence of the Eu3+ ion with the maximum λem of 616 nm after excitation at λ 274 nm. Another study of the influence of silver nanoparticles on the second-order scattering and the fluorescence of the complexes of Tb3+ with PIA was reported in the literature (Ding et al. 2006).

The fluorescence system of ENX-Tb3+-sodium dodecyl benzene sulfonate (SDBS) was investigated (Tong and Xiang 2007). The results indicated that the fluorescence intensity of Tb3+-SDBS was greatly enhanced by ENX. Studies of the complex between PFX and Tb3+ (Li and Song 2014), and the fluorescent characteristics and content determination of PFX in yttrium-PFX, were performed (Ping et al. 2010). On the other hand, Tb3+ was found to react with PFX to form a 1:2 coordination complex with the characteristics fluorescence of Tb3+ in a neutral medium (Liao et al. 2008a). In another study, a ternary coordination complex was formed among Eu3+, PFX and EDTA due to the intra-molecular energy transfer of the coordination complex (Bian and Xu 2007).

Metal complexation was also utilized for the spectrofluorimetric determination of FQs. The interactions between ENX and heavy metal ions were studied using fluorescence spectroscopy at different temperatures (Han et al. 2012). It was shown that the fluorescence intensity of ENX could be apparently quenched by Cu2+, Pb2+ and Mn2+ due to static quenching. On the other hand, in a hexamine-HCl buffer of pH 5.8, the synergistic sensitization effect of sodium dodecyl sulfate and Al3+ on the fluorescence of ENX was observed (Ma et al. 2011). In another report based on the evident increase in the relative fluorescence intensity of FRX by complexing with Al3+, a new method of synchronous fluorescence spectrometry to rapidly determine FRX was developed (Cai et al. 2012). It was also shown that FRX and Zn2+ have a powerful ability to quench the bovine serum albumin fluorescence via a non-radiative energy transfer mechanism (Wu et al. 2007).

Derivatization was also applied to assay some FQs. ENX, for instance, was determined based on derivatization with 4-chloro-7-nitrobenzofurazan in borate buffer of pH 9 to yield a yellow product (Ulu 2009). Meanwhile, ENX and PFX were assayed in their pharmaceutical dosage forms or in biological fluids through charge transfer complex formation with bromanil (Salem et al. 2007) and fluoranil (Geffken and Salem 2006). Another fluorescence spectrometric method for the determination of PFX was established based on the charge transfer reaction with 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (Xu et al. 2007).

Micellar-enhanced fluorimetry was also applied to determine FRX (Aodeng and Liu 2006) and PFX (Bian et al. 2006), because it was found that sodium dodecyl sulfate could greatly enhance the fluorescence signal of the latter using Britten-Robinson buffer solution of pH 5.3.

Fluorescence quenching could also be used to analyze FRX, PFX and ENX. The interaction between FRX and pepsin was investigated (Lian et al. 2013). Static quenching was suggested and it was proved that the fluorescence quenching of pepsin by FRX was related to the formation of a new complex and a non-radiation energy transfer. Meanwhile, the quantitative determination of traces PFX and ENX was accomplished based on fluorescence quenching of either quantum dot silica-coated nanoparticles or glutathione-capped CdTe, respectively (Chen et al. 2012a, Yang et al. 2016). Another report studied the quenching effect of palladium (II) or sodium dodecyl benzene sulfonate for the fluorescence of PEX (Wang et al. 2014) in acidic and neutral media.

Other spectrofluorimetric methods concerned with the assay of FQs include non-linear variable angle synchronous spectrofluorimetry for the determination of ENX in urine (Murillo Pulgarin et al. 2012) and irradiation of ENX for a few minutes using a high-power UV lamp which drastically increased its fluorescence quantum yield (Espinosa-Mansilla et al. 2007). Use of octadecyl silica membranes for sample pre-concentration and solid substrate for ENX fluorescence line narrowing spectroscopy (Yu et al. 2006) where measurements at liquid helium temperature (4.2 K) were easily made using a cryogenic fiber optic probe. A catalytic-kinetic spectrofluorometric method was described for the determination of traces PFX (Liang et al. 2006b); it was based on the inhibitory effect of PFX on the reaction of H2O2 oxidation of rhodamine B catalyzed by Cu2+.

Mass spectrometric methods

The stability of various classes of antibiotics – especially NDA and OXA – was tested in matrix and reference solutions using a straightforward procedure applying mass spectrometric detection (Berendsen et al. 2011). Both drugs were also analyzed by laser diode thermal desorption chemical ionization with tandem mass spectrometry (Lohne et al. 2012). A quasi-MS/MS/MS method was applied to investigate the fragmentation mechanism of FRX, which was analyzed using electrospray mass spectrometry by collision-induced dissociation (Jiao et al. 2009a). The speciation in solutions containing Al3+ and FRX was studied by electrospray mass spectrometry (ESI-MS/MS) and laser desorption ionization (Cvijovic et al. 2012).

Resonance Rayleigh scattering method

A new resonance Rayleigh scattering method for the determination of FRX has been developed (Wang et al. 2010). FRX reacts with Co2+ to form chelated cations in Britton-Robinson buffer over the pH range of 4.2–6.8, which further binds with Congo red to form the ion-association complexes, resulting in great enhancement of resonance Rayleigh scattering intensity. The maximum scattering wavelengths are located at 372 and 560 nm. A similar approach for the assay of PFX in tablets, human urine and plasma was also established (Han et al. 2011) where three scattering peaks at 278, 380 and 560 nm appeared. On the other hand, upon using a Britton-Robinson buffer medium, PIA was protonated and reacted with methyl orange to form an ion-pair complex, which then further formed a six-membered ring chelate with Pd (II). As a result, new resonance Rayleigh scattering spectra appeared. The method was applied for the determination of the drug in pharmaceutical formulations and human urine samples (Qiao et al. 2015).

Infrared spectroscopy

Near-IR spectroscopy has been applied to analyze injection samples of PFX. Partial least-squares regression analysis and principal components regression have been utilized to establish the developed method (Xie et al. 2010).

NMR spectroscopy

Non-selective and selective spin-lattice relaxation rates and spin-spin relaxation measurements were used to investigate and characterize interaction processes between FRX and bacterial cells (Waibel and Holzgrabe 2007). The signals of three hydrogens at different moieties of the FRX were considered to get an insight into the complexation behavior.

Chemiluminescence

Dysprosium-sensitized chemiluminescence (CL) reactions have been suggested for the determination of ENX, FRX, PFX and PIA (Sun et al. 2011a). The CL spectra are formed from the narrow characteristic emission of trivalent dysprosium (Dy3+) at 482 and 578 nm through the intermolecular energy transfer from the excited SO to analyte, followed by intra-molecular energy transfer from analyte* to Dy3+. With the FQs including ENX, FRX and RFX, the luminescence and CL properties of Tb3+-FQ and Eu3+-FQ complexes were studied in this contribution (Sun et al. 2011b). An Ag (III) complex CL system was applied for the assay of ENX. The method was applied for the determination of the drug in pharmaceutical preparations, spiked serum and urine samples (Chen and Sun 2010). Another batch-type CL analysis of ENX in pharmaceuticals was described (Karim et al. 2006). On the other hand, the CL determination of PFX was established (Wang et al. 2009a), where the addition of the drug to the Ce4+-Na2SO3-H2SO4 redox system could improve the CL phenomenon. In another report, the nitrogen atom in PFX was easily protonated in acidic medium and formed ion complexes with AuCl4−, the ion-complexes were extracted using dichloromethane, when the ion-complexes entered a reversed micellar system of cetyl trimethyl ammonium chloride containing luminol, and the dissociated AuCl4- reacted with luminol and produced a CL signal (Shi 2008).

Electrochemiluminescence

An electrochemiluminescence (ECL) based on energy transfer from electro-generated triplet sulfur dioxide to PIA was studied (Liang et al. 2006a). A weak ECL from triplet sulfur dioxide was observed when sulfite was electrochemically oxidized in sulfuric acid on a platinum electrode. When PIA was present, the weak ECL was enhanced.

The ECL of the Tb3+-ENX-Na2SO3 system in an aqueous solution was reported (Chen et al. 2006). ECL is generated by the oxidation of Na2SO3, which is enhanced by the Tb3+-ENX complex. The ECL intensity peak versus potential corresponds to oxidation of Na2SO3, and the ECL emission spectra match the characteristic emission spectrum of Tb3+, indicating that the emission is from the excited state of Tb3+.

Flow injection analysis (FIA)

A method for the analysis of ENX by flow injection coupled with CL detection was described, based on the ENX-enhancing effect on a weak CL system of luminol-H2O2 in alkaline solution (Du et al. 2012). FIA was also investigated for the assay of ENX using the luminol-H2O2 system in the presence of Cu2+. It was observed that the interaction of ENX with Cu2+ caused the sensitization of the CL intensity of the system strongly (Alam et al. 2011). On the other hand, the Dy3+-sensitized CL method was developed for the analysis of ENX using flow injection sampling based on the CL associated with the reaction of the Dy3+-Ce4+-S2O32−-ENX system and the Dy3+-MnO4-S2O32−-ENX system (Sun et al. 2009b). It was also found that the CL reaction between luminol and potassium ferricyanide was significantly sensitized by ENX (Li et al. 2008d). Another FIA method for the determination of ENX was developed based on the inhibiting behavior of ENX on the emission intensity of the CL reaction of luminol-H2O2-manganese tetrasulfonatophthalocyanine in a basic medium (Li and Wei 2006).

A new CL reaction system was established for the analysis of FRX. The Dy3+-sensitized CL emission mechanism was investigated by comparing the fluorescence emission with CL spectra (Sun and Li 2011). The CL spectra of the FRX-KMnO4-Na2S2O3-H6P4O13 system are from the narrow characteristic emission of Dy3+ at 482 and 578 nm through the energy transfer from the excited SO2* to analyte, followed by intra-molecular energy transfer from analyte* to Dy3+. Another report based on the enhancement of CL of the luminol-hydrogen peroxide-gold nanoparticles system by FRX was reported for its assay (Wang et al. 2007a).

An FIA method to determine PFX residue in urine and serum was established based on the fact that the presence of Tb3+ enhances the luminous intensity of the Ce4+-SO32--PFX system (Ren and Li 2012).

Voltammetric methods

Stripping continuous cyclic voltammetry was presented to determine NDA (Norouzi et al. 2008). The potential waveform was applied to a golden disk microelectrode in a continuous way. It was concluded that the best performance was achieved with the basic parameters set at pH 2, sweep rate of 60 V/s, accumulation potential 100 mV and accumulation time 0.7 s. A square wave adsorptive stripping voltammetric method has also been developed for the individual and simultaneous determination of NDA acid and its main metabolite, 7-hydroximethylnalidixic acid (Cabanillas et al. 2007). Variables that affect accumulation process, such as concentration of perchloric acid, accumulation potential and accumulation time, have been optimized by using an experimental design.

A micro-fluid-enzyme sensor for the quantification of PIA was proposed (Bertolino et al. 2011). PIA has a potential to inhibit topoisomerase II (DNA gyrase) of bacteria. PIA detection in pharmaceutical samples was based on the use of tyrosinase enzyme that was immobilized on 3-aminopropyl-modified-controlled-pore glass packet in a central channel of the microfluidic-enzymic device.

Another sensitive cathodic stripping voltammetric method has been developed for PIA using the hanging mercury drop electrode as a working electrode versus Ag/AgCl reference electrode (Solangi et al. 2009a). We used 0.1 m hydrochloric acid as medium and 0.1 m potassium chloride as base electrolyte.

An electrochemical sensor based on carbon paste and inclusion of ionic liquid crystal (1-butyl-1-methylpiperidinium hexafluorophosphate) in the presence of sodium dodecyl sulfate for the determination of ENX was prepared (Atta et al. 2015). Different ionic liquids were used and compared. The simultaneous determination of binary mixtures of ENX with either dopamine or epinephrine was demonstrated with good peak potential separations; furthermore, the method was applied for the direct determination of ENX in human urine samples. In another report, a polythionine-modified carbon paste electrode was prepared, and the electrochemical behavior of ENX at this modified electrode was studied by cyclic voltammetry (Gu et al. 2013). Besides, a mercury-free electrochemical method for the assay of ENX was established by using a glassy carbon electrode modified by multi-wall carbon nanotubes functionalized with carboxylic groups (Sun and Xing 2007), where differential voltammograms of ENX were obtained in 0.1 m phosphate buffer of pH 5.91 at 100 mV/s. Another rapid anodic adsorptive voltammetric method was developed for the analysis of trace amounts of ENX at a carbon paste electrode where it was adsorbed on the surface of the electrode in 0.4 mol/l acetate buffer solution (pH 4.5) yielding one oxidation peak at 1.17 V (Yi et al. 2007a).

Concerning FRX, its electrochemical behavior at the glassy carbon electrode was studied by linear scanning voltammetry and cyclic voltammetry (Yu et al. 2012b). In 0.1 m phosphate buffer solution of pH 6.5 containing Cu2+ ions, two reduction peaks given by Cu2+ ion were observed at −0.136 and −0.728 V, and their peak current decreased with the addition of FRX while keeping their reduction peak potentials unchanged.

The anodic behavior and analysis of PFX on boron-doped diamond and glassy carbon electrodes were investigated using cyclic, linear sweep, differential pulse and square wave voltammetric techniques (Uslu et al. 2008). In cyclic voltammetry, PFX shows one main irreversible oxidation peak and additional one irreversible ill-defined wave depending on pH values for both electrodes. The results indicated that the oxidation of PFX is irreversible and diffusion controlled on the boron-doped diamond electrode and irreversible but adsorption controlled on the glassy carbon electrode. Another highly selective and rapid new anodic adsorptive voltammetric method has been developed for the determination of trace amounts of PFX by using a carbon paste electrode (Yi et al. 2006). PFX was adsorbed on the surface of the electrode yielding an oxidation peak at 1.03 V using an acetate buffer solution 0.40 m of pH 4.9.

Microbiological assay

Several microbiological assay methods were reported for the determination of FQs of our interest; such methods include fluoroimmunoassay (Mi et al. 2013, Zhang et al. 2013) and enzyme-linked immunosorbent assays (Huet et al. 2006, Iwasaki et al. 2006, Lu et al. 2006, Wang et al. 2006, 2007b, Adrian et al. 2008, Burkin 2008, Li et al. 2008a, Scortichini et al. 2009, Chang et al. 2011, Jiang et al. 2011, 2013, Sheng et al. 2011, Fan et al. 2012, Wen et al. 2012, Tao et al. 2013, Tian et al. 2013, Zhao et al. 2013).

Separation techniques

Capillary electrophoresis (CE)

The literature survey revealed several CE methods for the assay of FQs; such methods could be summarized as follows.

The applicability of capillary zone electrophoresis for the separation of ENX with five other quinolones in acidic background electrolyte was studied (Rusu et al. 2015b). Furthermore, the migration behavior and separation of 13 quinolone antibacterials including ENX were investigated by CE (Rusu et al. 2015a). It was proved that the electrophoretic mobility of ionized quinolones can be described with Offord’s equation, and the migration order depends on their charge-to-mass ratios. Meanwhile, molecularly imprinted polymers were evaluated as sorbent for the construction of an in-line solid phase extraction analyte concentrator in CE coupled with mass spectrometry for the determination of eight regulated veterinary quinolones in bovine milk samples (including ENX and OXA) (David et al. 2014). Different parameters affecting the analyte concentrator performance, such as sample pH, volume and composition of the elution plug and injection time, were studied. Single drop micro-extraction coupled with CE for the analysis of six FQs including ENX was developed. The method was eventually applied for the extraction and pre-concentration of FQs in human urine samples (Gao et al. 2011a). Another method for the simultaneous determination of ENX and ofloxacin was established using CE coupled with ECL detection based on the ECL enhancement of tri(2,2-bipyridyl)ruthenium(II) (Liu et al. 2010). A method for the simultaneous separation and detection of six 4-quinolones including ENX by capillary zone electrophoresis was developed. The most suitable running buffer was found to be 30 mm sodium borate-10 mm NaH2PO4 (pH 8.5), and the optimal applied voltage, temperature and UV detection wavelength were 18 kV, 25°C and 278 nm, respectively (Li et al. 2009b). Another CE method was developed for the simultaneous assay of tetracaine, proline and ENX in human urine with ECL detection. The effects of applied voltage signal, the potential of working electrode, pH value, the flow rate of carrier solution, concentration of Ru(bpy)32+ and the ECL intensity of the drugs were investigated in detail (Sun et al. 2010b). Another CE method was developed for the simultaneous determination of five quinolone antibacterials including ENX. At the detection wavelength of 268 nm, the electrophoresis parameters were optimized where the buffer was 15 mm sodium borate-15 mm potassium dihydrogen phosphate at pH 8.8, the applied voltage was 8 kV and the sampling time was 20 s (Tian et al. 2009). Meanwhile, a CE-potential gradient detection method was developed for the determination of ENX together with RFX and moxifloxacin. The FQs were baseline separated within 3.5 min with background electrolyte composed of 50 mm acetic acid and 6 mm potassium hydroxide at pH 3.7 (Fan et al. 2009). The influence of bovine serum albumin as an additive on the CE-potential gradient determination of five quinolones including ENX was described with 10 mg/l of bovine serum albumin present in the buffer of 30 mm Tris and 3 mm H3PO4 at pH 9 (Qin et al. 2009). Another CE coupled to a self-made conductometric detector was developed for the separation and detection of five quinolones including ENX in a buffer containing bovine serum albumin in 30 mm Tris, 3 mm phosphoric acid at pH 9 (Liu et al. 2008c). Another method for the effective assay of eight FQs including ENX in human urine was reported. The method applied a voltage of 22 kV, using a mixture of 4×10−2m Na2B4O7 and 0.1 m H3PO4 (pH 9.15) as running buffer, and detecting by using a diode array detector at wavelength 278 nm (Sun et al. 2008a). A rapid CE coupled with potential gradient detection for the determination of four quinolones, namely, ENX in a mixture with ofloxacin, FRX and pazufloxacin, was described. Separation was performed in a fused-silica capillary using a buffer of 30 mm Tris and 4 mm phosphoric acid at pH 8.9 (Fan et al. 2007). The interactions between FQs and human serum albumin were investigated by affinity CE. Based on the efficient separation of several FQs (including ENX) using a simple phosphate buffer (Zhang et al. 2007b), a simple method was developed for the effective separation of ENX, PFX together with other FQ residues in porcine tissues by CE with a diode array detector. A mixture consisted of 25 mm NaH2PO4, 25 mm Na2B4O7 and 25 mm H3BO3 (pH 9) was used as a running buffer (Sun et al. 2007).

Regarding PIA, a novel method was developed and validated for the separation and simultaneous quantitation of seven structurally different drugs: PIA and ofloxacin, pseudoephedrine, piroxicam, thiamin, pyridoxine and cyanocobalamin by capillary zone electrophoresis (Solangi et al. 2009b). The coupling of Ru(bpy)23+-based ECL detection with CE was developed for the simultaneous determination of proline and PIA in human urine (Sun et al. 2010a). A specific pressure-assisted CE-MS method is described for the analysis of PIA in combination with danofloxacin, enrofloxacin, flumequine and ofloxacin. The most suitable electrolyte was 60 mm (NH4)2CO3 at pH 9.2. Using this method, the FQs were analyzed in fortified samples of chicken and fish (Juan-Garcia et al. 2006). One report used narrow-bore fused-silica capillaries to perform high-efficiency separation of PIA and NDA using a buffer composed of 40 mm sodium tetraborate and 5% methanol as organic modifier (Rusu et al. 2011).

For the analysis of OXA, a magnetic solid-phase extraction method combined with CE for the simultaneous determination of the concerned drug with other FQs using (S)-(+)-6-methoxy-α-methyl-2-naphthaleneacetic acid as internal standard in milk samples was developed (Ibarra et al. 2012). OXA together with other FQs was also assayed in bovine and porcine plasma, bovine milk using CE (Francisco et al. 2006, Hermo et al. 2011).

