QuEChERS and soil analysis. An Overview.

Jose Vera 1 , Luísa Correia-Sá 1 , Paula Paíga 1 , Idalina Bragança 1 , Virgínia C. Fernandes 1 , Valentina F. Domingues 1 , and Cristina Delerue-Matos 1
  • 1 REQUIMTE, Instituto Superior de Engenharia, Instituto Politécnico do Porto Rua Drº António Bernardino de Almeida, 431, 4200-072 Porto Portugal


This paper reviews the Quick Easy Cheap Effective Rugged Safe (QuEChERS) methods used for the analysis of several pollutants in soil. The recent advances made with this method are discussed.The analysis of pesticide residues and other analytes in soil requires the extraction of analytes from this matrix. Following extraction, a clean-up procedure may be performed, if necessary, prior to instrumental analysis. This review considers all aspects of sample preparation, including extraction and cleanup. Several parameters are discussed in extraction optimization namely: soil type and sample amount, hydration, solvent of extraction QuEChERS content, extraction time and agglomeration prevention. In addition, method performance characteristics in soil studies are critically discussed.

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  • [1] Correia-Sá L., Fernandes V.C., Carvalho M., Calhau C., Domingues V.F., and Delerue-Matos C., Optimization of QuEChERS method for the analysis of organochlorine pesticides in soils with diverse organic matter. J. Sep. Sci., 2012, 35, 1521-1530.

  • [2] Pinto C.G., Martín S.H., Pavón J.L.P., and Cordero B.M., A simplified Quick, Easy, Cheap, Effective, Rugged and Safe approach for the determination of trihalomethanes and benzene, toluene, ethylbenzene and xylenes in soil matrices by fast gas chromatography with mass spectrometry detection. Anal. Chim. Acta, 2011, 689, 129-136.

  • [3] Rashid A., Nawaz S., Barker H., Ahmad I., and Ashraf M., Development of a simple extraction and clean-up procedure for determination of organochlorine pesticides in soil using gas chromatography-tandem mass spectrometry. J. Chromatogr. A, 2010, 1217, 2933-2939.

  • [4] Getenga Z.M., Keng’ara F.O., and Wandiga S.O., Determination of organochlorine pesticide residues in soil and water from River Nyando drainage system within Lake Victoria Basin, Kenya. Bull. Environ. Contam. Toxicol., 2004, 72, 335-343.

  • [5] Prestes O.D., Padilla-Sánchez J.A., Romero-González R., Grio S.L., Frenich A.G., and Martínez-Vidal J.L., Comparison of several extraction procedures for the determination of biopesticides in soil samples by ultrahigh pressure LC-MS/MS. J. Sep. Sci., 2012, 35, 861-868.

  • [6] Aelion C.M., Soil contamination monitoring, ed. E. Monitoring. Vol. II. Encyclopedia of Life Support Systems (EOLSS).

  • [7] Wauchope R.D., Yeh S., Linders J., Kloskowski R., Tanaka K., Rubin B., Katayama A., Kordel W., Gerstl Z., Lane M., and Unsworth J.B., Pesticide soil sorption parameters: theory, measurement, uses, limitations and reliability. Pest Manage. Sci., 2002, 58, 419-445.

  • [8] Caldas S.S., Bolzan C.M., Cerqueira M.B., Tomasini D., Furlong E.B., Fagundes C., and Primel E.G., Evaluation of a Modified QuEChERS Extraction of Multiple Classes of Pesticides from a Rice Paddy Soil by LC-APCI-MS/MS. J. Agric. Food Chem., 2011, 59, 11918-11926.

  • [9] Garimella U.I., Stearman G.K., and Wells M.J.M., Comparison among soil series and extraction methods for the analysis of trifluralin. J. Agric. Food Chem., 2000, 48, 5874-5880.

  • [10] Vig K., Singh D.K., Agarwal H.C., Dhawan A.K., and Dureja P., Insecticide residues in cotton crop soil. J. Environ. Sci. Health, Part B, 2001, 36, 421-434.

  • [11] Pinto C.G., Laespada M.E.F., Martín S.H., Ferreira A.M.C., Pavón J.L.P., and Cordero B.M., Simplified QuEChERS approach for the extraction of chlorinated compounds from soil samples. Talanta, 2010, 81, 385-391.

  • [12] Wang Y.H., Du L.W., Zhou X.M., Tan H.H., Bai L.Y., Zeng D.Q., and Tian H., QuEChERS extraction for high performance liquid chromatographic determination of pyrazosulfuron-ethyl in soils. J. Chem. Soc. Pak., 2012, 34, 28-32.

  • [13] Method AOAC. Official Methods of Analysis 2007.01, Pesticide Residues in Foods by Acetonitrile Extraction and Partitioning with Magnesium Sulfate. 2007, 18 th: Available from: http://www.weber.hu/PDFs/QuEChERS/AOAC_2007_01.pdf, accessed December 2012.

  • [14] EN15662. Foods of Plant Origin - Determination of Pesticide Residues Using GC-MS and/or LC-MS/MS Following Acetonitrile Extraction/Partitioning and Clean-up by Dispersive SPE. 2008, Available from: https://www.astandis.at/shopV5/Preview.action%3Bjsessionid=0591FE94A94C9C6E7117064F9A22C0CE?preview=&dokkey=321612&selectedLocale=en, accessed November 2012.

  • [15] Plossl F., Giera M., and Bracher F., Multiresidue analytical method using dispersive solid-phase extraction and gas chromatography/ion trap mass spectrometry to determine pharmaceuticals in whole blood. J. Chromatogr. A, 2006, 1135, 19-26.

  • [16] Lesueur C., Gartner M., Mentler A., and Fuerhacker M., Comparison of four extraction methods for the analysis of 24 pesticides in soil samples with gas chromatography-mass spectrometry and liquid chromatography-ion trap-mass spectrometry. Talanta, 2008, 75, 284-293.

  • [17] Fagerquist C.K., Alan R., and Lehotay S.J., Confirmatory and quantitative analysis of β-lactam antibiotics in bovine kidney tissue by dispersive solid-phase extraction and liquid chromatography-tandem mass spectrometry. Anal. Chem., 2005, 77, 1473-1482.

  • [18] Aguilera-Luiz M., Vidal J.L.M., Romero-González R., and Frenich A.G., Multi-residue determination of veterinary drugs in milk by ultra-high-pressure liquid chromatography-tandem mass spectrometry. J. Chromatogr. A, 2008, 1205, 10-16.

  • [19] Kinsella B., Lehotay S.J., Mastovska K., Lightfield A.R., Furey A., and Danaher M., New method for the analysis of flukicide and other anthelmintic residues in bovine milk and liver using liquid chromatography-tandem mass spectrometry. Anal. Chim. Acta, 2009, 637, 196-207.

  • [20] Stubbings G. and Bigwood T., The development and validation of a multiclass liquid chromatography tandem mass spectrometry (LC-MS/MS) procedure for the determination of veterinary drug residues in animal tissue using a QuEChERS (QUick, Easy, CHeap, Effective, Rugged and Safe) approach. Anal. Chim. Acta, 2009, 637, 68-78.

  • [21] Bragança I., Plácido A., Paíga P., Domingues V.F., and Delerue-Matos C., QuEChERS: A new sample preparation approach for the determination of ibuprofen and its metabolites in soils. Sci. Total Environ., 2012, 433, 281-289.

  • [22] Rouvière F., Buleté A., Cren-Olivé C., and Arnaudguilhem C., Multiresidue analysis of aromatic organochlorines in soil by gas chromatography-mass spectrometry and QuEChERS extraction based on water/dichloromethane partitioning. Comparison with accelerated solvent extraction. Talanta, 2012, 93, 336-344.

  • [23] Andreu V. and Picó Y., Determination of pesticides and their degradation products in soil: critical review and comparison of methods. TrAC, Trends Anal. Chem., 2004, 23, 772-789.

  • [24] Asensio-Ramos M., Hernandez-Borges J., Ravelo-Perez L.M., and Rodriguez-Delgado M.A., Evaluation of a modified QuEChERS method for the extraction of pesticides from agricultural, ornamental and forestal soils. Anal. Bioanal. Chem., 2010, 396, 2307-2319.

  • [25] Brondi S.H.G., de Macedo A.N., Vicente G.H.L., and Nogueira A.R.A., Evaluation of the QuEChERS method and gas chromatography-mass spectrometry for the analysis pesticide residues in water and sediment. Bull. Environ. Contam. Toxicol., 2011, 86, 18-22.

  • [26] Fernandes V.C., Domingues V.F., Mateus N., and Delerue-Matos C., Multiresidue pesticides analysis in soils using modified QuEChERS with disposable pipette extraction and dispersive solid-phase extraction. J. Sep. Sci., 2013, 36, 376-382.

  • [27] Kvicalova M., Doubravova P., Jobanek R., Jokesova M., Ocenaskova V., Sussenbekova H., and Svobodova A., Application of different extraction methods for the determination of selected pesticide residues in sediments. Bull. Environ. Contam. Toxicol., 2012, 89, 21-26.