Several other methods were reported for the quantitation of FRX. Field-enhanced sample injection for sample stacking prior to the CE separation was developed inside a bubble cell capillary for highly sensitive detection of five typical FQs in bovine milk of which we concern FRX (Deng et al. 2014). Ethylene diamine was proposed as the main component for the antibiotics separation. A rapid method for the determination of residues of FRX with other three FQs in blood samples was developed. The method was based on matrix solid-phase dispersion extraction followed by CE with UV detection. 1-Butyl-3-methylimidazolium tetrafluoroborate was used as the background electrolyte (Li et al. 2011). A CE method based on ECL detection with Ru(bpy)32+ was developed for the simultaneous determination of FRX and proline in human urine. The most favorable resolution and high sensitivity were obtained using a 15 mm phosphate buffer at pH 9.6 with the detection potential at 1.15 V (Sun et al. 2009a). FRX was also determined with other FQs by CE using silica nanoparticles as running buffer additive (Wang et al. 2009b). A method for the simultaneous separation of FQs (including FRX) and tetracyclines by CE was developed. The UV detection wavelength was 262 nm, the running buffer consisted of 50 mm NaB4O7-200 mm H3BO3 with pH 8.41 and the separation voltage was at 18 kV (Shen et al. 2012). FRX together with eight FQs was separated by CE-UV based on poly(methacrylic acid-co-ethylene glycol dimethacrylate) monolith microextraction coupled with an online preconcentration technique of field-amplified sample stacking (He et al. 2010a).

For the assay of PFX, novel methods to determine its pharmacokinetics in urine of healthy adults were developed. The proposed methodologies were based on the ECL of tris(2,2′-bipyridine)ruthenium (II) at a platinum electrode (Li et al. 2008b, Deng et al. 2009).

The determination of five FQs, namely, RFX, ciprofloxacin, enrofloxacin, gatifloxacin and moxifloxacin, in acidic buffer by a CE-capacitively coupled contactless conductometric detection technique was prescribed. The separation was carried out in a fused-silica capillary using a buffer composed of 10 mm tartaric acid, 14 mm sodium acetate and 15% (v/v) methanol at pH 3.8 (Yang and Qin 2009).

A Micellar electrokinetic capillary chromatography (MEKC) method was developed using 1-butyl-3-methylimidazolium hexafluorophosphate (BMIM) PF6 as a modifier for separating ENX together with other seven FQs. Under the optimal conditions of 10 mm sodium borate, pH 7.1, 1.7% (w/w) SDS, 1.5% (w/w) [BMIM] PF6 with 18 kV as running voltage, the eight investigated FQs were baseline separated within 15 min (Chen et al. 2012b).

Another MEKC method has been developed for the simultaneous separation of seven FQs including FRX. Baseline separation was achieved in a carrier electrolyte containing 1% (v/v) heptane, 100 mm SDS, 10% (v/v) 1-butanol and 8-mm phosphate-sodium tetraborate buffer at pH 7.3 (Wei et al. 2008).

Thin layer chromatography (TLC)

The densitometric analysis of NFX in microemulsions was developed and validated. The compact spot for NFX was found at an Rf value of 0.39±0.02 at an absorption wavelength of 288 nm using a mobile phase consisting of chloroform:methanol:formic acid (7.5:2.0:0.5, v/v) (Kumar et al. 2010). Another work described the HPTLC method for the analysis of NFX and mometasone furoate in topical cream. The separation was carried out using dichloroethane:di-ethyl ether:ammonia:methanol:ethylacetate (6:3:0.2:1.75:3.5, v/v) as the mobile phase. The densitometric scanning was carried out at 254 nm (Amol et al. 2010). PIA and PFX together with other FQs were separated with TLC using either buffer (pH=5.5)-methanol, or 40:10 (v/v) or acetonitrile-water-acetic acid, 6:40:4 (v/v/v) (Bober 2008).

Gas chromatography (GC)

Derivatization of some pharmaceutical substances for GC analysis including NDA was performed using many derivatizing reagents of different types; the derivatization was followed by the GC/MS detection of the resultant products. The number of labile hydrogen atoms in the initial molecules substituted by the structural fragments of derivatizing reagents was determined (Gulyaev and Revel’skii 2010).

High performance liquid chromatography

Several HPLC methods were developed to separate FQs in pure form, pharmaceutical preparations, biological fluids, environmental samples, cosmetics, animals’ tissues and so on. Such methods are abridged in Table 2.

Table 2:

Reported HPLC methods for the determination of FQs.

NameMatrixColumnMobile phaseDetectionReferences
NDA and metronidazoleTabletsC18Mixed phosphate buffer (pH 4.5; KH2PO4+K2HPO4):methanol:acetonitrile; 30:50:20 v/vUV detectionKumar et al. 2015
Seven FQs including NDA, OXAGilthead sea breamC18Gradient elution using 0.1% trifluoroacetic acid (pH=1), acetonitrile and methanolTandem mass spectrometryEvaggelopoulou et al. 2014
Nineteen FQs including NDA, OXA, PIA, ENX, FRX, PFXEnvironmental water samplesC18Gradient elution using 0.02% aqueous formic acid and acetonitrileTandem mass spectrometryLombardo-Agüí et al. 2014
NDA, OXA with other classes of antibioticsFresh egg samplesC18Gradient elution using (methanol-acetonitrile 8:2, v/v) and (0.1% formic acid)Tandem mass spectrometryPiatkowska et al. 2014
NDA, OXA, PMA, PIA, ENX together with other FQs and β lactamsRaw cow milkC18Gradient elution using 50 mm aqueous ammonium formate pH 4 and methanolMS/MSJunza et al. 2014
FRXHuman plasmaC18Acetonitrile-0.1% trifluoroacetic acid-water (20:20:60)UV detectionSong-feng et al. 2015
NFXBulk powderC180.05% v/v trifluoroacetic acid and acetonitrile (65:35 v/v)UV detectionAyyagari et al. 2014
Several quinolones (NDA, FRX, PFX) with sulfonamidesMilk samplesC18Gradient elution using acetonitrile and 0.1% formateTandem mass spectrometryCao et al. 2013
Nineteen quinolone antibiotics including OXACosmeticsC18Methanol:acetonitrile (85:15, v/v)-0.05 m phosphate buffer (pH 3.6) under gradient elutionDiode array detectionChen et al. 2013
Some quinolones including PIA and PFXTap water and human urineC18Gradient elution with of 10 mm sodium citrate at pH 4 (solvent A) and acetonitrile (solvent B)Fluorescence detectionFrancisco et al. 2013
Ten quinolones (NDA) and eight cephalosporinsMilk samplesC18 columnGradient elution using a mobile phase of 0.1% TFA in water and 0.1% TFA in ACNMS/MSKarageorgou et al. 2013
Quinolone antibacterials (NDA, OXA)Sewage sludgeC18Gradient mobile phase consisting of 0.2% (v/v) formic acid aqueous solution (solvent A) and methanol (solvent B)MS/MSDorival-Garcia et al. 2013a
Thirty-one antibiotics including NDA and ENXDrinking water, surface water and reclaimed watersC18Gradient elution using a mobile composed of water, methanol, acetonitrile, 0.1% formic acidMS/MSPanditi et al. 2013
Eighty-four veterinary drug residues (benzimidazoles, FQs: ENX, OXA, NDA, nitroimidazoles, β-lactams, macrolides, triphenylmethane dyes, sulfonamides and tetracyclines)Chicken muscles and tissuesC18Gradient elution using a mobile composed of 0.1% formic acid in water, 0.1% formic acid in acetonitrileMS/MSBiselli et al. 2013
Thirty-four antibacterial drugs (aminoglycosides, β-lactams, fluoroquinolones including OXA, NDA, macrolides, sulfonamides, trimethoprim and tetracyclines)Fish samplesC18Gradient elution using a mobile composed of (A): acetonitrile; (B): 0.025% Heptafluorobutyric in waterTandem mass spectrometryGbylik et al. 2013
Two hundred and twenty undesirable chemical residues including PIA, PFX, ENX, OXA, NDAInfant formulaeC18 columnMethanol containing 0.1% (v/v) formic acid and water containing 0.1% (v/v) formic acid/0.5 mm ammonium acetateTandem mass spectrometryZhan et al. 2013
Seven veterinary drugs, including furazolidone, 4 sulfonamides, OXA, NDAAquatic productsC18 columnGradient elution with mixtures of acetonitrile and 0.08 m acetic acidUV detectionMeng et al. 2012
Fifty-three antibiotic residues including OXA, NDA, PIAHospital and urban wastewatersC18 columnSolvent (A) acetonitrile, solvent (B) HPLC grade water acidified with 0.1% formic acidTandem mass spectrometryGros et al. 2013
Thirty-six antibiotics from seven different chemical classes (aminoglycosides, macrolides, lincosamides, sulfonamides, tetracyclines, FQs including ENX, OXA, NDA and trimethoprimChicken meatPhenyl columnGradient elution using solvent (A) 1 mm heptafluorobutyric acid+0.5% formic acid in water and (B) 0.5% formic acid in acetonitrile/methanol (1:1, v/v)Tandem mass spectrometryBousova et al. 2013
Seventy-two veterinary residues including NDA, FRXShrimps samplesC18 columnGradient elution with acetonitrile and 0.1% formic acidTandem mass spectrometryBu et al. 2012
Fifty-four veterinary drug residues of six families including sulfanilamide, nitroimidazoles, macrolide antibiotics, lincosamides, praziquantel, FQs including NDA, OXA, ENXPork meat samplesC8 columnGradient elution with acetonitrile, methanol and formic acidMS/MSXie et al. 2012
FQs including NDA, OXA, PIA, ENX, PMAUrban waste watersC18 columnGradient mobile phase consisting of 0.2% (v/v) aqueous formic acid solution (solvent A) and methanol (solvent B)MS/MSDorival-Garcia et al. 2013b
Seven quinolone antibacterials including OXA, NDATissue of Atlantic salmonC18 column0.1% trifluoroacetic acid (pH 1), acetonitrile and methanolPhotodiode array detectorEvaggelopoulou and Samanidou 2013
Veterinary drug residue anal. (sulfonamides, tetracyclines and FQs including OXA, ENX, NDAAnimal urine samplesC18 columnGradient elution using mobile phase of acetonitrile and formic acidMass spectrometryKaufmann and Walker 2013
Two hundred and fifty-five veterinary drug residues and contaminants of different classes including PIA, PFX, ENX, OXA, NDAMilk samplesC18 columnGradient elution using mobile phase composed of: 0.1% (v/v) formic acid in water containing 0.5 mm (v/v) ammonium acetate, methanol containing 0.1% (v/v) formic acidTandem mass spectrometryZhan et al. 2012
Eight FQs including OXA, NDAGround waterC18 columnH3PO4 (50 mm) and acetonitrile in different ratiosFluorescence detectionVazquez et al. 2012
Forty-two pesticides and veterinary drugs including NDA, OXAMilk samplesC18 columnGradient elution using a mobile phases of acetonitrile and water containing 0.1% formic acidMass spectrometryGao et al. 2012
FQs including NDA, OXAEgg samplesLuna C8Gradient elution using a mobile phases of acetonitrile (A) and 0.02 m oxalic acid, pH=4.0 (B)MS/MSGajda et al. 2012
FQs including OXA, NDASurface watersC18 columnPhosphoric acid and 5% methanolFluorescence detectionGarcia et al. 2012
FQs: cinoxacin, OXA, NDA, flumequineUnderground water, river and sea waterC18 columnGradient elution using a mobile phases of (A): 0.1% formic acid and 10% methanol in and (B): 100% methanolMass spectrometryWang and Wang 2012
Tetracyclines, quinolones (OXA, NDA) and sulfonamidesMeat samplesC18 columnGradient elution using solvent A (aqueous solution 0.1% formic acid) and solvent B (acetonitrile with 0.1% formic acid)Tandem mass spectrometryBittencourt et al. 2012
Several FQs including PIA, OXA, NDA, PMAFish samplesC18 columnMixtures of methanol-acetonitrile-10 mm citrate buffer at pH 4.5, delivered under optimum gradient programPhotodiode array and fluorescence detectionCanada-Canada et al. 2012
Thirty-seven antibiotic substances from the six antibiotic groups: macrolides, lincosamides, quinolones (NDA, OXA, ENX), tetracyclines, pleuromutilines and diamino-pyrimidine derivativesHoney samplesC18 columnGradient elution using A: water (with 0.2% formic acid) and B: acetonitrile (with 0.2% formic acid)Tandem mass spectrometryBohm et al. 2012
Fifteen kinds of FQs including ENX, FRX, PFX, NDAFood of animal originC18 columnThree gradient system with methanol/acetonitrile/0.02 m citric acid and 0.03 m ammonium acetateUV detectionYu et al. 2012c
Nine quinolones including OXA, NDAHoney samplesC18 columnSolvent mixture of acetonitrile (25%) and SDS solution (75%) (pH 2.5)Fluorescence detectionDu et al. 2011
Twenty-three antibiotics of different classes: sulfonamides, tetracyclines, macrolides, β lactams, diaminopyrimidines, nitro-imidazoles, FQs including NDA, OXA, PIA, ENXEnvironmental water samplesC18 columnGradient elution using UP-water+0.1% formic acid (A) and acetonitrile+0.1% formic acid (B)MS/MSDinh et al. 2011
Forty-seven pharmaceuticals of different classes including PFX, OXA, NDA, PIAEnvironmental and wastewaterC18 columnGradient elution using: water/methanol, 0.1 mm ammonium acetate and 0.01% formic acidMS/MSGracia-Lor et al. 2011
Thirty-three analytes from 13 classes of antibiotics: tetracyclines, FQs; (NDA, OXA), penicillins, macrolides, sulfonamides, quinoxalines, phenicols, lincosamides, diaminopyrimidines, polypeptides, streptogramins and pleuromutilinsAnimal feedsC18 columnGradient elution with A: water with 0.1% formic acid and B: mixture of acetonitrile/methanol (70/30, v/v) with 0.1% formic acidMS/MSBoscher et al. 2010
Eighteen FQs including ENX, OXA, NDA, PMA and PIAMilk, chicken, pork, fish and shrimpC8 columnGradient elution using 20 mm ammonium formate in 0.1% formic acid-acetonitrileMS/MSChang et al. 2010
FQs including PIA, ENX, OXA, NDAFish tissuesC18 columnGradient elution using 0.2% formic acid in water as solvent A and 0.2% formic acid in acetonitrile as solvent BFluorescence detectionZhang et al. 2010
FQs including (OXA, NDA)Porcine muscle, table eggs and milkC18 columnGradient mobile phase composed of acetonitrile and 0.01 m oxalic acid buffer at pH 3.5Fluorescence detectionCho et al. 2010
FQs: NDA, ENX, PFXAquatic productsC18 columnWater and acetonitrile (contains 0.4% formic acid)Tandem mass spectrometryKang et al. 2008
OXA, NDA and flumequineMilk samplesC18 column0.1% phosphoric acid and acetonitrile with gradient elutionUV detectionZeng et al. 2009
Some FQs including OXA, NDA, PMASwine musclesC18 columnAcetonitrile: 0.05 m sodium dihydrogen phosphate (pH 2.5) (35:65, v/v) containing 3.7 mm SDSDiode array detectionTsai et al. 2009
Forty-seven substances of the antibiotic groups tetracyclines, FQs (OXA, NDA, ENX), macrolides, sulfonamides, diaminopyrimidine derivatives and lincosamidesMilk samplesC18 columnGradient elution using A (water with 0.2% formic acid) and B (acetonitrile with 0.2% formic acid)Mass spectrometryBohm et al. 2009
FQs including NDA, OXAAnimal feedsC18 columnGradient elution with acetonitrile and o-phosphoric acid 25 mm at pH 3Fluorescence detection and photodiode arrayGalarini et al. 2009
Nineteen kinds of FQs: NDA, OXA, ENX, FRX, PFXAnimal foodsC18 column0.1% formic acid-methanol system as the mobile phase with a linear gradient elution programTandem mass spectrometryLi et al. 2008c
Eleven FQs including OXA, NDAChicken, pork, fish and shrimpC18 columnLinear gradient elution of 0.1% formic acid and acetonitrileFluorescence detectionChang et al. 2008
OXA, ENX, PFX, NDA, PIA together with other FQsPig and fishC18 column0.1% formic acid-methanol with a linear gradient elutionMS/MSLi et al. 2009c
Nineteen quinolones residues including OXA, FRX, ENX, PIA, PFX, NDAHoney samplesC18 columnLinear gradient elution program of methanol and 0.1% formic acid solutionMS/MSDing et al. 2009
Eighty-nine compounds including NDA, OXAMilk samplesC18 columnGradient system of 0.1% formic acid-acetonitrile containing 0.1% formic acidMS/MSFujita et al. 2008
Five antibiotic groups: FQs: (OXA, NDA, PIA, ENX), sulfonamides, nitro-imidazole and diaminopyrimidineNatural watersC18 columnGradient elution with ultra-pure water (solvent A) and acetonitrile (solvent B), both solvents acidified with 0.01% formic acidTandem mass spectrometryTamtam et al. 2009
Twenty FQs (PIA, FRX, PFX, ENX, OXA, NDA, PMA)Influent, effluent and river watersC18 columnGradient elution with methanol (A) and purified water containing 0.1% formic acid (v/v) (B)Tandem mass spectrometryXiao et al. 2008
Twelve FQs, such as PFX, OXA, NDAEgg samplesC18 columnAcetonitrile-citric acid/ammonium acetate buffer in water as the mobile phase using a linear gradient elution programFluorescence detectionLiao et al. 2008b
Seven quinolones (OXA, NDA)Gilthead sea breamC18 columnGradient elution using a mixture of 0.2% (v/v) formic acid, methanol and acetonitrileMS/MSSamanidou et al. 2008
Twelve quinolones (NDA, OXA)Muscles, liver, chicken eggs, milk, prawn and rainbow troutC18 columnGradient system of 0.1% phosphoric acid-acetonitrileFluorescence detectionChonan et al. 2008
Several FQs such as NDAUrine, ground water, hospital wastewater and chicken muscleC18 columnCitrate buffer (0.001 m) of pH 4.5, methanol and acetonitrile using gradient elutionUV detectionKumar et al. 2008
Ten quinolones: ENX, OXA, NDABovine liver and porcine kidneyC18 columnGradient elution using a mixture of TFA 0.1%-acetonitrile-methanolPhotodiode arrayChristodoulou et al. 2008
Ten quinolones: ENX, OXA, NDAVarious tissues of food-producing animalsC18 column0.1% TFA-methanol-acetonitrile using a gradient programPhotodiode arrayChristodoulou et al. 2007b
Ten FQs (ENX, OXA, NDA)Chicken muscle and egg yolkC18 columnGradient elution using a mixture of 0.1% trifluoroacetic acid-acetonitrile-methanolPhotodiode arrayChristodoulou et al. 2007a
Ten FQs (ENX, OXA, NDA)Cow’s milkC18 columnMixture of TFA 0.1%-acetonitrile-methanol delivered by a gradient programPhotodiode arrayChristodoulou and Samanidou 2007
OXA, NDAShrimp samplesC8 column60% oxalic acid (0.01 m), 30% acetonitrile and 10% methanol (v/v/v)Fluorescence, mass spectrometryKarbiwnyk et al. 2007
Fifteen FQs (PIA, ENX, OXA, NDA, PMA)Urine and pharmaceutical samplesC18 columnMixtures of methanol-acetonitrile-10 mm citrate buffer at pH 3.5 and 10 mm citrate buffer at pH 4.5, delivered under an optimum gradient programDiode array and fluorescence detectionCanada-Canada et al. 2007
Sixty-three veterinary drugs including OXABovine, porcine and poultry musclesC18 column0.1% formic acid-acetonitrile in a gradient modeTandem mass spectrometryTagiri-Endo and Yanagita 2007
OXAFish farmsC18 columnMixture of acetonitrile and orthophosphoric acidFluorescence detectionPouliquen et al. 2006
Flumequine and oxolinic acidAquatic sediments and agricultural soilsC8 column10 mm oxalic acid buffer at pH 4-acetonitrile (65:35, v/v)Fluorimetric detectionPrat et al. 2006
Eighteen drugs of different classes including NDA, OXARaw shrimp, meat samplesPhenyl columnA: 5% (v/v) acetonitrile/water, with 0.1% formic acid; B: 85% (v/v) acetonitrile/water with 0.05% formic acid. Two gradients were usedMass spectrometryLi et al. 2006b
Several quinolones (ENX, OXA, NDA)Soil samplesC18 columnLinear gradient elution using: A (3.16 mm formic acid, pH 2.5) and B (acetonitrile)UV detectionTuriel et al. 2006
Sulfonamides and quinolones residues (OXA)Milk samplesC18 columnGradient elution using acetonitrile and 0.1% formate in waterTandem mass spectrometryCao et al. 2013
Fifty antimicrobials from 13 different families including OXAAnimal feedsC18 columnGradient elution using A (5 mm aqueous formic acid), B (50 mm aqueous formic acid/acetonitrile (10/90, v/v)Tandem mass spectrometryBorras et al. 2013
Twenty-nine veterinary drugs residues including 6 quinolones (OXA), 14 sulfonamides, 3 nitrofurans and 6 macrolidesAnimal feed samplesC18 columnAcetonitrile and water (containing 0.1% formic acid) in gradient elutionTandem mass spectrometryLiu et al. 2013
Twenty-five antibiotics: 11 sulfonamides and 14 FQs (PIA, FRX, PFX, OXA)Mineral and run-off watersC18 columnGradient elution using 0.3% (v/v) formic acid in Milli-Q water as mobile phase A and acetonitrile as mobile phase BDiode array detectionHerrera-Herrera et al. 2013
Twenty-nine veterinary drugs, FQs (OXA), sulfonamides, macrolides, nitrofuranFeed samplesC18 columnGradient elution program of methanol and water (containing 0.2%formicacid)Mass spectrometryLi et al. 2012
Twenty-nine veterinary drug:14 sulfonamide drugs, 3 nitrofuran drugs, 6 macrolide drugs, 6 FQs such as OXAFeed premix samplesC18 columnMethanol and water (containing 0.1% formic acid) in gradient elutionMS/MSLiu et al. 2012a
Twenty-nine veterinary drugs: sulfonamides, macrolides and nitrofurans, FQs (OXA)Compound feedsC18 columnGradient elution with the mobile phases of methanol and 0.1% (v/v) formic acid solutionTandem mass spectrometryZhao et al. 2012
One hundred and twenty drug analytes from 11 different classes including OXABovine kidneyC18 columnGradient elution using (A) 0.1% aqueous formic acid and (B) 0.1% formic acid in acetonitrileTandem mass spectrometrySchneider et al. 2012
Thirty-two veterinary drug residues belonging to several families including OXAFish samplesC18 columnGradient elution using 0.1% formic acid in acetonitrile (eluent A) and 0.1% formic acid in water (eluent B)Tandem mass spectrometryLopes et al. 2012b
Eight quinolones of veterinary use (OXA)Bee productsC18 column0.02% formic acid solution and acetonitrileMass spectrometryLombardo-Agüí et al. 2012
Twenty veterinary drug residues belonging to several classes: sulfonamides, macrolides, anthelmintics, diamino derivatives, FQs (OXA)Chicken musclesC18 columnGradient elution using 0.1% (v/v) formic acid in acetonitrile (eluent A) and 0.1% (v/v) formic acid in water (eluent B)Tandem mass spectrometryLopes et al. 2012a
Eight quinolone residues OXAChicken tissuesC18 column0.1% trifluoroacetic acid aqueous solution (pH 3), methanol and acetonitrile (82:12:6 v/v)Fluorescence detectionXia and Peng 2011
Fifteen FQs such as: OXA, ENX, FRXRaw bovine and skimmed milkC18 columnGradient elution using mobile phase consisting of (A) ultra-pure water and (B) acetonitrile, both acidified with 0.2% formic acidTandem mass spectrometryKantiani et al. 2011
Twelve FQs (PIA, OXA, FRX, PFX)Different infant and young children powdered milksC18 columnGradient elution using water containing 0.1%–0.2%, v/v formic acid as mobile phase A, methanol and acetonitrile (both with and without 0.1% v/v formic acid) as mobile phase BMS/MSHerrera-Herrera et al. 2011
Six antibiotic residues including tetracyclines, sulfanilamides and FQs: OXA, ENX, FRXCoastal watersC18 columnBinary eluent containing methanol and water with 0.1% formic acidMS/MSNa et al. 2011
Nine quinolones such as OXAEgg matricesC18 columnMobile phase A: an aqueous solution of 0.01 m oxalic acid, mobile phase B: acetonitrile, applying gradient elutionFluorescence detectionJimenez et al. 2011a
Several FQs: OXA, PIA, PMABovine and porcine plasmaC8 columnGradient program with mobile phase that combined solvent A (10 mm citric acid-acetonitrile (91:9, v/v), adjusted with NH3 and solvent B (acetonitrile)UV detection, mass spectrometry and tandem mass spectrometryHermo et al. 2011
Forty-one antimicrobial agents belonging to seven families (sulfonamides, diaminopyridine derivates, quinolones: OXA, tetracyclines, macrolides, penicillins and lincosamides)Egg matricesC18 columnGradient elution using mobile phase A: an aqueous solution of 0.02% formic acid and 1 mm oxalic acid, and mobile phase B: acetonitrile with 0.1% formic acidTandem mass spectrometryJimenez et al. 2011b
Twenty-four important veterinary drugs including aminoglycosides, β-lactams, lincosamides, macrolides, FQs: OXA, sulfonamides, tetracyclines and amproliumChicken musclesC18 column50 mm ammonium formate in water at pH 2.5 (mobile phase A) and acetonitrile (mobile phase B) using gradient elutionMS/MSChiaochan et al. 2010
Nitroimidazoles, sulfonamides and FQs: OXA, ENX, FRX, PFXHoney samplesC18 columnGradient solvent system (acetonitrile-methanol-formic acid solution)Tandem mass spectrometryHe et al. 2010b
FQs: OXAFish musclesC18 column0.065 m sodium dodecyl sulfate, 12.5% propanol and 0.5% triethylamine buffered at pH 3Fluorescence detectionRambla-Alegre et al. 2010
Fifteen FQs: OXA, FRXHoney samplesC18 columnGradient solvent system (acetonitrile-0.1% formic acid)Electrospray ionization, tandem mass spectrometricHe et al. 2010c
Thirty-eight compounds from a variety of drug classes including OXAFour species of fishPhenyl columnGradient elution using mobile phase A: 0.1% formic acid with 10 mm NaOH in water and B: acetonitrileMass spectrometrySmith et al. 2009
Seven trace FQs: OXAMilk, egg, chicken and fishC18 columnA mixture of formic acid solution and acetonitrile was used in gradient elutionMass spectrometryZheng et al. 2009
Several FQs such as OXA and sulfonamidesSwine and chicken muscle tissuesC18 columnFormic acid solution-acetonitrile system as mobile phase with a linear gradient elution programUV detection and fluorescence detectionLi et al. 2009d
Nine quinolones including OXAPorcine, chicken and bovine musclesC8 columnGradient elution using a mobile phase of 200 mm ammonium acetate buffer (pH 4.5) and acetonitrileFluorescence detectorLee et al. 2009
Oxolinic acid and flumequinePure formC18 columnWater-acetonitrile (2:1, v/v) at pH 2.5Fluorescence detectionFeas et al. 2009
Flumequine and oxolinic acidEel tissuesC8 column0.01 mol/l oxalic acid and acetonitrile (65:35)Fluorescence detectionLiu et al. 2009
Several FQs as OXATilapia filletsC18 columnGradient elution using water and acetonitrile, both containing 0.1% of acetic acidTandem mass spectrometryPaschoal et al. 2009
Several FQs as PFX, OXAChicken musclesC18 columnGradient elution (acetonitrile and water as mobile phases)Fluorescence detectorLin 2009
FQs including OXA, ENX, FRXHoney samplesC18 columnMethanol-ammonia solution (19:1, v/v)Tandem mass spectrometryCao et al. 2008
Seven quinolone antibacterials: OXAWhole eggsC18 columnGradient elution using component A (acetonitrile) and component B (water). Both components were acidified with 20 mm formic acidTandem mass spectrometryBogialli et al. 2009
OXA with other FQsBovine milk samplesC18 columnFormic acid solution 0.1% (v/v) and acetonitrile using linear gradient elutionMass spectrometryZafra-Gomez et al. 2008
OXA with other FQsPig liverC8 column0.005 m ammonium acetate and formate solution and acetonitrile (86:14, v/v) at pH 2.5 using gradient elutionMass spectrometryHermo et al. 2008
Several veterinary drugs including OXALivestock foods and fishC18 column0.1% formic acid-acetonitrileTandem Mass spectrometryKai et al. 2007
OXA and other FQsPig kidneyC8 columnAcetonitrile and 10 mm citrate buffer of pH 4.5 using linear gradient elutionFluorescence detectionHassouan et al. 2007b
PIA, OXA with other FQsFish, chicken muscle, chicken liver and pig kidneyC18 columnPhosphoric acid:water:triethylamine:acetonitrilePhotodiode array and fluorescence detectionRomero-Gonzalez et al. 2007
OXA and other FQsEgg samplesC18 columnAcetonitrile and 10 mm citrate buffer solution of pH 4.5 using linear gradient elutionFluorescence detectionHassouan et al. 2007a
Nine quinolones such as OXABovine musclesC18 columnWater/acetonitrile mixtures containing acetic acidTandem mass spectrometryRubies et al. 2007
OXASerum and muscles of the Chinese mitten crabC18 columnAcetonitrile and 0.02 m phosphate buffered saline pH 3 (25:75)Fluorescence detectionTu et al. 2006
OXAFish farmsC18 columnAcetonitrile and aqueous orthophosphoric acid solutionFluorescence detectionPouliquen et al. 2006
Antibiotics including sulfonamides, macrolides, quinolones (OXA), tetracyclines and trimethoprimChlorine-disinfected drinking waterC18 columnAcidified methanol (0.1% formic acid)Tandem mass spectrometryYe et al. 2007
Oxolinic acid and flumequineAquatic sediments and agricultural soilsC18 column65% aqueous oxalic buffer at pH 4 and 35% acetonitrileFluorescence detectionPrat et al. 2006
OXA with erythromycin, fungicides and parasiticideEdible portion of salmonC18 columnGradient elution using acetonitrile as solvent A and 0.1% formic acid in water (pH 3.5) as solvent BMass spectrometryHernando et al. 2006
Several FQs such as OXAChicken musclesC8 columnGradient elution using 0.02 m ammonium acetate solution adjusted at pH 2.5 using formic acid/acetonitrile (86:14)Mass spectrometryBailac et al. 2006
Some FQs such as OXAPig musclesC8 column0.005 m ammonium acetate and formate solution and acetonitrile (86:14, v/v) at pH 2.5 with gradient elutionTandem mass spectrometryHermo et al. 2006
Ten quinolones such as OXA, NDA, PFX, PIA and penicillinsGroundwater and surface watersC18 column8 mm ammonium acetate at pH 2.5 adjusted with formic acid (A) and acetonitrile with 0.1% formic acid (B) with gradient elutionElectrospray tandem mass spectrometryPozo et al. 2006
FQs such as OXABee productsC18 column0.02% aqueous formic acid solution and acetonitrileMS/MSLombardo-Agüí et al. 2012
PIA with other FQsPharmaceuticalsC18 column0.15 m sodium dodecyl sulfate, 2.5% propanol and 0.5% triethylamine at pH 3UV detectionCollado-Sanchez et al. 2010
PIA, ENX, FRX, PFXHuman urineC18 columnAcetonitrile:0.02 m tetrabutyl ammonium bromide (9:91, v/v) adjusting pH 2.87 by trifluoroacetic acid bufferDiode array detectorSun et al. 2008b
Thirty-one antimicrobials including β-lactams, lincosamides, macrolides, quinolones (PIA), sulfonamides, tetracyclines, nitroimidazoles and trimethoprimCattle and pig meatC18 columnGradient elution using component A: methanol with 10 mm formic acid, and B: water with 10 mm formic acidMS/MSCarretero et al. 2008
Fifty antibiotic drugs including chloramphenicol, sulfonamides, FQs (ENX), tetracyclines and macrolidesSewage sludgeC18 column0.1% formic acid-methanol or acetonitrile-water by gradient elutionMS/MSWang et al. 2013
Ten kinds of antibiotics such as ENX, PFXCosmeticsC18 columnAcetonitrile-0.05 m ammonium dihydrogen phosphateUV detectionYang et al. 2012
One hundred and nineteen pharmaceuticals including ENXSewage sludgeC18 columnMobile phase composed of (A) 0.01% NH4OH and (B) acetonitrile, using gradient elutionMass spectrometryWilliam and Emmanuelle 2013
Fifty-eight pharmaceuticals including ENXEnvironmental watersC18 column0.1% formic acid+0.02% trifluoroacetic acid using gradient elutionElectrospray tandem mass spectrometryLopez-Serna et al. 2012
Ten FQs such as ENX, FRX, PFXGrass carpC18 columnGradient elution program with acetonitrile and water (containing 0.05% formic acid)Mass spectrometryLiu et al. 2012b
Two FQs (ENX and lomefloxacin), sulfonamides and tetracyclineAnimal tissues matrixC18 columnAcetonitrile-dichloromethane (1:1, v/v). acetonitrile and acetic acid (0.1%) were combined in a gradient elutionDiode array detectionYu et al. 2012a
ENXEstuarine and coastal seawaterC18 columnAcetonitrile and water containing 0.2% formic acidTandem mass spectrometryYang et al. 2011
Some antibiotics such as ENX, PFXMilk samplesC18 columnGradient elution using a mobile phase consisting of acetonitrile (A) and aqueous solution: 2.9 mm [1-ethyl-3-methylimidazolium tetrafluoroborate], 0.7 mm ammonium acetate-acetic acid, pH=2.70) (B)UV detectionGao et al. 2011b
Twenty antibiotic residues including cephalosporins, macrolides, quinolones: ENX, FRXMilk and powdered milkC18 columnAcetonitrile (containing 0.2% formic acid)-0.006 m ammonium acetateTandem mass spectrometryWang et al. 2011
Twelve FQs such as ENX, FRX, PFXHoney samplesC18 columnMobile phase (pH 2.5) consisted of methanol and 1% aqueous formic acid (29:71, v/v) in gradient elutionDiode array detectorYu et al. 2011
ENX and its related substancesPure formC18 columns0.025 m phosphoric acid solution-methanol-acetonitrile in gradient elutionUV detectionDu and Cao 2011
Nineteen antibiotics, including tetracyclines, sulfonamides, macrolides, quinolones (ENX) and β-lactam antibioticsEnvironmental water samplesC18 columnsMethanol-0.1% formic acid as mobile phase in gradient elutionMS/MSLu et al. 2010
Norfloxacin and ENXSerum and urineC18 column20 mm sodium dihydrogenphosphate (pH 3) and acetonitrile (85:15, v/v)UV detectionKobayashi et al. 2011
Seventy-four pharmaceuticals including ENXEnvironmental waters and sewageC18 columnAcetonitrile/0.1% (v/v) formic acid in a gradient elutionElectrospray tandem mass spectrometryLopez-Serna et al. 2010
Twenty-eight antibiotics residues including FRX, ENX, PFXHoney samplesC18 columnPhase A [methanol (containing 0.4% formic acid)-acetonitrile, 65:35] and phase B (0.4% formic acid solution in gradient elution)Tandem mass spectrometryZuo et al. 2009
Norfloxacin, ciprofloxacin and ENXPure formC18 column15 mm sulfuric acid and 35% (v/v) methanolFluorescence detectionSong et al. 2008
FRX, ENX and other FQsChicken tissuesC18 columnFormic acid solution and acetonitrileFluorescence detectionMa et al. 2008
ENX, ELR with other FQsPure formC18 column11 mm tetrabutyl ammonium bromide solution:acetonitrile (96:4) of pH 4.2UV detectionShi et al. 2009
Enoxacin and related substancesPure formC18 columnSodium dodecanesulfonate-methanol-acetonitrile (45:30:25, pH 3 adjusted by triethylamine)UV detectionYi et al. 2007b
Some residual antibiotics: sulfonamides, FQs (ENX, FRX)Chicken tissuesC18 columnGradient elution program of acetonitrile and water (containing 0.05% formic acid)Electrospray tandem mass spectrometryLiu et al. 2008a
EnoxacinHuman serumC18 columnAcetonitrile: 0.05 m citric buffer (15:85, pH 3.5)UV detectionSun et al. 2006
PFX, ENX and other FQsPure formC18 columnAcetonitrile: methanol: 1% trifluoroacetic acid (4:7:89)Fluorescence detectionYu and Bi 2007
ENX, FRX and other FQsPork samplesC18 columnAcetonitrile (containing 0.1% phosphatic acid)UV detectionHou et al. 2007
Enoxacin gluconate and related substancesEnoxacin gluconate injectionC18 column0.01 m citric acid (pH 3.5)-methanol-acetonitrile (78:12:10) or acetonitrile-phosphate buffer-0.05 m tetrabutyl ammonium bromide (5:37.5:1)UV detectionGao 2007
Norfloxacin, ciprofloxacin and ENXPure formC18 column15 mm H2SO4 and 35% methanol (v/v)Fluorescence detectionZhang et al. 2007a
Three sulfonamides and seven fluoroquinolones ENX, FRXPork samplesC18 columnMethanol-0.02 m phosphate buffer-triethylamine (25.5/74.5, v/v, pH 2.8)Diode array detectorLiu et al. 2006
Several FQs such as ENXEnvironmental watersC8 column5 mm ammonium formate (pH 3)/acetonitrile (85/15, v/v)Tandem mass spectrometryMitani and Kataoka 2006
Several FQs such as ENXUrine and serumC18 columnTetrahydrofuran (8%) and phosphate buffer (pH 3, 30 mm, 92%)Fluorescence detectionEspinosa-Mansilla et al. 2006
Eleven classes of antibiotics including FRXSurface waters and sludgeC18 columnGradient elution using (A): 5 mm oxalic acid, 0.1% formic acid, with 5 mm ammonium acetate and (B): acetonitrileTandem mass spectrometryZhou et al. 2012
FleroxacinFleroxacin and glucose injectionC18 columnTriethylamine and phosphoric acid-acetonitrile (83:17)UV detectionSong and Hao 2011
Twenty-two antibiotics (quinolones, sulfonamides and macrolides)Fish samplesC18 columnMethanol-acetonitrile (1:1, v/v)MS/MSLi et al. 2010
Fleroxacin and other FQsChicken breast muscleC18 columnAqueous solution of 54 mm formic acid and 10 mm ammonium acetate and acetonitrile in gradient elutionTandem mass spectrometryXu et al. 2011
FRX and other FQsSoil samplesC18 columnGradient elution using A: 25 mm H3PO4 and B: acetonitrileFluorescence detectionSturini et al. 2010b
Twenty-two antibiotics including FRXEnvironmental water samplesC18 columnA: methanol-acetonitrile (1:1, v/v) and B: 0.3% formic acid/water (containing 0.1% ammonium formate, v/v; pH 2.9) in gradient elutionTandem mass spectrometryGao et al. 2010
Several FQs such as FRXWater samplesC18 columnMixture of 0.25% formic acid and 10 mm ammonium acetate and acetonitrile using gradient elutionTandem mass spectrometryChen et al. 2010
Several FQs such as FRXBovine, ovine and caprine milkC18 column5 mm BMIM-BF4, 10 mm ammonium acetate at pH 3 and 13% (v/v) acetonitrile using gradient elutionFluorescence detectionHerrera-Herrera et al. 2009
Fleroxacin, levofloxacin, norfloxacin and ciprofloxacinHuman serumC18 columnMixture of isoleucine and CuSO4:methanol (80:20, v/v)Fluorescence detectionWang et al. 2008
FleroxacinFleroxacin and glucose injectionC18 columnTriethylamine and phosphoric acid-acetonitrile (82:18)UV detectionZhu et al. 2008
FleroxacinHuman plasmaC18 columnWater solution including L-isoleucine and CuSO4:methanol (80:20, v/v)Fluorescence detectionWang and Bai 2007
FRX with other FQsWater samplesC18 column5 mm BF4 and 10 mm ammonium acetate at pH 3 with 13% acetonitrileFluorescence detectionHerrera-Herrera et al. 2008
FleroxacinHuman blood plasmaC18 column1% triethylamine at pH 4.8 and acetonitrile (80/20, v/v)Fluorescence detectionFang et al. 2007
NadifloxacinCream dosage formsC18 columnAcetonitrile: tetrahydrofuran-0.025 m ammonium dihydrogen phosphate (35:5:60, pH 3)UV detectionZhang et al. 2006a
Pefloxacin mesylateBulk drug and in tablets dosage formC18 columnMethanol-buffer (30:70, v/v)UV detectionAgrahari et al. 2013
Eight kinds of quinolones such as PFXVeterinary drugs preparationsC18 columnPhosphoric acid-pure water-triethylamine-acetonitrile as mobile phase at a gradient elutionFluorescence detectionZhao and Fan 2012
Several FQs such as PFXWhole eggsC18 columnAcetonitrile-0.1% formic acid (13:87)MS/MSTian et al. 2010
Five fluoroquinolones including PFXWaste waterPhenyl columnMethanol or acetonitrile was used as the organic modifier (solvent A) and 10 mm acetate buffer (pH 9) was used as solvent B applying gradient elutionMS and fluorescence detectionSeifrtova et al. 2010
Pefloxacin, norfloxacin, ciprofloxacin and ofloxacinPharmaceutical preparations and human serumC18 columnWater-acetonitrile (50:50, v/v) mobile phase of pH 2.9 adjusted with phosphoric acidUV detectionSiddiqui et al. 2009
PFX and other FQsChicken muscleC18 columnMethanol/acetonitrile/0.2% formic acid (15/15/70, v/v/v)MS/MSChen et al. 2008b
Seventy-six pharmaceutical agents of nine classes of drugs including PFXSlaughterhouse waste waterC18 columnWater-acetonitrile using gradient elutionTandem mass spectrometryShao et al. 2009
Nine fluoroquinolone residues including PFXMilk samplesC18 columnMethanol/acetonitrile/0.2% formic acidMS/MSChen et al. 2008a
Pefloxacin mesilate and its related substanceTabletsC18 columnAcetonitrile-mixture of cetytrimethylammonium bromide with boric acid solution-2,2′-thiodiglycol (30:70:0.2, v/v/v)UV detectionLi et al. 2009a
PefloxacinBulk material, tablets and human plasmaC18 columnAcetonitrile: 0.025 m phosphoric acid solution (13:87, v/v); pH 2.9UV detectionGauhar et al. 2009
PFX together with other FQsRoyal jelly samplesC18 columnMethanol/acetonitrile/0.1% trifluoroacetic acid (8:4:88, v/v/v) pH 2.5Fluorescence detectionZhou et al. 2009
Related substances and contents in pefloxacin mesylatePefloxacin mesylate injectionC18 column0.04 m potassium dihydrogen orthophosphate-acetonitrile-0.05 m tetrabutyl ammonium bromide (80:9:8) pH 2.5UV detectionLi et al. 2006a
PFX and other FQsFish and shellfish muscleC18 column0.1 m phosphoric acid and acetonitrile (91:9, v/v)Fluorescence detectionJo et al. 2006
PFX and other FQsPharmaceutical preparationsC18 columnWater: acetonitrile (80:20, v/v) with 0.3% of triethylamine and pH 3.3UV detectionSantoro et al. 2006
RFX and other FQsMilk samplesC18 columnMethanol-10 mm ammonium acetate solution (25:75)MS/MSJiao et al. 2009b