  • [28] Mei M., Du Z.X., and Chen Y., QuEChERS-Ultra performance liquid chromatography-tandem mass spectrometry for determination of 5 currently used herbicides. Chin. J. Anal. Chem., 2011, 39, 1659-1664.

  • [29] Yang X.B., Ying G.G., and Kookana R.S., Rapid multiresidue determination for currently used pesticides in agricultural drainage waters and soils using gas chromatography-mass spectrometry. J. Environ. Sci. Health, Part B, 2010, 45, 152-161.

  • [30] Li Y., Dong F., Liu X., Xu J., Li J., Kong Z., Chen X., Liang X., and Zheng Y., Simultaneous enantioselective determination of triazole fungicides in soil and water by chiral liquid chromatography/tandem mass spectrometry. J. Chromatogr. A, 2012, 1224, 51-60.

  • [31] Wang J., Zhao L.L., Li X.S., Jiang Y.P., Li N., Qin Z.H., and Pan C.P., Residue dynamic of pyrimorph on tomatoes, cucumbers and soil under greenhouse trails. Bull. Environ. Contam. Toxicol., 2011, 86, 326-330.

  • [32] Wang L., Zhao P.Y., Zhang F.Z., Du F.P., and Pan C.P., Diafenthiuron residue and decline in pakchoi and soil under field application. Ecotoxicol. Environ. Saf., 2012, 79, 75-79.

  • [33] Zhang F.Z., Wang L., Zhou L., Wu D., Pan H.J., and Pan C.P., Residue dynamics of pyraclostrobin in peanut and field soil by QuEChERS and LC-MS/MS. Ecotoxicol. Environ. Saf., 2012, 78, 116-122.

  • [34] Drozdzynski D. and Kowalska J., Rapid analysis of organic farming insecticides in soil and produce using ultra-performance liquid chromatography/tandem mass spectrometry. Anal. Bioanal. Chem., 2009, 394, 2241-2247.

  • [35] Padilla-Sánchez J.A., Plaza-Bolaños P., Romero-González R., Garrido-Frenich A., and Martínez Vidal J.L., Application of a quick, easy, cheap, effective, rugged and safe-based method for the simultaneous extraction of chlorophenols, alkylphenols, nitrophenols and cresols in agricultural soils, analyzed by using gas chromatography–triple quadrupole-mass spectrometry/mass spectrometry. J. Chromatogr. A, 2010, 1217, 5724-5731.

  • [36] Jiang Y.P., Jiang Y.T., He S., Zhang H.L., and Pan C.P., Dissipation of diethyl aminoethyl hexanoate (DA-6) residues in pakchoi, cotton crops and soil. Bull. Environ. Contam. Toxicol., 2012, 88, 533-537.

  • [37] Martín S.H., Pinto C.G., Pavón J.L.P., and Cordero B.M., Determination of trihalomethanes in soil matrices by simplified quick, easy, cheap, effective, rugged and safe extraction and fast gas chromatography with electron capture detection. J. Chromatogr. A, 2010, 1217, 4883-4889.

  • [38] Dreyer A., Thuens S., Kirchgeorg T., and Radke M., Ombrotrophic Peat Bogs Are Not Suited as Natural Archives To Investigate the Historical Atmospheric Deposition of Perfluoroalkyl Substances. Environ. Sci. Technol., 2012, 46, 7512-7519.

  • [39] Salvia M.-V., Vulliet E., Wiest L., Baudot R., and Cren-Olivé C., Development of a multi-residue method using acetonitrile-based extraction followed by liquid chromatography–tandem mass spectrometry for the analysis of steroids and veterinary and human drugs at trace levels in soil. J.Chromatogr. A, 2012, 1245, 122-133.

  • [40] Sun J., Feng N., Tang C., and Qin D., Determination of Cyantraniliprole and its Major Metabolite Residues in Pakchoi and Soil Using Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry. Bull. Environ. Contam. Toxicol., 2012, 89, 845-852.

  • [41] Zhang J.M., Chai W.G., and Wu Y.L., Residues of chlorantraniliprole in rice field ecosystem. Chemosphere, 2012, 87, 132-136.

  • [42] Wang L., Zhao P.Y., Zhang F.Z., Li Y.J., Du F.P., and Pan C.P., Dissipation and residue behavior of emamectin benzoate on apple and cabbage field application. Ecotoxicol. Environ. Saf., 2012, 78, 260-264.