  1. ACN, acetonitril; BMIM, 1-butyl-3-methylimidazolium hexafluorophosphate; ENX, enoxacin; FQs, fluoroquinolones; FRX, fleroxacin; HPLC, high performance liquid chromatography; NDA, nalidixic acid; NFX, nadifloxacin; OXA, oxolinic acid; PFX, pefloxacin; PIA, pipemidic acid; PMA, piromidic acid; TFA, trifluoroacetic acid.

Conclusions

The analysis of some selected 4-quinolone drugs from the first and second generation since 2006 up till now has been fully covered by the comprehensive review. Different analytical techniques were summarized to facilitate the literature reviewing effort that many researchers perform to get up-to-date knowledge about this category of antibacterial agents. In spite of that numerous analytical tools were suggested for their determination, it was noticed that separation techniques constitute the main core for their quantitative measurement. This could be attributed to the fact that FQs exist in the form of a mixture in many samples whether it is per se pharmaceutical formulation, biological and environmental samples, cosmetics, animal tissues and feed-premix samples. CE and HPLC are two principal methods for the assay of such class. In spite of that CE is characterized by its high separation efficiency owing to the use of narrow tubes in the apparatus, besides its simple instrumentation which does not need experienced staff, HPLC is more spread because it is superior to CE in many aspects. Small pH changes affect a molecule’s charge and flow in CE; thus, small variations in pH have a greater impact in CE than in HPLC. Compared with HPLC, the control of the pH is critical in CE, and there are many factors, including temperature, that affect pH. Moreover, band broadening, poor repeatability and lower sensitivity are other limitations of CE. Thus, the reason of such numerous reports in this review applying HPLC for FQ assay could be inferred.

References

Adegoke, O. A.; Balogun, B. B. Spectrophotometric determination of some quinolones antibiotics following oxidation with cerium sulphate. Int. J. Pharm. Sci. Rev. Res.2010, 4, 1–10. Search in Google Scholar

Adrian, J.; Pinacho, D. G.; Granier, B.; Diserens, J.-M.; Baeza, S.; Marco, F.; Pilar, M. A multianalyte ELISA for immunochemical screening of sulfonamide, fluoroquinolone and β-lactam antibiotics in milk samples using class-selective bioreceptors. Anal. Bioanal. Chem.2008, 391, 1703–1712. Search in Google Scholar

Agrahari, V.; Bajpai, M.; Nanda, S. Development and validation of a stability indicating HPLC method for analysis of pefloxacin in bulk drug and tablet dosage form. Int. J. Pharm. Pharm. Sci.2013, 5, 263–268. Search in Google Scholar

Ajuan, L.; Hui-min, H. Simultaneous spectrophotometric determination of enoxacin and ciprofloxacin with aid of a chemometric approach. Ziran Kexueban2008, 29, 176–178. Search in Google Scholar

Alam, M.; Ferdous, T.; Kamruzzaman, M.; Lee, S. H.; Kim, Y. H.; Suh, J. K.; Chung, H. Y.; Suh, Y. S. Sensitive Chemiluminescence Determination of Enoxacin by Flow-Injection Analysis in Biological Fluids and Pharmaceutical Formulation Using Copper(II) in Luminol-H2O2. System Sensor Lett.2011, 9, 518–525. Search in Google Scholar

Amol, A. K.; Rabindra, N. K.; Ranjane, M. N.; Ranjane, P. Simultaneous estimation of nadifloxacin and mometasone furoate in topical cream by HPTLC method. Pharm. Chem.2010, 2, 25–30. Search in Google Scholar

Aodeng, G.; Liu, H.-M. Determination of ofloxacin by charge transfer spectrophotometry and its analytical application. Neimenggu Daxue Xuebao2006, 37, 513–515. Search in Google Scholar

Askal, H. F.; Refaat, I. H.; Darwish, I. A.; Marzouq, M. A. Evaluation of N-Bromosuccinimide as a new analytical reagent for the spectrophotometric determination of fluoroquinolone antibiotics. Chem. Pharm. Bull.2007, 55, 1551–1556. Search in Google Scholar

Askal, H. F.; Refaat, I. H.; Darwish, I. A.; Marzouq, M. A. A selective spectrophotometric method for determination of rosoxacin antibiotic using sodium nitroprusside as a chromogenic reagent. Spectrochim. Acta2008, 69, 1287–1291. Search in Google Scholar

Atta, N. F.; Galal, A.; Azab, S. M.; Ibrahim, A. H. Electrochemical sensor based on ionic liquid crystal modified carbon paste electrode in presence of surface active agents for enoxacin antibacterial drug. J. Electrochem. Soc.2015, 162, 1–10. Search in Google Scholar

Ayyagari, R. M.; Raghu, B. K.; Ngaji, A. V. Analytical method development and validation of nadifloxacin by high performance liquid chromatography. Int. J. Pharm. Pharm. Sci.2014, 9, 344–346. Search in Google Scholar

Bailac, S.; Barron, D.; Sanz-Nebot, V.; Barbosa, J. Determination of fluoroquinolones in chicken tissues by LC-coupled electrospray ionisation and atmospheric pressure chemical ionisation. J. Sep. Sci. 2006, 29, 131–136. Search in Google Scholar

Ball, P. Quinolone generations: natural history or natural selection?. J. Antimicrob. Chemother.2000, 46, 17–24. Search in Google Scholar

Basavaiah, K.; Prameela, H. C.; Somashekar, B. C. Spectrophotometric determination of pefloxacin mesylate in pharmaceuticals. Acta Pharm. 2007, 57, 221–230. Search in Google Scholar

Berendsen, B. J. A.; Elbers, I. J. W.; Stolker, A. A. M. Determination of the stability of antibiotics in matrix and reference solutions using a straightforward procedure applying mass spectrometric detection. Food Addit. Contam. 2011, 28, 1657–1666. Search in Google Scholar

Bertolino, F. A.; De Vito, I. E.; Messina, G. A.; Fernandez, H.; Raba, J. Microfluidic-enzymatic biosensor with immobilized tyrosinase for electrochemical detection of pipemidic acid in pharmaceutical samples. J. Electroanal. Chem.2011, 651, 204–210. Search in Google Scholar

Bian, J.-Y.; Xu, L.-Y. Fluorescence characteristics of the coordination complex formed among Eu(III), pefloxacin and EDTA and its application. Lihua Jianyan2007, 43, 580–581. Search in Google Scholar

Bian, J.-Y.; Xu, L.-Y.; Sun, J.-F. Fluorescence characteristics of pefloxacin mesylate in micellar systems and its application. Fenxi Kexue Xuebao2006, 22, 40–42. Search in Google Scholar

Biselli, S.; Schwalb, U.; Meyer, A.; Hartig, L. A multi-class, multi-analyte method for routine analysis of 84 veterinary drugs in chicken muscle using simple extraction and LC-MS/MS. Food Addit. Contam.2013, 30, 921–939. Search in Google Scholar

Bittencourt, M. S.; Martins, M. T.; De Albuquerque, F. G. S.; Barreto, F.; Hoff, R. High-throughput multiclass screening method for antibiotic residue analysis in meat using liquid chromatography-tandem mass spectrometry: a novel minimum sample preparation procedure. Food Addit. Contam.2012, 29, 508–516. Search in Google Scholar

Bober, K. Determination of Selected Quinolones and Fluoroquinolones by Use of TLC. Anal. Lett.2008, 41, 1909–1913. Search in Google Scholar

Bogialli, S.; D’Ascenzo, G.; Di Corcia, A.; Lagana, A.; Tramontana, G. Simple assay for monitoring seven quinolone antibacterials in eggs: extraction with hot water and liquid chromatography coupled to tandem mass spectrometry: laboratory validation in line with the European Union Commission Decision 657/2002/EC. J. Chromatogr. A2009, 1216, 794–800. Search in Google Scholar

Bohm, D. A.; Stachel, C. S.; Gowik, P. Multi-method for the determination of antibiotics of different substance groups in milk and validation in accordance with Commission Decision 2002/657/EC. J. Chromatogr. A2009, 1216, 8217–8223. Search in Google Scholar

Bohm, D. A.; Stachel, C. S.; Gowik, P. Validation of a multi-residue method for the determination of several antibiotic groups in honey by LC-MS/MS. J. Anal. Bioanal. Chem.2012, 403, 2943–2953. Search in Google Scholar

Borras, S.; Companyo, R.; Guiteras, J.; Bosch, J.; Medina, M.; Termes, S. Multiclass method for antimicrobial analysis in animal feeds by liquid chromatography–tandem mass spectrometry. Anal. Bioanal. Chem.2013, 405, 8475–8486. Search in Google Scholar

Boscher, A.; Guignard, C.; Pellet, T.; Hoffmann, L.; Bohn, T. Development of a multi-class method for the quantification of veterinary drug residues in feedingstuffs by liquid chromatography-tandem mass spectrometry. J. Chromatogr. A2010, 1217, 6394–6404. Search in Google Scholar

Bousova, K.; Senyuva, H.; Mittendorf, K. Quantitative multi-residue method for determination antibiotics in chicken meat using turbulent flow chromatography coupled to liquid chromatography–tandem mass spectrometry. J. Chromatogr. A2013, 1274, 19–27. Search in Google Scholar

Bu, M.-N.; Shi, Z.-H.; Kang, J.; Fan, C.-L.; Pang, G.-F. Simultaneous determination of 72 veterinary drugs in shrimp by modified QuEChERS and high performance liquid chromatography-tandem mass spectrometry. Fenxi Ceshi Xuebao2012, 31, 552–558. Search in Google Scholar

Burkin, M. A. Enzyme-linked immunosorbent assays of fluoroquinolones with selective and group specificities. Food Agr. Immunol. 2008, 19, 131–140. Search in Google Scholar

Cabanillas, A. G.; Caceres, M. I. R.; Canas, M. A. M.; Burguillos, J. M. O.; Diaz, T. G. Square wave adsorptive stripping voltametric determination of the mixture of nalidixic acid and its main metabolite (7-hydroxymethylnalidixic acid) by multivariate methods and artificial neural network. Talanta2007, 72, 932–940. Search in Google Scholar

Cai, Q.-H.; Xu, D.-F.; Ruan, L.-Q.; Li, C.-L. Study on new fluorescence analytical method for fleroxacin. Xiandai Huagong2012, 32, 98–101. Search in Google Scholar

Canada-Canada, F.; Espinosa-Mansilla, A.; Munoz de la Pena, A. Separation of fifteen quinolones by high performance liquid chromatography: application to pharmaceuticals and ofloxacin determination in urine. J. Sep. Sci.2007, 30, 1242–1249. Search in Google Scholar

Canada-Canada, F.; Espinosa-Mansilla, A.; Jimenez Giron, A.; Munoz de la Pena, A. Simultaneous determination of the residues of fourteen quinolones and fluoroquinolones in fish samples using liquid chromatography with photometric and fluorescence detection. Czech J. Food Sci.2012, 30, 74–82. Search in Google Scholar

Cao, Y.; Pang, G.; Zhang, J.; Shi, Y.; Li, X.; Fan, C.; Liu, Y.; Jia, G.; Liu, X.; Zhang, Y. Simultaneous determination of 14 quinolones residues in honey by high performance liquid chromatography-tandem mass spectrometry. Fenxi Ceshi Xuebao2008, 27, 1141–1146. Search in Google Scholar

Cao, H.; Chen, X.-Z.; Zhu, Y.; Li, Z.-G.; Wu, X.-G.; Zhu, Y. Determination of sulfonamides and quinolones in milk by QuEChERS and ultra performance liquid chromatographytandem mass spectrometry. Shipin Keji2013, 38, 323–329. Search in Google Scholar

Carretero, V.; Blasco, C.; Pico, Y. Multi-class determination of antimicrobials in meat by pressurized liquid extraction and liquid chromatography–tandem mass spectrometry. J. Chromatogr. A2008, 1209, 162–173. Search in Google Scholar

Chang, C.-S.; Wang, W-H.; Tsai, C.-E. Simultaneous determination of eleven quinolones antibacterial residues in marine products and animal tissues by liquid chromatography with fluorescence detection. Yaowu Shipin Fenxi2008, 16, 87–96. Search in Google Scholar

Chang, C.-S.; Wang, W.-H.; Tsai, C.-E. Simultaneous determination of 18 quinolone residues in marine and livestock products by liquid chromatography/tandem mass spectrometry. Yaowu Shipin Fenxi2010, 18, 87–97. Search in Google Scholar

Chang, B.; Xing, Y.; Gu, Y. Establishment of indirect competitive elisa method for detecting pefloxacin. Heilongjiang Xumu Shouyi2011, 9, 76–78. Search in Google Scholar

Chen, P.; Sun, H. An application of Ag(III) complex chemiluminescence system for the determination of enoxacin in capsule and biological fluid. Drug Test. Anal. 2010, 2, 24–27. Search in Google Scholar

Chen, S.-L.; Ding, F.; Liu, Y.; Zhao, H.-C. Electrochemiluminescence of terbium (III)-two fluoroquinolones-sodium sulfite system in aqueous solution. Spectrochim. Acta2006, 64A, 130–135. Search in Google Scholar

Chen, X.; Yao, X.; Shi, J. Determination of nine fluoroquinolone residues with high-performance liquid chromatography-mass spectrometry. Zhongguo Yufang Yixue Zazhi2008a, 9, 995–998. Search in Google Scholar

Chen, X.-H.; Yao, X.-P.; Li, X.-P. High – performance liquid chromatography coupled with tandem mass spectrometry for the determination of fluoroquinolones residues in chicken muscle. Zhongguo Weisheng Jianyan Zazhi2008b, 1273, 1239–1241. Search in Google Scholar

Chen, L.; Zhang, X.; Xu, Y.; Du, X.; Sun, X.; Sun, L.; Wang, H.; Zhao, Q.; Yu, A.; Zhang, H. Determination of fluoroquinolone antibiotics in environmental water samples based on magnetic molecularly imprinted polymer extraction followed by liquid chromatography–tandem mass spectrometry. Anal. Chim. Acta2010, 662, 31–38. Search in Google Scholar

Chen, X.-L.; He, C.-H.; Zhang, Z.-F. Determination of pefloxacin by fluorescence quenching of CdTe quantum dots. Fenxi Kexue Xuebao2012a, 28, 803–806. Search in Google Scholar

Chen, Z.; Zhong, Z.; Xia, Z.; Yang, F.; Mu, X. Separation of fluoroquinolones by MEKC modified with hydrophobic ionic liquid as a modifier. Chromatographia2012b, 75, 65–70. Search in Google Scholar

Chen, J.; Zheng, R.; Ji, S.; Wang, K. Determination of 19 quinolone antibiotics in cosmetics by ultra performance liquid chromatography. Fenxi Huaxue2013, 41, 931–935. Search in Google Scholar

Chiaochan, C.; Koesukwiwat, U.; Yudthavorasit, S.; Leepipatpiboon, N. Efficient hydrophilic interaction liquid chromatography–tandem mass spectrometry for the multiclass analysis of veterinary drugs in chicken muscle. Anal. Chim. Acta2010, 682, 117–129. Search in Google Scholar

Cho, H.-J.; Yi, H.; Cho, S. M.; Lee, D. G.; Cho, K.; Abd El-Aty, A. M.; Shim, J.-H.; Lee, S.-H.; Jeong, J.-Y.; Shin, H.-C. Single-step extraction followed by LC for determination of (fluoro)quinolone drug residues in muscle, eggs, and milk. J. Sep. Sci.2010, 33, 1034–1043. Search in Google Scholar

Chonan, T.; Fujimoto, T.; Inoue, M.; Tazawa, T.; Ogawa, H. [Multiresidue determination of quinolones in animal and fishery products by HPLC]. Shokuhin Eiseigaku Zasshi2008, 49, 244–248. Search in Google Scholar

Christodoulou, E. A.; Samanidou, V. F. Multiresidue HPLC analysis of ten quinolones in milk after solid phase extraction: validation according to the European Union Decision 2002/657/EC. J. Sep. Sci.2007, 30, 2421–2429. Search in Google Scholar

Christodoulou, E. A.; Samanidou, V. F.; Papadoyannis, I. N. Validation of an HPLC-UV method according to the European Union Decision 2002/657/EC for the simultaneous determination of 10 quinolones in chicken muscle and egg yolk. J. Chromatogr. B2007a, 859, 246–255. Search in Google Scholar

Christodoulou, E. A.; Samanidou, V. F.; Papadoyannis, I. N. Development and validation of an HPLC confirmatory method for residue analysis of ten quinolones in tissues of various food-producing animals, according to the European Union Decision 2002/657/EC. J. Sep. Sci.2007b, 30, 2676–2686. Search in Google Scholar

Christodoulou, E. A.; Samanidou, V. F.; Papadoyannis, I. N. Development of an HPLC multi-residue method for the determination of ten quinolones in bovine liver and porcine kidney according to the European Union Decision 2002/657/EC. J. Sep. Sci.2008, 31, 119–127. Search in Google Scholar

Collado-Sanchez, M. A.; Rambla-Alegre, M.; Carda-Broch, S.; Esteve-Romero, J. Simultaneous separation and determination of quinolones in pharmaceuticals by micellar liquid chromatograpHY. J. Liq. Chromatogr. Relat. Technol.2010, 33, 513–525. Search in Google Scholar

Cvijovic, M.; Di Marco, V.; Traldi, P.; Stankov, M. J.; Djurdjevic, P. Mass spectrometic study of speciation in aluminium-fluoroquinolone solutions. Eur. J. Mass Spectrom.2012, 18, 313–322. Search in Google Scholar

Darwish, I. A.; Refaat, I. H.; Askal, H. F.; Marzouok, M. A. Generic non extractive spectrophotometric method for determination of 4-quinolone antibiotic by formation of ion pair complexes with beta naphthol. J. AOAC Int.2006, 89, 334–340. Search in Google Scholar

David, M.-G.; Francisco, J. L.; Gámiz-Gracia, L.; García-Campana, A. M. Molecularly imprinted polymer as in-line concentrator in capillary electrophoresis coupled with mass spectrometry for the determination of quinolones in bovine milk samples. J. Chromatogr. A2014, 1360, 1–8. Search in Google Scholar

Deng, B.; Li, L.; Shi, A.; Kang, Y. Pharmacokinetics of pefloxacin mesylate in human urine using capillary electrophoresis electrochemiluminescence detection. J. Chromatogr. B2009, 877, 2585–2588. Search in Google Scholar

Deng, Y.; Gasilova, N.; Qiao, L.; Zhou, Y.-L.; Zhang, X-X; Girault, H. H. Highly sensitive detection of five typical fluoroquinolones in low-fat milk by field-enhanced sample injection-based CE in bubble cell capillary. Electrophoresis2014, 35, 3355–3362. Search in Google Scholar

Ding, F.; Zhao, H.; Jin, L.; Zheng, D. Study of the influence of silver nanoparticles on the second-order scattering and the fluorescence of the complexes of Tb(III) with quinolones and determination of the quinolones. Anal. Chim. Acta2006, 566, 136–143. Search in Google Scholar

Ding, T.; Shen, D.; Xu, J.; Wu, B.; Chen, H.; Shen, C.; Shen, W.; Zhao, Z.; Lian, H. Simultaneous determination of 19 quinolone residues in honey using high performance liquid chromatography tandem mass spectrometry. Sepu2009, 27, 34–38. Search in Google Scholar

Dinh, Q. T.; Alliot, F.; Moreau-Guigon, E.; Eurin, J.; Chevreuil, M.; Labadie, P. Measurement of trace levels of antibiotics in river water using on-line enrichment and triple-quadrupole LC-MS/MS. Talanta2011, 85, 1238–1245. Search in Google Scholar

Dorival-Garcia, N.; Zafra-Gomez, A.; Camino-Sanchez, F. J.; Navalon, A.; Vilchez, J. L. Analysis of quinolone antibiotic derivatives in sewage sludge samples by liquid chromatography-tandem mass spectrometry: comparison of the efficiency of three extraction techniques. Talanta2013a, 106, 104–118. Search in Google Scholar

Dorival-Garcia, N.; Zafra-Gomez, A.; Cantarero, S.; Navalon, A.; Vilchez, J. L. Simultaneous determination of 13 quinolone antibiotic derivatives in wastewater samples using solid-phase extraction and ultra performance liquid chromatography–tandem mass spectrometry. Microchem. J.2013b, 106, 323–333. Search in Google Scholar

Du, X.; Cao, X. Determination of enoxacin and its related substances by HPLC. Zhongguo Kangshengsu Zazhi2011, 36, 282–284. Search in Google Scholar

Du, W.; Yao, J. G.; Li, Y. Q.; Hashi, Y. Rapid determination of residual quinolones in honey samples by fast HPLC with an on-line sample pretreatment system. Am. J. Anal. Chem.2011, 2, 200–205. Search in Google Scholar

Du, J.-J.; Zhou, M.; Liu, Y.-Y.; Liu, Y.-M. Determination of enoxacin by flow-injection chemiluminescence. Fenxi Shiyanshi2012, 31, 19–22. Search in Google Scholar

Espinosa-Mansilla, A.; De la Pena, A. M.; Gomez, D. G.; Salinas Lopez, F. Determination of fluoroquinolones in urine and serum by using high performance liquid chromatography and multiemission scan fluorimetric detection. Talanta2006, 68, 1215–1221. Search in Google Scholar

Espinosa-Mansilla, A.; De la Pena, A. M.; Gomez, D. G. Determination of fluoroquinolones and nonsteroidal anti-inflammatory drugs in urine by extractive spectrophotometry and photoinduced spectrofluorimetry using multivariate calibration. Chem. Anal.2007, 52, 619–633. Search in Google Scholar

Evaggelopoulou, E. N.; Samanidou, V. F. HPLC confirmatory method development for the determination of seven quinolones in salmon tissue (Salmo salar L.) validated according to the European Union Decision 2002/657/EC. Food Chem.2013, 136, 479–484. Search in Google Scholar

Evaggelopoulou, E. N.; Samanidou, V. F.; Michaelidis, B.; Papadoyannis, I. Development and validation of an LC-DAD method for the routine analysis of residual quinolones in fish edible tissue and fish feed. Application to farmed gilthead sea bream following dietary administration. J. Liq. Chromatogr. Rel. Technol. 2014, 37, 2142–2161. Search in Google Scholar

Fan, Y.; Gan, X.; Li, S.; Qin, W. A rapid CE-potential gradient detection method for determination of quinolones. Electrophoresis2007, 28, 4101–4107. Search in Google Scholar

Fan, Y.; Tian, Z.; Qin, W. Quick and sensitive determination of fluoroquinolones by capillary electrophoresis–potential gradient detection. Anal. Lett.2009, 42, 1057–1069. Search in Google Scholar

Fan, G.-Y.; Yang, R.-S.; Jiang, J.-Q.; Chang, X.-Y.; Chen, J.-J.; Qi, Y.-H.; Wu, S.-X.; Yang, X.-F. Rapid and simple determination of sarafloxacin and difloxacin in beef by capillary 2 electrophoresis coupled with solid-phase extraction. Science2012, 13, 545–554. Search in Google Scholar

Fang, Z.-J.; Zhang, B.; Sun, D.-Q. Determination of fleroxacin in human plasma by HPLC with fluorescence detection and the pharmacokinetic study. J.Chin. Pharm. Sci.2007, 16, 257–261. Search in Google Scholar

Feas, X.; Fente, C. A.; Hosseini, S. V.; Cepeda, A. New near ultraviolet laser-induced native fluorescence detection coupled to HPLC to analyse residues of oxolinic acid and flumequine: a comparison with conventional xenon flash lamp. J. Food2009, 7, 15–21. Search in Google Scholar

Francisco, L. J.; Garcia-Campana, A. M.; Ales-Barrero, F.; Bosque-Sandra, J. M.; Garcia-Ayuso, L. Multiresidue method for the determination of quinolone antibiotics in bovine raw milk by capillary electrophoresis-tandem mass spectrometry. Anal. Chem. 2006, 78, 7665–7673. Search in Google Scholar

Francisco, L. J.; Del Olmo-Iruela, M.; Garcia-Campana, A. M. On-line anion exchange solid-phase extraction coupled to liquid chromatography with fluorescence detection to determine quinolones in water and human urine. J. Chromatogr. A2013, 1310, 91–97. Search in Google Scholar

Freccero, M.; Fasani, E.; Mella, M.; Manet, I.; Albini, A. Modeling the photochemistry of the reference phototoxic drug lomefloxacin by steady-state and time-resolved experiments, and DFT and post-HF calculations. Chem. Eur. J.2008, 14, 653–663. Search in Google Scholar

Fujita, M.; Tamura, W.; Tozawa, T.; Kometani, T. [Application of simultaneous determination method of residual veterinary drugs to processed foods]. Shokuhin Eiseigaku Zasshi2008, 49, 416–421. Search in Google Scholar

Gajda, A.; Posyniak, A.; Zmudzki, J.; Gbylik, M.; Bladek, T. Determination of (fluoro)quinolones in eggs by liquid chromatography with fluorescence detection and confirmation by liquid chromatography-tandem mass spectrometry. Food Chem. 2012, 135, 430–439. Search in Google Scholar

Galarini, R.; Fioroni, L.; Angelucci, F.; Tovo, G. R.; Cristofani, E. Modifications of the Molteno implant and implant procedure. J. Chromatogr. A2009, 1216, 8158–8164. Search in Google Scholar

Gandhi, L.; Sekhon, B. S. Complexation equilibria of nalidixic acid and norfloxacin with proton and metal ions in aqueous-organic mixtures. J.Indian Council Chem. 2007, 24, 68–72. Search in Google Scholar

Gao, D. Determination of enoxacin gluconate and related substances in enoxacin gluconate injection by HPLC. Zhongguo Yaoshi2007, 21, 412–414. Search in Google Scholar

Gao, L.; Shi, Y.; Li, W.; Liu, J.; Cai, Y. [Determination of 22 antibiotics in environmental water samples using high performance liquid chromatography-electrospray ionization tandem mass spectrometry]. Sepu2010, 28, 491–497. Search in Google Scholar

Gao, W.; Chen, G.; Chen, Y.; Zhang, X.; Yin, Y.; Hu, Z. Application of single drop liquid-liquid-liquid microextraction for the determination of fluoroquinolones in human urine by capillary electrophoresis. J. Chromatogr. B2011a, 879, 291–295. Search in Google Scholar

Gao, S.-Q.; Jin, H.-Y.; You, J.-Y.; Ding, Y.; Zhang, N.; Wang, Y.; Ren, R.-B.; Zhang, R.; Zhang, H.-Q. Ionic liquid-based homogeneous liquid-liquid microextraction for the determination of antibiotics in milk by high-performance liquid chromatography. J. Chromatogr. A2011b, 1218, 7254–7263. Search in Google Scholar

Gao, F.; Zhao, Y.; Shao, B.; Zhang, J. [Determination of residues of pesticides and veterinary drugs in milk by ultra performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry]. Sepu2012, 30, 560–567. Search in Google Scholar

Garcia, M. D. G.; Gallegos, A. B.; Valverde, R. S.; Galera, M. M. Determination of (fluoro)quinolones in environmental water using online preconcentration with column switching linked to large sample volumes and fluorescence detection. J. Sep. Sci.2012, 35, 823–831. Search in Google Scholar

Gauhar, S.; Ali, S. A.; Shoaib, H.; Naqvi, S. B. S.; Muhammad, I. N. Development and validation of a HPLC method for determination of pefloxacin in tablet and human plasma. Iran. J. Basic Med. Sci.2009, 12, 33–42. Search in Google Scholar

Gbylik, M.; Posyniak, A.; Mitrowska, K.; Bladek, T.; Zmudzki, J. Multi-residue determination of antibiotics in fish by liquid chromatography-tandem mass spectrometry. Food Addit. Contam.2013, 30, 940–948. Search in Google Scholar

Geffken, D.; Salem, H. Spectrofluorimetric study of the charge-transfer complexation of certain fluoroquinolones with 2,3,5,6-tetrafluoro-p-bezoquinone. Am. J. Appl. Sci.2006, 3, 1952–1960. Search in Google Scholar

Gracia-Lor, E.; Sancho, J. V.; Hernandez, F. Multi-class determination of around 50 pharmaceuticals, including 26 antibiotics, in environmental and wastewater samples by ultra-high performance liquid chromatography-tandem mass spectrometry. J. Chromatogr. A2011, 1218, 2264–2275. Search in Google Scholar

Gros, M.; Rodriguez-Mozaz, S.; Barcelo, D. Rapid analysis of multiclass antibiotic residues and some of their metabolites in hospital, urban wastewater and river water by ultra-high-performance liquid chromatography coupled to quadrupole-linear ion trap tandem mass spectrometry. J. Chromatogr. A2013, 1292, 173–188. Search in Google Scholar

Gu, L.; Zhang, M.; He, Y.-M. Differential pulse voltammetric determination of enoxacin with polythionine modified carbon paste electrode. Huaxue Fence2013, 49, 420–424. Search in Google Scholar

Gulyaev, I. V.; Revel’skii, A. I. Analyssis of pharmaceutical substances by reaction gas chromatography/mass spectrometry J. Anal. Chem.2010, 65, 1341–1346. Search in Google Scholar

Han, Q.; Wang, M.; Yang, X.; Yang, N. Determination of pefloxacin in tablet, human urine and plasma by resonance Rayleigh scattering method. Zhongguo Kangshengsu Zazhi2011, 36, 366–369. Search in Google Scholar

Han, T.-T.; Ling, J.; Dai, X.-L.; Lei, Y.; Li, R.-P. Interactions between heavy metal ions and enoxacin by fluorescence spectroscopy. Huanjing Kexue Yu Jishu2012, 35, 117–119. Search in Google Scholar

Hassouan, M. K.; Ballesteros, O.; Taoufiki, J.; Vilchez, J. L.; Cabrera-Aguilera, M.; Navalon, A. Multiresidue determination of quinolone antibacterials in eggs of laying hens by liquid chromatography with fluorescence detection. J. Chromatogr. B2007a, 852, 625–630. Search in Google Scholar

Hassouan, M. K.; Ballesteros, O.; Zafra, A.; Vilchez, J. L.; Navalon, A. Multiresidue method for simultaneous determination of quinolone antibacterials in pig kidney samples by liquid chromatography with fluorescence detection. J. Chromatogr. B2007b, 859, 282–288. Search in Google Scholar

He, H.-B.; Lv, X.-X.; Yu, Q.-W.; Feng, Y.-Q. Multiresidue determination of (fluoro)quinolone antibiotics in chicken by polymer monolith microextraction and field-amplified sample stacking procedures coupled to CE-UV. Talanta2010a, 82, 1562–1570. Search in Google Scholar

He, Q.; Kong, X.-H.; Li, J.-H.; Yue, A.-S.; Wu, S.-M. Simultaneous determination of nitroimidazoles, sulfonamides and quinolones residues in honey by ultra performance liquid chromatography with electrospray ionization tandem mass spectrometric detection. Fenxi Shiyanshi2010b, 29, 61–65. Search in Google Scholar

He, Q.; Kong, X.-H.; Li, J.-H.; Yue, A.-S.; Ma, Y.-L. Simultaneous determination of 15 quinolones residues in honey by ultra performance liquid chromatography with electrospray ionization tandem mass spectrometric detection. Fenxi Shiyanshi2010c, 29, 101–105. Search in Google Scholar

Hermo, M. P.; Barron, D.; Barbosa, J. Development of analytical methods for multiresidue determination of quinolones in pig muscle samples by liquid chromatography with ultraviolet detection, liquid chromatography-mass spectrometry and liquid chromatography-tandem mass spectrometry. J. Chromatogr. A2006, 1104, 132–139. Search in Google Scholar

Hermo, M. P.; Barron, D.; Barbosa, J. Determination of multiresidue quinolones regulated by the European Union in pig liver samples. High-resolution time-of-flight mass spectrometry versus tandem mass spectrometry detection. J. Chromatogr. A2008, 1201, 1–14. Search in Google Scholar

Hermo, M. P.; Nemutlu, E.; Barbosa, J.; Barron, D. Multiresidue determination of quinolones regulated by the European Union in bovine and porcine plasma. Application of chromatographic and capillary electrophoretic methodologies. Biomed. Chromatogr.2011, 25, 555–569. Search in Google Scholar

Hernando, M. D.; Mezcua, M.; Suarez-Barcena, J. M.; Fernandez-Alba, A. R. Liquid chromatography with time-of-flight mass spectrometry for simultaneous determination of chemotherapeutant residues in salmon. Anal. Chim. Acta2006, 562, 176–184. Search in Google Scholar

Herrera-Herrera, A. V.; Hernandez-Borges, J.; Rodriguez-Delgado, M. A. Ionic liquids as mobile phase additives for the high-performance liquid chromatographic analysis of fluoroquinolone antibiotics in water samples. Anal. Bioanal. Chem. 2008, 392, 1439–1446. Search in Google Scholar

Herrera-Herrera, A. V.; Hernandez-Borges, J.; Rodriguez-Delgado, M. A. Fluoroquinolone antibiotic determination in bovine, ovine and caprine milk using solid-phase extraction and high-performance liquid chromatography-fluorescence detection with ionic liquids as mobile phase additives. J. Chromatogr. A2009, 1216, 7281–7287. Search in Google Scholar

Herrera-Herrera, A. V.; Hernandez-Borges, J.; Rodriguez-Delgado, M. A.; Herrero, M.; Cifuentes, A. Determination of quinolone residues in infant and young children powdered milk combining solid-phase extraction and ultra-performance liquid chromatography-tandem mass spectrometry. J. Chromatogr. A2011, 1218, 7608–7614. Search in Google Scholar

Herrera-Herrera, A. V.; Hernandez-Borges, J.; Borges-Miquel, T. M.; Rodriguez-Delgado, M. A. Dispersive liquid-liquid microextraction combined with ultra-high performance liquid chromatography for the simultaneous determination of 25 sulfonamide and quinolone antibiotics in water samples. J. Pharm. Biomed. Anal.2013, 75, 130–137. Search in Google Scholar

Hou, X.; Dong, X.; Yang, G.; Hu, Q.; Han, Y. Study on determination of seven fluoroquinolones in pork sample by rapid high performance liquid chromatography. Yunnan Minzu Daxue Xuebao2007, 16, 225–227. Search in Google Scholar

Huet, A-C; Charlier, C.; Tittlemier, S. A.; Singh, G.; Benrejeb, S.; Delahaut, P. Simultaneous determination of (fluoro)quinolone antibiotics in kidney, marine products, eggs, and muscle by enzyme-linked immunosorbent assay (ELISA). J. Agric. Food. Chem.2006, 54, 2822–2827. Search in Google Scholar

Ibarra, I. S.; Rodriguez, J. A.; Paez-Hernandez, M. E.; Santos, E. M.; Jose. M. M. Determination of quinolones in milk samples using a combination of magnetic solid-phase extraction and capillary electrophoresis. Electrophoresis2012, 33, 2041–2048. Search in Google Scholar

Irgi, E. P.; Geromichalos, G. D.; Balala, S.; Kljun, J.; Kalogiannis, S.; Papadopoulos, A.; Psomas, I. T. G. Cobalt(II) complexes with the quinolone antimicrobial drug oxolinic acid: structure and biological perspectives. RSC Adv.2015, 5, 36353–36367. Search in Google Scholar

Iwasaki, Y.; Ito, T.; Kitamura, W.; Kato, M.; Kodaira, T.; Horie, M.; Ito, R.; Saito, K.; Nakazawa, H. Analysis of fluoroquinolones in meat samples by enzyme-linked immunosorbent assay and HPLC. Bunseki Kagaku2006, 55, 943–948. Search in Google Scholar

Jiang, J.; Zhang, H.; Wang, Z. Multiresidue determination of sarafloxacin, difloxacin, norfloxacin, and pefloxacin in fish using an enzyme-linked immunosorbent assay. Procedia Environ. Sci.2011, 8, 301–306. Search in Google Scholar

Jiang, W.; Wang, Z.; Beier, R. C.; Jiang, H.; Wu, Y.; Shen, J. Simultaneous determination of 13 fluoroquinolone and 22 sulfonamide residues in milk by a dual-colorimetric enzyme-linked immunosorbent assay. Anal. Chem.2013, 85, 1995–1999. Search in Google Scholar

Jiao, H.; Xu, F.; Tian, Y.; Zhang, Z. Fluoroquinolones by triple quadrupole mass spectrometer. Zhongguo Kangshengsu Zazhi2009a, 34, 344–347. Search in Google Scholar

Jiao, H.; Xu, F.; Tian, Y.; Zhang, Z. Determination of fluoroquinolones multi-residues in milk by solid- phase extraction-LC-MS/MS. Zhongguo Yaoke Daxue Xuebao2009b, 40, 62–66. Search in Google Scholar

Jimenez, V.; Companyo, R.; Guiteras, J. Validation of a method for the analysis of nine quinolones in eggs by pressurized liquid extraction and liquid chromatography with fluorescence detection. Talanta2011a, 85, 596–606. Search in Google Scholar

Jimenez, V.; Rubies, A.; Centrich, F.; Companyo, R.; Guiteras, J. Development and validation of a multiclass method for the analysis of antibiotic residues in eggs by liquid chromatography-tandem mass spectrometry. J. Chromatogr. A2011b, 1218, 1443–1451. Search in Google Scholar

Jo, M. R.; Kim, P. H.; Lee, H. J.; Lee, T. S. A new analytical method for fluoroquinolones in fisheries products by high performance liquid chromatography. Han’guk Susan Hakhoechi2006, 39, 59–65. Search in Google Scholar

Juan-Garcia, A.; Font, G.; Pico, Y. Determination of quinolone residues in chicken and fish by capillary electrophoresis-mass spectrometry. Electrophoresis2006, 27, 2240–2249. Search in Google Scholar

Junza, A.; Dorival-García, N.; Zafra-Gómez, A.; Barrón, D.; Ballesteros, O.; Barbosa, J.; Navalón, A. Multiclass method for the determination of quinolones and β-lactams, in raw cow milk using dispersive liquid-liquid microextraction and ultra high performance liquid chromatography-tandem mass spectrometry. J. Chromatogr. A2014, 1356, 10–22. Search in Google Scholar

Kai, S.; Akaboshi, T.; Fujimaki, T.; Itoh, S.-I.; Kanazawa, H. Screening method for veterinary drugs in livestock foods and fish by liquid chromatography/tandem mass spectrometry. Bunseki Kagaku2007, 56, 1105–1113. Search in Google Scholar

Kalantre, U. L.; Pishwikar, S. A. Development and validation of multiwavelength method for simultaneous estimation of nadifloxacin and ibuprofen in formulated hydrogel. Int. J. Pharm Tech. Res.2012, 4, 1575–1580. Search in Google Scholar

Kang, L.; Liu, H.-H.; Li, Y.; Liu, G.-H. Determination of (fluoro) quinolones residues in aquatic products by high performance liquid chromatography/tandem mass spectrometry. Zhongguo Weisheng Jianyan Zazhi2008, 18, 1941–1944. Search in Google Scholar

Kantiani, L.; Farre, M.; Barcelo, D. Rapid residue analysis of fluoroquinolones in raw bovine milk by online solid phase extraction followed by liquid chromatography coupled to tandem mass spectrometry. J. Chromatogr. A2011, 1218, 9019–9027. Search in Google Scholar

Karageorgou, E.; Myridakis, A.; Stephanou, E. G.; Samanidou, V. Multiresidue LC-MS/MS analysis of cephalosporins and quinolones in milk following ultrasound-assisted matrix solid-phase dispersive extraction combined with the quick, easy, cheap, effective, rugged, and safe methodology. J. Sep. Sci.2013, 36, 2020–2027. Search in Google Scholar

Karbiwnyk, C. M.; Carr, L. E.; Turnipseed, S. B.; Andersen, W. C.; Miller, K. E. Determination of quinolone resi. Anal. Chim. Acta2007, 596, 257–263. Search in Google Scholar

Karim, M. M.; Lee, S. H.; Lee, H. S.; Bae, Z. U.; Choi, K. H. A batch chemiluminescence determination of enoxacin using a tris-(1,10-phenanthroline)ruthenium(II)-cerium(IV) system. J. Fluoresc.2006, 16, 535–540. Search in Google Scholar

Kaufmann, A.; Walker, S. Post-run target screening strategy for ultra high performance liquid chromatography coupled to Orbitrap based veterinary drug residue analysis in animal urine. J. Chromatogr. A2013, 1292, 104–110. Search in Google Scholar

Kaura, K.; Kumara, A.; Malika, A. K.; Singha, B.; Rao, A. L. Spectrophotometric methods for the determination of fluoroquinolones: a review. J. Crit. Rev. Anal. Chem.2008, 38, 2–18. Search in Google Scholar

Kulkarni, A. A.; Nanda, R. K.; Ranjane, M. N.; Ranjane, P. N. Spectrophotometric estimation of nadifloxacin in pharmaceutical dosage form. J. Pharm. Tech.2010, 3, 429–431. Search in Google Scholar

Kumar, A.; Malik, A. K.; Tewary, D. K.; Singh, B. Gradient HPLC of antibiotics in urine, ground water, chicken muscle, hospital wastewater, and pharmaceutical samples using C-18 and RP-amide columns. J. Sep. Sci.2008, 31, 294–300. Search in Google Scholar

Kumar, A.; Sinha, S.; Agarwal, S. P.; Ali, J.; Ahuja, A.; Baboota, S. Validated stability-indicating thin layer chromatographic determination of nadifloxacin in microemuision and bulk drug formulations. Yaowu Shipin Fenxi2010, 18, 358–365. Search in Google Scholar

Kumar, S. Y.; Sivaprasad, P.; Ashok Kumar, A. RP-HPLC method development and validation for simultaneous quantitative estimation of metronidazole and nalidixic acid in tablets. Int. J. Pharmacy Pharm. Sci.2015, 7, 367–371. Search in Google Scholar

Kobayashi, T.; Homma, M.; Momo, K.; Kobayashi, D.; Kohda, Y. A simple chromatographic method for determining norfloxacin and enoxacin in pharmacokinetic study assessing CYP1A2 inhibition. Biomed. Chromatogr. 2011, 25, 435–438. Search in Google Scholar

Lee, S.; Shim, Y.; Kim, H.; Shin, D. Multiresidue determination of quinolones in porcine, chicken, and bovine muscle using liquid chromatography with fluorescence detection. Food Sci. Biotech.2009, 18, 978–984. Search in Google Scholar

Lesher, G. Y.; Foelich, E. J.; Gruett, M. D.; Baily, J. H.; Brundage, P. R. 1,8-naphthyridine derivatives. A new class of chemotherapeutic agents. J. Med. Pharma. Chem.1962, 91, 1063–1065. Search in Google Scholar

Li, A.; Song, Z. Spectrofluorimetric determination of human serum albumin using terbium-danofloxacin probe. Sci. World J.2014, 14, 7–15. Search in Google Scholar

Li, S.-F.; Wei, X.-W. Chemiluminescence determination of enoxacin with luminol-H2O2-manganese tetrasulfonatophthalocyanine system. Guangpu Shiyanshi2006, 23, 944–947. Search in Google Scholar

Li, H.-k.; Zhang, M.-H. The spectrophotometric determination of enoxacin based on the charge transfer reaction between enoxacin and alizarin red. Huaxue Fence2008, 44, 45–46. Search in Google Scholar

Li, Y.; Yin, L.; Hu, C. Related substances and assay method of pefloxacin mesylate injection by high performance liquid chromatography. Zhongguo Yaopin Biaozhun2006a, 7, 14–19. Search in Google Scholar

Li, H.; Kijak, P. J.; Turnipseed, S. B.; Cui, W. Analysis of veterinary drug residues in shrimp: a multi-class method by liquid chromatography-quadrupole ion trap mass spectrometry. J. Chromatogr. B2006b, 836, 22–38. Search in Google Scholar

Li, Y.; Ji, B.; Chen, W.; Liu, L.; Xu, C.; Peng, C.; Wang, L. Production of new class-specific polyclonal antibody for determination of fluoroquinolones antibiotics by indirect competitive ELISA. Food Agr. Immunol. 2008a, 19, 251–264. Search in Google Scholar

Li, L.; Shi, A.; Deng, B. Determination of pefloxacin mesylate in human urine by capillary electrophoresis with electrochemiluminescence. Fenxi Ceshi Xuebao2008b, 27, 718–720. Search in Google Scholar

Li, Y.; Hao, X.; Ji, B.; Xu, C.; Shen, C.; Ding, T. Simultaneous and high sensitivity determination of nineteen kinds of quinolone multiresidues in animal food by HPLC-ESI-MS/MS. Shipin Kexue2008c, 29, 502–506. Search in Google Scholar

Li, S.-F.; Wei, X.-W.; Zhu, C.-Q.; Xiao, Y.-L.; Chen, H.-Q.; Zhou, Y.-H. Flow injection chemiluminescence determination of enoxacin by the reaction system of luminol and potassium ferricyanide. Huaxue Fence2008d, 44, 247–248. Search in Google Scholar

Li, X.-L.; Li, X.; Zeng, J.; Liu, Y.-Q. Determination of content and related substance in pefloxacin mesilate tablets by HPLC. Erke Yaoxue Zazhi2009a, 15, 49–51. Search in Google Scholar

Li, R.-F.; Wu, H.; Zong, M.-H. Simultaneous separation and detection of six quinolones by capillary zone electrophoresis. Xiandai Shipin Keji2009b, 25, 1468–1471. Search in Google Scholar

Li, Y. L.; Hao, X. L.; Ji, B. Q.; Xu, C. L.; Chen, W.; Shen, C. Y.; Ding, T. Rapid determination of 19 quinolone residues in spiked fish and pig muscle by high-performance liquid chromatography (HPLC) tandem mass spectrometry. Food Addit. Contam.2009c, 26, 306–313. Search in Google Scholar

Li, C.; Jiang, H.-Y.; Wu, Y.-L.; Wang, Z.-H.; Zhao, S.-J.; Li, J.-C.; Shi, Y.-X.; Shen, J.-Z. Determination of multiclass drug residues in animal muscle tissues by high performance liquid chromatography with fluorescence and ultraviolet detection. Fenxi Huaxue2009d, 37, 1102–1106. Search in Google Scholar

Li, W.; Shi, Y.; Gao, L.; Liu, J.; Cai, Y. Simultaneous determination of quinolones, sulfonamides and macrolides in fish samples using accelerated solvent extraction followed by high performance liquid chromatography-electrospray ionization tandem mass spectrometry. Fenxi Ceshi Xuebao2010, 29, 987–992. Search in Google Scholar

Li, D.; Yang, Q.; Wang, Z.; Su, R.; Xu, X.; Zhang, H. Determination of fluoroquinolones in blood by matrix solid-phase dispersion extraction and CE. J. Sep. Sci.2011, 34, 822–829. Search in Google Scholar

Li, X.; Zhao, Y.; Liu, Y.; Jin, Y.; Jiang, S.; Xu, Y.; Zhong, Y.; Yu, L.; Zhou, J. Simultaneous analysis of 29 veterinary drugs residues in feed by ultra performance liquid chromatography-mass Spectrometry. Xiandai Yiqi2012, 18, 78–82. Search in Google Scholar

Lian, S.; Wang, G.; Zhou, L.; Yang, D. Fluorescence spectroscopic analysis on interaction of fleroxacin with pepsin. Luminescence2013, 28, 967–972. Search in Google Scholar

Liang, Y.-D.; Gao, W.; Song, J.-F. Electrochemiluminescence determination of pipemidic acid using sulfite as energy transfer mediator. Bioorg. Med. Chem. Lett.2006a, 16, 5328–5333. Search in Google Scholar

Liang, L.-H.; Du, L.-M.; Wang, J.-P.; Zhuo, J.; Chen, F.-Y. Determination of trace pefloxacin by catalytic kinetics spectrofluorometry. Fenxi Kexue Xuebao2006b, 22, 594–596. Search in Google Scholar

Liao, L.; Cao, X.-M.; Du, L.-M.; Wu, H. Determination of pefloxacin by terbium (III) ion fluorescence probe sensitized by the surfactant. Fenxi Kexue Xuebao2008a, 24, 221–223. Search in Google Scholar

Liao, L.; Rao, Y.; Yang, G.-X.; Huang, X.-H.; Zeng, Z.-L.; Zeng, Z.-L. Development of HPLC method for multiresidue determination of 12 quinolones in egg. Zhongguo Nongye Kexue2008b, 41, 2419–2424. Search in Google Scholar

Lin, B. Multi-residue determination of 11 quinolones in chicken muscle by high performance liquid chromatography with fluorescence detection. Sepu2009, 27, 206–210. Search in Google Scholar

Liu, P.; Jiang, N.; Wang, H. Simultaneous determination of sulfonamides and fluoroquinolones residues in pork by solid-phase extraction and high performance liquid chromatography. Huaxue Tongbao2006, 69, 572–576. Search in Google Scholar

Liu, P.; Jiang, N.; Wang, Y.; Yan, L. Fast determination of polybrominated diphenyl ethers in human milk using gas chromatography-negative chemical ionization/mass spectrometry. Sepu2008a, 26, 348–352. Search in Google Scholar

Liu, Z.; Xu, S.-k.; Sun, S.-L.; Yang, D.-Z. Determination of pipemidic acid by time-resolved fluorescence using europium (III) ion as fluorescent probe. Fenxi Shiyanshi2008b, 27, 1–4. Search in Google Scholar

Liu, Q.; Fan, Y.; Qin, W. The use of protein in quick determination of quinolones by capillary electrophoresis-conductivity measurement. Ziran Kexueban2008c, 44, 396–399. Search in Google Scholar

Liu, Y.; Leng, K.; Wang, Q.; Wang, Z.; Sun, W.; Tan, Z.; Guo, M. Determination of flumequine and oxolinic acid in eel with HPLC method. Shanghai Haiyang Daxue Xuebao2009, 18, 332–337. Search in Google Scholar

Liu, Y.-M.; Shi, Y.-M.; Liu, Z.-L. Determination of enoxacin and ofloxacin by capillary electrophoresis with electrochemiluminescence detection in biofluids and drugs and its application to pharmacokinetics. Biomed. Chromatogr. 2010, 24, 941–947. Search in Google Scholar

Liu, Y.; Zhao, Y.; Zhang, P.-Y.; Jin, Y.; Jiang, S.; Li, X.-D.; Xu, Y.-H.; Zhong, Y.; Yu, L.; Zhou, J.-N. Determination of 29 veterinary drugs in the compound premix feed by ultra performance liquid chromatographytandem mass spectrometry. Fenxi Shiyanshi2012a, 31, 77–81. Search in Google Scholar

Liu, P.-Y.; Shen, J.; Liu, L. Determination of fluoroquinolones in grass carp by high performance liquid chromatography-ion trap mass spectrometry using mixed-templates imprinted polymer extraction. Fenxi Huaxue2012b, 40, 693–698. Search in Google Scholar

Liu, Y.; Zhao, Y.; Li, X.; Jin, Y.; Jiang, S.; Xu, Y.; Zhong, Y.; Zeng, F.; Yu, L.; Zhou, J. Determination of multi-veterinary drugs in the concentrated feed by ultra performance liquid chromatography-tandem mass spectrometry. Huaxue Tongbao2013, 76, 157–162. Search in Google Scholar

Lohne, J. J.; Andersen, W. C.; Clark, S. B.; Turnipseed, S. B.; Madson, M. R. Laser diode thermal desorption mass spectrometry for the analysis of quinolone antibiotic residues in aquacultured seafood. Rapid Commun. Mass Spectrom.2012, 26, 2854–2864. Search in Google Scholar

Lombardo-Agüí, M.; Garcia-Campana, A. M.; Gamiz-Gracia, L.; Cruces-Blanco, C. Determination of quinolones of veterinary use in bee products by ultra-high performance liquid chromatography-tandem mass spectrometry using a QuEChERS extraction procedure. Talanta2012, 93, 193–199. Search in Google Scholar

Lombardo-Agüí, M.; Cruces-Blanco, C.; García-Campaña, A. M.; Gámiz-Gracia, L. Multiresidue analysis of quinolones in water by ultra-high perfomance liquid chromatography with tandem mass spectrometry using a simple and effective sample treatment. J. Sep. Sci.2014, 37, 2145–2152. Search in Google Scholar

Lopes, R. P.; Reyes, R. C.; Romero-Gonzalez, R.; Frenich, A. G.; Vidal, J. L. M. Development and validation of a multiclass method for the determination of veterinary drug residues in chicken by ultra high performance liquid chromatography-tandem mass spectrometry. Talanta2012a, 89, 201–208. Search in Google Scholar

Lopes, R. P.; Reyes, R. C.; Romero-Gonzalez, R.; Vidal, J. L. M.; Frenich, A. G. Multiresidue determination of veterinary drugs in aquaculture fish samples by ultra high performance liquid chromatography coupled to tandem mass spectrometry. J. Chromatogr. B2012b, 895–896, 39–47. Search in Google Scholar

Lopez-Serna, R.; Perez, S.; Ginebreda, A.; Petrovic, M.; Barcelo, D. Fully automated determination of 74 pharmaceuticals in environmental and waste waters by online solid phase extraction-liquid chromatography-electrospray-tandem mass spectrometry. Talanta2010, 83, 410–424. Search in Google Scholar

Lopez-Serna, R.; Petrovic, M.; Barcelo, D. Direct analysis of pharmaceuticals, their metabolites and transformation products in environmental waters using on-line TurboFlow™ chromatography-liquid chromatography-tandem mass spectrometry. J. Chromatogr. A2012, 1252, 115–129. Search in Google Scholar

Lu, S.; Zhang, Y.; Liu, J.; Zhao, C.; Liu, W.; Xi, R. Preparation of anti-pefloxacin antibody and development of an indirect competitive enzyme-linked immunosorbent assay for detection of pefloxacin residue in chicken liver. J. Agric. Food. Chem.2006, 54, 6995–7000. Search in Google Scholar

Lu, K.; Sui, M.; Gao, N. Simultaneous determination of 19 antibiotics in environmental water samples using solid phase extraction-ultra pressure liquid chromatography coupled with tandem mass spectrometry. Fenxi Ceshi Xuebao2010, 29, 1209–1214. Search in Google Scholar

Ma, J.-W.; Yan, D.-L. Determination of seven FQs in chicken by HPLC. Zhongguo Weisheng Jianyan Zazhi2008, 18, 595–596, 606. Search in Google Scholar

Ma, H.-Y.; Gao, R.; Wang, H.-L. FI-fluorophotometric determination of enoxacin. Lihua Jianyan2011, 47, 177–179. Search in Google Scholar

Maheshwari, R. K.; Chaturvedi, S. C.; Jain, N. K. Novel spectrophotometric estimation of some poorly water soluble drugs using hydrotropic solubilizing agents. Ind. J. Pharm. Sci.2006, 68, 195–198. Search in Google Scholar

Maheshwari, K.; Priya, G.; Akshay, F.; Sugandha, S. New spectrophotometric analysis of gatifloxacin tablets utilizing mixed solvency concept. Int. J. Pharm. Chem. Anal.2015, 2, 42–45. Search in Google Scholar

Martinez, M.; McDermott, P.; Walker, R. Pharmacology of the fluoroquinolones: a perspective for the use in domestic animals. Vet. J.2006, 172, 10–28. Search in Google Scholar

Meng, Y.; Zhang, M.-Q.; Wang, J.; Tan, X.-H.; Wu, G.-H. HPLC determination of residual amounts of 7 veterinary drugs in aquatic products. Huaxue Fence2012, 48, 543–546. Search in Google Scholar

Mi, T.; Wang, Z.; Eremin, S. A.; Shen, J.; Zhang, S. Simultaneous determination of multiple (fluoro)quinolone antibiotics in food samples by a one-step fluorescence polarization immunoassay. J. Agric. Food. Chem.2013, 61, 9347–9355. Search in Google Scholar

Misra, M.; Misra, A. K.; Panpalia, G. M. Development and validation of spectrophotometric method for estimation of pefloxacin mesylate in bulk and dosage form. Pharmbit2008, 18, 108–114. Search in Google Scholar

Mitani, K.; Kataoka, H. Determination of fluoroquinolones in environmental waters by in-tube solid-phase microextraction coupled with liquid chromatography–tandem mass spectrometry. Anal. Chim. Acta2006, 562, 16–22. Search in Google Scholar

Murillo Pulgarin, J. A.; Alanon Molina, A.; Boras, N. Application of non-linear angle synchronous spectrofluorimetry to the determination of complex mixtures of drugs in urine: a comparative study. Spectrochim Acta A Mol Biomol Spectrosc.2012, 98, 190–198. Search in Google Scholar

Na, G.; Gu, J.; Ge, L.; Zhang, P.; Wang, Z.; Liu, C.; Zhang, L. Detection of 36 antibiotics in coastal waters using high performance liquid chromatography-tandem mass spectrometry. Chin. J. Oceanol. Limnol.2011, 29, 1093–1102. Search in Google Scholar

Ni, Y.; Wang, Y.; Kokot, S. Multicomponent kinetic spectrophotometric determination of pefloxacin and norfloxacin in pharmaceutical preparations and human plasma samples with the aid of chemometrics. Spectrochim. Acta2008, 70, 1049–1059. Search in Google Scholar

Norouzi, P.; Ganjali, M. R.; Larijani, B.; Karamdoust, S. A fast stripping continuous cyclic voltammetry method for determination of ultra trace amounts of nalidixic acid. Croat. Chem. Acta2008, 81, 423–430. Search in Google Scholar

Panditi, V. R.; Batchu, S. R.; Gardinali, P. R. Online solid-phase extraction-liquid chromatography-electrospray-tandem mass spectrometry determination of multiple classes of antibiotics in environmental and treated waters. Anal. Bioanal. Chem.2013, 405, 5953–5964. Search in Google Scholar

Pang, Q.-X.; Sun, X.-H.; Chai, H.-M.; Gao, L.-J.; Liu, F.-L. Charge transfer reaction of pefloxacin mesylate with chloranilic acid. Guangpu Shiyanshi2013, 30, 1968–1971. Search in Google Scholar

Paschoal, J. A. R.; Reyes, F. G. R.; Rath, S. Quantitation and identity confirmation of residues of quinolones in tilapia fillets by LC-ESI-MS-MS QToF. Anal. Bioanal. Chem. 2009, 394, 2213–2221. Search in Google Scholar

Piatkowska, M.; Jedziniak, P.; Zmudzki, J. Comparison of different sample preparation procedures for multiclass determination of selected veterinary drug, coccidiostat and insecticide residues in eggs by liquid chromatography-tandem mass spectrometry. Anal. Methods2014, 6, 3034–3044. Search in Google Scholar

Ping, H.; Li, H.; Li, Y.; Kong, D.; Cui, W.; Sun, C. Fluorescent characteristics and content determination of pefloxacin in yttrium(III)-pefloxacin. Heilongjiang Xumu Shouyi2010, 12, 133–135. Search in Google Scholar

Pouliquen, H.; Le Bris, H.; Thorin, C.; Larhantec-Verdier, M.; Morvan, M. L. Quantitative HPLC determination and preliminary assessment of dissolved, suspended, and settled oxolinic acid from turbot farm. Acta Chromatogr.2006, 17, 173–187. Search in Google Scholar

Pozo, O. J.; Guerrero, C.; Sancho, J. V.; Ibanez, M.; Pitarch, E. Hogendoorn, E.; Hernandez, F. Efficient approach for the reliable quantification and confirmation of antibiotics in water using on-line solid-phase extraction liquid chromatography/tandem mass spectrometry. J. Chromatogr. A2006, 1103, 83–93. Search in Google Scholar

Prat, M. D.; Ramil, D.; Compano, R.; Hernandez-Arteseros, J. A.; Granados, M. Determination of flumequine and oxolinic acid in sediments and soils by microwave-assisted extraction and liquid chromatography-fluorescence. Anal. Chim. Acta2006, 567, 229–235. Search in Google Scholar

Qiao, M.; Wang, Y.; Liu, S.; Liu, Z.; Yang, J.; Zhu, J.; Hu, X. A rapid and sensitive resonance Rayleigh scattering spectra method for the determination of quinolones in human urine and pharmaceutical preparation. Luminescence2015, 30, 207–215. Search in Google Scholar

Qin, W.; Liu, Q.; Fan, Y. CE determination of quinolones in the presence of bovine serum albumin. J. Sep. Sci.2009, 32, 118–124. Search in Google Scholar

Quan, H.; Bai, X.; Wang, X. Chrome azurol S-fleroxacin spectrophotometry for determining contents of fleroxacin in powder for injection. Shanxi Yike Daxue Xuebao2009, 40, 60–63. Search in Google Scholar

Raghunath, M.; Patil, S.; Dhamne, A. Validated HPTLC method for simultaneous determination of ofloxacin and dexamethasone sodium phosphate in eye drops. World J. Pharm. Pharm. Sci.2015, 4, 874–882. Search in Google Scholar

Rambla-Alegre, M.; Peris-Vicente, J.; Esteve-Romero, J.; Carda-Broch, S. Analysis of selected veterinary antibiotics in fish by micellar liquid chromatography with fluorescence detection and validation in accordance with regulation 2002/657/EC. Food Chem.2010, 123, 1294–1302. Search in Google Scholar

Ren, N.-L.; Li, H. Determination of pefloxacin residue in urine and serum by flow injection chemiluminescence. Shipin Kexue2012, 33, 215–218. Search in Google Scholar

Romero-Gonzalez, R.; Lopez-Martinez, J. C.; Gomez-Milan, E.; Garrido-Frenich, A.; Martinez-Vidal, J. L. Simultaneous determination of selected veterinary antibiotics in gilthead seabream (Sparus Aurata) by liquid chromatography-mass spectrometry. J. Chromatogr. B2007, 857, 142–148. Search in Google Scholar

Rubies, A.; Vaquerizo, R.; Centrich, F.; Compano, R.; Granados, M.; Prat, M. D. Validation of a method for the analysis of quinolones residues in bovine muscle by liquid chromatography with electrospray ionisation tandem mass spectrometry detection. Talanta2007, 72, 269–276. Search in Google Scholar

Rusu, A.; Hancu, G.; Gyeresi, A. Optimization of a capillary electrophoresis method for the separation of quinolone derivatives. Acta Medica Marisiensis2011, 57, 236–239. Search in Google Scholar

Rusu, A.; Hancu, G.; Völgyi, G.; Tóth, G.; Noszál, B.; Gyéresi, Á. Separation and determination of quinolone antibacterials by capillary electrophoresis. J. Chromatogr. Sci.2015a, 52, 919–925. Search in Google Scholar

Rusu, A.; Hancu, G.; Gyeresi, A. Separation by capillary electrophoresis of 6 extensively used antibacterial compounds. Acta Medica Marisiensis2015b, 60, 109–115. Search in Google Scholar

Saleh, G. A.; Askal, H. F.; Refaat, I. H.; Abdel-Aal, F. A. M. Review on recent separation methods for determination of some fluoroquinolones. J. Liq. Chromatogr. Relat. Technol. 2013, 36, 1401–1420. Search in Google Scholar

Salem, H.; Foda, L.; Khater, W. Spectrofluorimetric determination of certain fluoroquinolones through charge transfer complex formation. Am. J. Pharmacol. Toxicol.2007, 2, 18–25. Search in Google Scholar

Samanidou, V. F.; Christodoulou, E. A.; Papadoyannis, I. N. Recent advances in analytical techniques used for the determination of fluoroquinolones in pharmaceuticals and samples of biological origin – a review article. Curr. Pharm. Anal.2005a, 1, 155–193. Search in Google Scholar

Samanidou, V. F.; Christodoulou, E. A.; Papadoyannis, I. N. Advances in chromatographic analyses of fluoroquinolones in pharmaceuticals and biological samples – a review article. Curr. Pharm. Anal.2005b, 1, 283–308. Search in Google Scholar

Samanidou, V.; Evaggelopoulou, E.; Trotzmuller, M.; Guo, X.; Lankmayr, E. Multi-residue determination of seven quinolones antibiotics in gilthead seabream using liquid chromatography-tandem mass spectrometry. J. Chromatogr. A2008, 1203, 115–123. Search in Google Scholar

Santoro, M. I. R. M.; Kassab, N. M.; Singh, A. K.; Kedor-Hackmam, E. R. M. Quantitative determination of gatifloxacin, levofloxacin, lomefloxacin and pefloxacin fluoroquinolonic antibiotics in pharmaceutical preparations by high-performance liquid chromatography. J. Pharm. Biomed. Anal.2006, 40, 179–184. Search in Google Scholar

Schentag, J. J. Clinical pharmacology of the fluoroquinolones: studies in human dynamic/kinetic models. Clin. Infect. Dis.2000, 31, S40–S44. Search in Google Scholar

Schneider, M. J.; Lehotay, S. J.; Lightfield, A. R. Evaluation of a multi-class, multi-residue liquid chromatography-tandem mass spectrometry method for analysis of 120 veterinary drugs in bovine kidney. Drug Test. Anal.2012, 4, 91–102. Search in Google Scholar

Scortichini, G.; Annunziata, L.; Di Girolamo, V.; Buratti, R.; Galarini, R. Validation of an enzyme-linked immunosorbent assay screening for quinolones in egg, poultry muscle and feed samples. Anal. Chim. Acta2009, 637, 273–278. Search in Google Scholar

Seifrtova, M.; Aufartova, J.; Vytlacilova, J.; Pena, A.; Solich, P.; Novakova, L. Determination of fluoroquinolone antibiotics in wastewater using ultra high-performance liquid chromatography with mass spectrometry and fluorescence detection. J. Sep. Sci.2010, 33, 2094–2108. Search in Google Scholar

Shao, B.; Chen, D.; Zhang, J.; Wu, Y.; Sun, C. Determination of 76 pharmaceutical drugs by liquid chromatography-tandem mass spectrometry in slaughterhouse wastewater. J. Chromatogr. A2009, 1216, 8312–8318. Search in Google Scholar

Shen, H.-Q.; Tan, H.-R.; Qi, K.-Z.; Tian, C.-Q. Separation and determination of fluoroquinolones and tetracyclines by high performance capillary electrophoresis. Anhui Nongye Daxue Xuebao2012, 39, 207–210. Search in Google Scholar

Sheng, W.; Li, Y.; Xu, X.; Yuan, M.; Wang, S. Enzyme-linked immunosorbent assay and colloidal gold-based immunochromatographic assay for several (fluoro)quinolones in milk. Mikrochim. Acta2011, 173, 307–316. Search in Google Scholar

Shi, W. Sichuan Daxue Xuebao, Chemiluminescence analysis of pefloxacin mesylate with reversed micellar. Ziran Kexueban2008, 45, 143–146. Search in Google Scholar

Shi, Z.; Zhao, Y.; Ouyang, S. Separation and determination of five fluoroquinolone antibiotics by ion pair-HPLC. Zhongguo Xiandai Yingyong Yaoxue2009, 26, 162–165. Search in Google Scholar

Siddiqui, F. A.; Arayne, M. S.; Sultana, N.; Qureshi, F.; Mirza, A. Z.; Shehnaz, H. Quantitative determination of fluoroquinolonic antibiotics: pefloxacin, norfloxacin, ciprofloxacin and ofloxacin in pharmaceutical preparations and human serum by high-performance liquid chromatography using multi-wavelength calibration technique. Chemia Analityczna2009, 54, 1465–1485. Search in Google Scholar

Siddiqui, F. A.; Arayne, M. S.; Sultana, N.; Mirza, A. Z.; Qureshi, F.; Zuberi, M. H. Facile and manifest spectrophotometric methods for the determination of six quinolone antibiotics in pharmaceutical formulations using iron salts. Med. Chem. Res.2010, 19, 1259–1272. Search in Google Scholar

Smirnova, T. D.; Nevryueva, N. V. Fluorimetric determination of oxolinic and nalidixic acids using micellar surfactant solutions. Zavodskaya Laboratoriya2010, 76, 12–15. Search in Google Scholar

Smith, S.; Gieseker, C.; Reimschuessel, R.; Decker, C.-S.; Carson, M. C. Simultaneous screening and confirmation of multiple classes of drug residues in fish by liquid chromatography-ion trap mass spectrometry. J. Chromatogr. A2009, 1216, 8224–8232. Search in Google Scholar

Solangi, A. R.; Mallah, A.; Khuhawar, M. Y.; Bhanger, M. I. Cathodic stripping voltammetry of pipemidic acid and ofloxacin in pharmaceutical dosages and human urine. J. Iran. Chem. Soc.2009a, 6, 71–76. Search in Google Scholar

Solangi, A. R.; Bhanger, M. I.; Memon, S. Q.; Khuhawar, M. Y.; Mallah, A. A capillary zone electrophoretic method for simultaneous determination of seven drugs in pharmaceuticals and in human urine. J. AOAC Int.2009b, 92, 1382–1389. Search in Google Scholar

Song, X.-H.; Hao, Z. Control of quality of fleroxacin and glucose injection and stability analysis. Jiefangjun Yaoxue Xuebao2011, 27, 352–353, 376. Search in Google Scholar

Song, Z.-H.; Hu, X.-M.; Zhang, P.-M.; Zhu, Y. Simultaneous determination of 3 quinolone antimicrobial agents by ion chromatography with fluorescence detection. Zhongguo Weisheng Jianyan Zazhi2008, 18, 14–15. Search in Google Scholar

Song-feng, L. V.; Xiang-hong, W.; Hong-wei, L.; Xiao-lei, Z.; Zhaohang, L. Simultaneous determination of gatifloxacin and levofloxacin in todd-hewitt broth employing an in vitro pharmacokinetic-pharmacodynamic model. Lat. Am. J. Pharm. 2015, 34, 201–205. Search in Google Scholar

Sousa, J.; Alves, G.; Fortuna, A.; Falcão, A. Analytical methods for determination of new fluoroquinolones in biological matrices and pharmaceutical formulations by liquid chromatography: a review. Anal. Bioanal. Chem. 2012, 403, 93–129. Search in Google Scholar

Speltini, A.; Sturini, M.; Maraschi, F.; Profumo, A.; Albini, A. Analytical methods for the determination of fluoroquinolones in solid environmental matrices. Trend Anal. Chem.2011, 30, 1337–1350. Search in Google Scholar

Sturini, M.; Speltini, A.; Maraschi, F.; Profumo, A.; Pretali, L.; Fasani, E.; Albini, A. Photochemical degradation of marbofloxacin and enrofloxacin in natural waters. Environ. Sci. Technol.2010a, 44, 4564–4569. Search in Google Scholar

Sturini, M.; Speltini, A.; Maraschi, F.; Rivagli, E.; Profumo, A. Solvent-free microwave-assisted extraction of fluoroquinolones from soil and liquid chromatography-fluorescence determination. J. Chromatogr. A2010b, 1217, 7316–7322. Search in Google Scholar

Sukul, P.; Spiteller, M. Fluoroquinolone antibiotics in the environment. Rev. Environ. Contam. Toxicol.2007, 191, 131–162. Search in Google Scholar

Sun, H.; Li, L. Flow-injection chemiluminescence determination of fleroxacin in pharmaceutical preparations and human urine. Int. J. Sci. Innov. Discov.2011, 1, 134–144. Search in Google Scholar

Sun, H.-W.; Xing, T. Determination of enoxacin using electrode modified by multi-wall carbonnanotubes functionalized with carboxylic Group. Ziran Kexueban2007, 27, 257–261. Search in Google Scholar

Sun, Y.; Ding, Y.; He, X.; Zhao, L. Determination of enoxacin in human plasma by high-performance liquid chromatography and its pharmacokinetics. Zhongguo Kangshengsu Zazhi2006, 31, 758–760. Search in Google Scholar

Sun, H.-W.; He, P.; Lv, Y.-K.; Liang, S.-X. Effective separation and simultaneous determination of seven fluoroquinolones by capillary electrophoresis with diode-array detector. J. Chromatogr. B Analyt. Technol. Biomed. Life Sci.2007, 852, 145–151. Search in Google Scholar

Sun, H.-W.; Zhao, W.; He, P. Electrochemical behavior and determination of ofloxacin on poly(crystal violet) film-modified glassy carbon electrode by differential pulse stripping voltammetry. Ziran Kexueban2008a, 28, 152–157. Search in Google Scholar

Sun, H.; Liu, G.; Qiao, F. Effective separation and simultaneous determination of seven quinolones by reversed phase high performance liquid chromatography. Zhongguo Kangshengsu Zazhi2008b, 33, 97–100. Search in Google Scholar

Sun, H.; Li, L.; Wu, Y. Capillary electrophoresis with electrochemiluminescence detection for simultaneous determination of proline and fleroxacin in human urine. Drug Test. Anal.2009a, 1, 87–92. Search in Google Scholar

Sun, H.-W.; Wu, Y.-Y.; Li, L.-Q. Dysprosium-sensitized chemiluminescence system for the determination of enoxacin in pharmaceutical preparations and biological fluids with flow-injection sampling. Drug Test. Anal.2009b, 1, 128–134. Search in Google Scholar

Sun, H.; Li, L.; Su, M. Simultaneous determination of proline and pipemidic acid in human urine by capillary electrophoresis with electrochemiluminescence detection. J. Clin. Lab. Anal.2010a, 24, 327–333. Search in Google Scholar

Sun, H.-W.; Su, M.; Li, L.-Q. Simultaneous Determination of tetracaine, proline, and enoxacin in human urine by CE with ECL detection. J. Chromatogr. Sci.2010b, 48, 49–54. Search in Google Scholar

Sun, H.; Li, L.; Wu, Y. Dysprosium-sensitized chemiluminescence reactions: their mechanism and application to the determination of synthetic quinolone antibiotics. J. Anal. Chem.2011a, 66, 720–727. Search in Google Scholar

Sun, C.-Y.; Ping, H.; Zhang, M.-W.; Li, H.-K.; Guan, F.-R. Spectroscopic studies on the lanthanide sensitized luminescence and chemiluminescence properties of fluoroquinolone with different structure. Spectrochim. Acta2011b, 82, 375–382. Search in Google Scholar

Sweetman, S.C. Martindale: The Complete Drug Reference; 36th Edition, The Pharmaceutical Press: London, 2009 (electronic version). Search in Google Scholar

Tagiri-Endo, M.; Yanagita, N. Simultaneous determination of residual veterinary drugs in muscle by on-line solid phase extraction/high-performance liquid chromatography/tandem mass spectrometry. Bunseki Kagaku2007, 56, 317–326. Search in Google Scholar

Tamtam, F.; Mercier, F.; Eurin, J.; Chevreuil, M.; Le Bot, B. Ultra performance liquid chromatography tandem mass spectrometry performance evaluation for analysis of antibiotics in natural waters. Anal. Bioanal. Chem.2009, 393, 1709–1718. Search in Google Scholar

Tao, X.; Chen, M.; Jiang, H.; Shen, J.; Wang, Z.; Wang, X.; Wu, X.; Wen, K. Chemiluminescence competitive indirect enzyme immunoassay for 20 fluoroquinolone residues in fish and shrimp based on a single-chain variable fragment. Anal. Bioanal. Chem.2013, 405, 7477–7484. Search in Google Scholar

The British Pharmacopoeia. The Stationary Office: London, 2009 (electronic version). Search in Google Scholar

Tian, J.; Deng, N.; He, J. Separation of five quinolones by capillary electrophoresis. Ziran Kexueban2009, 32, 1170–1172. Search in Google Scholar

Tian, Y.; Zhang, Z.; Li, J.; Li, W.; Chen, Y. Multiresidue determination of fluoroquinolones in eggs by solid-phase extraction-LC-MS/MS. Zhongguo Yaoke Daxue Xuebao2010, 41, 60–65. Search in Google Scholar

Tian, X.-M.; Zhang, Y.-Z.; Sun, X.-L.; Qian, H.; Ji, P. Preparation of anti-pefloxacin antibody and indirect competitive enzyme-linked immunosorbent assay for detection of pefloxacin residue in eggs. Fenxi Kexue Xuebao2013, 29, 371–375. Search in Google Scholar

Tong, C.; Xiang, G. Sensitive determination of enoxacin by its enhancement effect on the fluorescence of terbium(III)–sodium dodecylbenzene sulfonate and its luminescence mechanism. J. Lumin.2007, 126, 575–580. Search in Google Scholar

Tsai, W.-H.; Chuang, H.-Y.; Chen, H.-H.; Huang, J.-J.; Chen, H.-C.; Cheng, S.-H.; Huang, T.-C. Application of dispersive liquid-liquid microextraction and dispersive micro-solid-phase extraction for the determination of quinolones in swine muscle by high-performance liquid chromatography with diode-array detection. Anal. Chim. Acta2009, 656, 56–62. Search in Google Scholar

Tu, C.-Y.; Ho, S.-P.; Hung, S.-W.; Chen, B.-R.; Tsou, L.-T.; Wang, W.-S. Development of a technique to detect the residue of oxolinic acid in the serum and muscle of Chinese mitten crab, Eriocheir sinensis. Yaowu Shipin Fenxi2006, 14, 391–397. Search in Google Scholar

Turiel, E.; Martín-Esteban, A.; Tadeo, J. L. Multiresidue analysis of quinolones and fluoroquinolones in soil by ultrasonic-assisted extraction in small columns and HPLC-UV. Anal. Chim. Acta2006, 562, 30–35. Search in Google Scholar

Ulu, S. T. Spectrofluorimetric determination of fluoroquinolones in pharmaceutical preparations. Spectrochim. Acta A Mol. Biomol. Spectrosc.2009, 72, 138–143. Search in Google Scholar

United States Pharmacopoeia 30; National Formulary 25. US Pharmacopoeia Convention: Rockville, MD, 2007. Search in Google Scholar

Urbaniak, B.; Kokot, Z. J. Spectroscopic investigations of fluoroquinolones metal ion complexes. Acta Pol. Pharm.2013, 70, 621–629. Search in Google Scholar

Uslu, B.; Topal, B. D.; Ozkan, S. A. Electroanalytical investigation and determination of pefloxacin in pharmaceuticals and serum at boron-doped diamond and glassy carbon electrodes. Talanta2008, 74, 1191–1200. Search in Google Scholar

Vazquez, M. M. P.; Vazquez, P. P.; Galera, M. M.; Garcia, M. D. G. Determination of eight fluoroquinolones in groundwater samples with ultrasound-assisted ionic liquid dispersive liquid-liquid microextraction prior to high-performance liquid chromatography and fluorescence detection. Anal. Chim. Acta2012, 748, 20–27. Search in Google Scholar

Waibel, B.; Holzgrabe, U. 1H and 19F NMR relaxation studies of fleroxacin with Micrococcus luteus. J. Pharm. Biomed. Anal.2007, 43, 1595–1601. Search in Google Scholar

Wang, N.; Bai, X. Quick determination of plasma fleroxacin by solid phase extraction and RP-HPLC with fluorometry. Shanxi Yike Daxue Xuebao2007, 38, 923–925. Search in Google Scholar

Wang, M.-H.; Wang, S.-P. Analysis of quinolones by voltage-assisted liquid-phase microextraction combined with LC-MS. J. Sep. Sci.2012, 35, 702–706. Search in Google Scholar

Wang, W.-S.; Shih, C.-W.; Hung, S.-W.; Ling, Y.-F.; Tu, C.-Y.; Chen, B-R; Tsou, L.-T.; Ho, S.-P. Development and application of enzyme-linked immunosorbent assay residual detection kits for fluoroquinolones. Taiwan Shouyixue Zazhi2006, 32, 301–311. Search in Google Scholar

Wang, L.; Yang, P.; Li, Y.; Chen, H.; Li, M.; Luo, F. A flow injection chemiluminescence method for the determination of fluoroquinolone derivative using the reaction of luminol and hydrogen peroxide catalyzed by gold nanoparticles. Talanta2007a, 72, 1066–1072. Search in Google Scholar

Wang, Z.; Zhu, Y.; Ding, S.; He, F.; Beier, R. C.; Li, J.; Jiang, H.; Feng, C. Wan, Y.; Zhang, S. Development of a monoclonal antibody-based broad-specificity ELISA for fluoroquinolone antibiotics in foods and molecular modeling studies of cross-reactive compounds. Anal. Chem.2007b, 79, 4471–4483. Search in Google Scholar

Wang, N.; Duan, L.; Bai, X. Quick separation and determination of four fluoroquinolones in human plasma by SPE and RP-HPLC. Shanxi Yike Daxue Xuebao2008, 39, 1014–1017. Search in Google Scholar

Wang, R.; Wu, Y.; Zhai, S.; Li, J.; Zheng, W. Chemiluminescent determination of pefloxacin mesylate. Zhongguo Kangshengsu Zazhi2009a, 34, 383–384. Search in Google Scholar

Wang, Y.; Baeyens, W. R. G.; Huang, C.; Fei, G.; He, L.; Ouyang, J. Enhanced separation of seven quinolones by capillary electrophoresis with silica nanoparticles as additive. Talanta2009b, 77, 1667–1674. Search in Google Scholar

Wang, M.; Han, Q.; Yang, X.-H.; Tian, L. Determination of fleroxacin in human urine and plasma by resonance Rayleigh scattering method. Fenxi Shiyanshi2010, 29, 65–68. Search in Google Scholar

Wang, L.; Li, Y.-Q.; Zhang, L.-C. Simultaneous determination of twenty antibiotic residues including b-lactams, quinolones and macrolides in milk and powdered milk samples by ultra performance liquid chromatography. Fenxi Shiyanshi2011, 30, 23–27. Search in Google Scholar

Wang, S.; Zhang, J.; Shao, B. Analysis of chloramphenicol, sulfonamides, fluoroquinolones, tetracyclines and macrolides in sewage sludge by ultra performance liquid chromatography tandem mass spectrometry. Fenxi Ceshi Xuebao2013, 32, 179–185. Search in Google Scholar

Wang, J.; Kong, L.; Shen, W.; Hu, X.; Shen, Y.; Liu, S. Synergistic fluorescence quenching of quinolone antibiotics by palladium(II) and sodium dodecyl benzene sulfonate and the analytical application. Anal. Methods2014, 6, 4343–4352. Search in Google Scholar

Wei, S.-L.; Zhang, S.-B.; Yan, Z.-J. Separation and analysis of fluoroquinolones using microemulsion electrokinetic capillary chromatography. Fenxi Huaxue2008, 36, 499–503. Search in Google Scholar

Wen, K.; Noelke, G.; Schillberg, S.; Wang, Z.; Zhang, S.; Wu, C.; Jiang, H.; Meng, H.; Shen, J. Improved fluoroquinolone detection in ELISA through engineering of a broad-specific single-chain variable fragment binding simultaneously to 20 fluoroquinolones. Anal. Bioanal. Chem.2012, 403, 2771–2783. Search in Google Scholar

William, P.; Emmanuelle, V. Determination of 136 pharmaceuticals and hormones in sewage sludge using quick, easy, cheap, effective, rugged and safe extraction followed by analysis with liquid chromatography-time-of-flight-mass. J. Chromatogr. A2013, 1290, 46–61. Search in Google Scholar

Wu, G.-H.; Wang, J.; Guo, C.; Wang, D.-X.; Zhao, T.-T. Study on the ternary complex of FLRX, zinc(II) and BSA by the fluorescence method. Guangpuxue Yu Guangpu Fenxi2007, 27, 765–768. Search in Google Scholar

Wu, Y.; Wu, H.; Du, L.-M. Determination of enoxacin and norfloxacin by spectrophotometry with derivation. Fenxi Kexue Xuebao2010, 26, 91–93. Search in Google Scholar

Xia, H.; Peng, M. Determination of eight quinolones in chicken by high performance liquid chromatography. Shipin Keji2011, 36, 124–127. Search in Google Scholar

Xiao, Y.; Chang, H.; Jia, A.; Hu, J. Trace analysis of quinolone and fluoroquinolone antibiotics from wastewaters by liquid chromatography-electrospray tandem mass spectrometry. J. Chromatogr. A2008, 1214, 100–108. Search in Google Scholar

Xie, Y.; Song, Y.; Zhang, Y.; Zhao, B. Near-infrared spectroscopy quantitative determination of pefloxacin mesylate concentration in pharmaceuticals by using partial least squares and principal component regression multivariate calibration. Spectrochim. Acta2010, 75A, 1535–1539. Search in Google Scholar

Xie, W.; Han, C.; Hou, J.; Wang, F.; Qian, Y.; Xi, J. Simultaneous determination of multiveterinary drug residues in pork meat by liquid chromatography-tandem mass spectrometry combined with solid phase extraction. J. Sep. Sci.2012, 35, 3447–3454. Search in Google Scholar

Xu, L.; Cai, Y.; Wang, X.; Zhang, S. Determination of pefloxacin mesylate by charge-transfer reaction with fluorescence spectrometry. Zhongguo Yiyao Gongye Zazhi2007, 38, 123–125. Search in Google Scholar

Xu, H.; Chen, L.; Sun, L.; Sun, X.; Du, X.; Wang, J.; Wang, T.; Zeng, Q.; Wang, H.; Xu, Y. Microwave-assisted extraction and in situ clean-up for the determination of fluoroquinolone antibiotics in chicken breast muscle by LC-MS/MS. J. Sep. Sci.2011, 34, 142–149. Search in Google Scholar

Yamaguchi, T.; Nakao, M.; Nakahara, R.; Nishioka, Y.; Ikeda, C.; Fujita, Y. Spectrophotometric determination of quinolone antibiotics by an association complex formation with aluminum(III) and erythrosin. Anal. Sci.2009, 25, 125–128. Search in Google Scholar

Yan, X.-Y.; Jiang, G.-P.; Zhu, X.-P.; He, B. Ionic liquids aqueous two-phase system-UV spectrophotometric determination of oxolinic acid. Guangpu Shiyanshi2009, 26, 807–810. Search in Google Scholar

Yang, Z.; Qin, W. Separation of fluoroquinolones in acidic buffer by capillary electrophoresis with contactless conductivity detection. J. Chromatogr. A2009, 1216, 5327–5332. Search in Google Scholar

Yang, L.; Huang, D.-R.; Wen, Y.-Y. Measurement of fluoroquinolone antibiotics in estuarine and coastal seawater by liquid chromatography-tandem mass spectrometry. Ziran Kexueban2011, 16, 418–423. Search in Google Scholar

Yang, Y.-W.; Zhu, H.-J.; Zhu, Y.; Zhang, W.-Q. Trace analysis of trimethoprim and sulfonamide, macrolide, quinolone, and tetracycline antibiotics in chlorinated drinking water using liquid chromatography electrospray tandem mass spectrometry. Huanjing Yu Jiankang Zazhi2012, 29, 544–546. Search in Google Scholar

Yang, Q.; Tan, X.; Yang, J. Sensitive determination of enoxacin in pharmaceutical formulations by its quench effect on the fluorescence of glutathione-capped CdTe quantum dots. Luminescence2016, 31, 241–246. Search in Google Scholar

Ye, Z.; Weinberg, H. S.; Meyer, M. T. Trace analysis of trimethoprim and sulfonamide, macrolide, quinolone, and tetracycline antibiotics in chlorinated drinking water using liquid chromatography electrospray tandem mass spectrometry. Anal. Chem.2007, 79, 1135–1144. Search in Google Scholar

Yi, L.-H.; Fei, J.-J.; Li, J.-N. Anodic adsorptive voltammetric determination of pefloxacin at a carbon paste electrode. Huaxue Shiji2006, 28, 744–746. Search in Google Scholar

Yi, L.-H.; Fei, J.-J.; Li, J.-N. Anodic adsorptive voltammetric determination of enoxacin at carbon paste electrode. Fenxi Shiyanshi2007a, 26, 50–53. Search in Google Scholar

Yi, Q.; Qi, Z.; Cai, L.; Xiong, D.; Guo, M.; Li, X.; Xiang, Y. Determination of enoxacin and related substances by RP-HPLC. Yiyao Daobao2007b, 26, 1354–1355. Search in Google Scholar

Yu, H.-J.; Bi, S.-C. Research on determination of eleven fluoroquinolones by RP-ion pair liquid chromatography. Fenxi Shiyanshi2007, 26, 18–21. Search in Google Scholar

Yu, S.; Gomez, D. G.; Campiglia, A. D. Solid-liquid extraction fluorescence line narrowing spectroscopy of fluoroquinolones in aqueous samples. Appl. Spectrosc.2006, 60, 1174–1180. Search in Google Scholar

Yu, Y.-J.; Wu, H.-L.; Shao, S.-Z.; Kang, C.; Zhao, J.; Wang, Y.; Zhu, S.-H.; Yu, R.-Q. Using second-order calibration method based on trilinear decomposition algorithms coupled with high performance liquid chromatography with diode array detector for determination of quinolones in honey samples. Talanta2011, 85, 1549–1559. Search in Google Scholar

Yu, H.; Mu, H.; Hu, Y.-M. Determination of fluoroquinolones, sulfonamides, and tetracyclines multiresidues simultaneously in porcine tissue by MSPD and HPLC–DAD. J. Pharm. Anal.2012a, 2, 76–81. Search in Google Scholar

Yu, Q.-H.; Li, D.-H.; Chen, L.-S.; Mu, W. Linear scanning voltammetric determination of fleroxacin. Huaxue Fence2012b, 48, 1454–1456. Search in Google Scholar

Yu, H.; Tao, Y.; Chen, D.; Pan, Y.; Liu, Z.; Wang, Y.; Huang, L.; Dai, M.; Peng, D.; Wang, X. Simultaneous determination of fluoroquinolones in foods of animal origin by a high performance liquid chromatography and a liquid chromatography tandem mass spectrometry with accelerated solvent extraction. J. Chromatogr. B2012c, 885–886, 150–159. Search in Google Scholar

Zafra-Gomez, A.; Garballo, A.; Ballesteros, O.; Navalon, A.; Garcia-Ayuso, L. E. Simultaneous determination of quinolone antibacterials in bovine milk by liquid chromatography-mass spectrometry. Biomed. Chromatogr.2008, 22, 1186–1193. Search in Google Scholar

Zeng, Y.-B.; Zhao, D.-H.; Li, L.; Wang, L.; Shen, B.; Xi, Q.-H.; Zhang, M.-M. Simultaneous determination of three quinolones residues in milk by pyridinium ionic liquid-based aqueous two phase systems coupled with high performance liquid chromatography. Gaodeng Xuexiao Huaxue Xuebao2009, 30, 1956–1959. Search in Google Scholar

Zhan, J.; Yu, X.-J.; Zhong, Y.-Y.; Zhang, Z.-T.; Cui, X.-M.; Peng, J.-F.; Feng, R.; Liu, X.-T.; Zhu, Y. Generic and rapid determination of veterinary drug residues and other contaminants in raw milk by ultra performance liquid chromatography-tandem mass spectrometry. J. Chromatogr. B2012, 906, 48–57. Search in Google Scholar

Zhan, J.; Zhong, Y.-Y.; Yu, X.-J.; Peng, J.-F.; Chen, S.; Yin, J.-Y.; Zhang, J.-J.; Zhu, Y. Multi-class method for determination of veterinary drug residues and other contaminants in infant formula by ultra performance liquid chromatography-tandem mass spectrometry. Food Chem.2013, 138, 827–834. Search in Google Scholar

Zhang, S.-B.; Lin, H.-H. Spectrophotometric determination of pefloxacin mesylate based on the charge-transfer reaction. Huaxue Shiji2009, 31, 625–627. Search in Google Scholar

Zhang, J.; Ma, J.; Wu, C. Determination of nadifloxacin cream by HPLC. Zhongguo Yaoshi2006a, 9, 507–508. Search in Google Scholar

Zhang, X.; Aodeng, G.; Nie, H.-Y.; Zhang, H.-W.; Chen, H.-Y.; Li, M.-J. Determination of pefloxacin with aluminum sensitized UV-spectrophotometric method. Neimenggu Daxue Xuebao2006b, 37, 598–600. Search in Google Scholar

Zhang, Y.-Z.; Zhang, Z.-Y.; Zhou, Y.-C.; Liu, L.; Zhu, Y. Determination of fluorinated quinolone antibacterials by ion chromatography with fluorescence detection. J. Zhejiang Univ. Sci. B2007a, 8, 302–306. Search in Google Scholar

Zhang, L-W; Wang, K.; Zhang, X.-X. Study of the interactions between fluoroquinolones and human serum albumin by affinity capillary electrophoresis and fluorescence method. Anal. Chim. Acta2007b, 603, 101–110. Search in Google Scholar

Zhang, H.; Chen, S.; Lu, Y.; Dai, Z. Simultaneous determination of quinolones in fish by liquid chromatography coupled with fluorescence detection: comparison of sub-2 microm particles and conventional C18 columns. J. Sep. Sci.2010, 33, 1959–1967. Search in Google Scholar

Zhang, Z.; Liu, J.-F.; Feng, T.-T.; Yao, Y.; Gao, L.-H.; Jiang, G.-B. Time-resolved fluoroimmunoassay as an advantageous analytical method for assessing the total concentration and environmental risk of fluoroquinolones in surface waters. Environ. Sci. Technol.2013, 47, 454–462. Search in Google Scholar

Zhao, Y.-C.; Fan, G.-Y. Simultaneous determination of 8 kinds of fluoroquinolone drugs in Chinese medicine veterinary drugs by solid-phase extraction-HPLC. Heilongjiang Xumu Shouyi2012, 94, 90–91. Search in Google Scholar

Zhao, Y.; Liu, Y.; Jin, Y.; Xu, Y.; Zhong, Y.; Jiang, S.; Li, X.; Zeng, F.; Zhou, J. [Simultaneous determination of 29 veterinary drugs in compound feeds by ultra performance liquid chromatography-electrospray ionization tandem quadrupole mass spectrometry]. Sepu2012, 30, 908–914. Search in Google Scholar

Zhao, Y.; Wang, J.; Su, L. Establishment of blocking ELISA for detection of pefloxacin. Xumu Yu Shouyi2013, 45, 64–66. Search in Google Scholar

Zheng, M.-M.; Ruan, G.-D.; Feng, Y.-Q. Evaluating polymer monolith in-tube solid-phase microextraction coupled to liquid chromatography/quadrupole time-of-flight mass spectrometry for reliable quantification and confirmation of quinolone antibacterials in edible animal food. J. Chromatogr. A2009, 1216, 7510–7519. Search in Google Scholar

Zhou, J.; Xue, X.; Chen, F.; Zhang, J.; Li, Y.; Wu, L.; Chen, L.; Zhao, J. Simultaneous determination of seven fluoroquinolones in royal jelly by ultrasonic-assisted extraction and liquid chromatography with fluorescence detection. J. Sep. Sci.2009, 32, 955–964. Search in Google Scholar

Zhou, L.-J.; Ying, G.-G.; Liu, S.; Zhao, J.-L.; Chen, F.; Zhang, R.-Q.; Peng, F.-Q.; Zhang, Q.-Q. Simultaneous determination of human and veterinary antibiotics in various environmental matrices by rapid resolution liquid chromatography-electrospray ionization tandem mass spectrometry. J. Chromatogr. A2012, 1244, 123–138. Search in Google Scholar

Zhu, P.; Li, N.; Yuan, Q. Determination of fleroxacin in fleroxacin and glucose injection by high performance liquid chromatography. Shanxi Yike Daxue Xuebao2008, 39, 152–154. Search in Google Scholar

Zuo, Z.; Gao, L.; Tang, S. Studies on multiresidue determination of 28 antibiotics in honey by solid-phase extraction and high-performance liquid chromatography-tandem mass spectrometry. Yaowu Fenxi Zazhi2009, 29, 1196–1201. Search in Google Scholar

Received: 2015-12-15
Accepted: 2016-11-23
Published Online: 2017-5-26

©2017 Walter de Gruyter GmbH, Berlin/Boston

This article is distributed under the terms of the Creative Commons Attribution Non-Commercial License, which permits unrestricted non-commercial use, distribution, and reproduction in any medium, provided the original work is properly cited.