  • [43] Urvashi, Jyot G., Sahoo S.K., Kaur S., Battu R.S., and Singh B., Estimation of indoxacarb residues by QuEChERS technique and its degradation pattern in cabbage. Bull. Environ. Contam. Toxicol., 2012, 88, 372-376.

  • [44] Li Y., Dong F., Liu X., Xu J., Li J., Kong Z., Chen X., Song W., Wang Y., and Zheng Y., Simultaneous enantioselective determination of fenbuconazole and its main metabolites in soil and water by chiral liquid chromatography/tandem mass spectrometry. J. Chromatogr. A, 2011, 1218, 6667-6674.

  • [45] Temur C., Tiryaki O., Uzun O., and Basaran M., Adaptation and validation of QuEChERS method for the analysis of trifluralin in wind-eroded soil. J.Environ. Sci. Health Part B 2012, 47, 842-850.

  • [46] Li X.S., Jiang Y.P., Shan W.L., and Pan C.P., Dissipation and residues detection of dioctyldiethylenetriamine cetate in rice plant and environment by QuEChERS method and liquid chromatography/electrospray tandem mass spectrometry. Bull. Environ. Contam. Toxicol., 2010, 84, 596-601.

  • [47] Shi C.H., Gui W.J., Chen J., and Zhu G.N., Determination of oxadiargyl residues in environmental samples and rice samples. Bull. Environ. Contam. Toxicol., 2010, 84, 236-239.

  • [48] Chen L., Li X.-S., Wang Z.-Q., Pan C.-P., and Jin R.-C., Residue dynamics of procymidone in leeks and soil in greenhouses by smoke generator application. Ecotoxicol. Environ. Saf., 2010, 73, 73-77.

  • [49] Gilbert-López B., García-Reyes J.F., and Molina-Díaz A., Sample treatment and determination of pesticide residues in fatty vegetable matrices: A review. Talanta, 2009, 79, 109-128.

  • [50] UCT. Quechers Booklet. 2008; Available from: http://2008_uct_quechers_booklet.pdf, accessed November 2012.

  • [51] Anastassiades M., Lehotay S.J., Stajnbaher D., and Schenck F.J., Fast and easy multiresidue method employing acetonitrile extraction/partitioning and dispersive solid-phase extraction for the determination of pesticide residues in produce. J. AOAC Int., 2003, 86, 412-431.

  • [52] Pereira R.C., Martinez M.C.M., Cortizas A.M., and Macias F., Analysis of composition, distribution and origin of hexachlorocyclohexane residues in agricultural soils from NW Spain. Sci. Total Environ., 2010, 408, 5583-5591.

  • [53] Lehotay S.J., QuEChERS sample preparation approach for mass spectrometric analysis of pesticide residues in foods. Methods in molecular biology (Clifton, N.J.), 2011, 747, 65-91.

  • [54] Maštovská K. and Lehotay S.J., Evaluation of common organic solvents for gas chromatographic analysis and stability of multiclass pesticide residues. J. Chromatogr. A, 2004, 1040, 259-272.

  • [55] Lehotay S.J., Mastovska K., and Yun S.J., Evaluation of two fast and easy methods for pesticide residue analysis in fatty food matrixes. J. AOAC Int., 2005, 88, 630-638.

  • [56] Taverniers I., De Loose M., and Van Bockstaele E., Trends in quality in the analytical laboratory. II. Analytical method validation and quality assurance. TrAC, Trends Anal. Chem., 2004, 23, 535-552.

  • [57] Schmeck T. and Wenclawiak B.W., Sediment Matrix Induced Response Enhancement in the Gas Chromatographic–Mass Spectrometric Quantification of Insecticides in Four Different Solvent Extracts from Ultrasonic and Soxhlet Extraction. Chromatographia, 2005, 62, 159-165.

  • [58] Poole C.F., Matrix-induced response enhancement in pesticide residue analysis by gas chromatography. J. Chromatogr. A, 2007, 1158, 241-250.

  • [59] Cappiello A., Famiglini G., Palma P., Pierini E., Termopoli V., and Trufelli H., Overcoming matrix effects in liquid chromatography−Mass Spectrometry. Anal. Chem., 2008, 80, 9343-9348.

  • [60] Mansilha C., Melo A., Rebelo H., Ferreira I.M.P.L.V.O., Pinho O., Domingues V., Pinho C., and Gameiro P., Quantification of endocrine disruptors and pesticides in water by gas chromatography–tandem mass spectrometry. Method validation using weighted linear regression schemes. J. Chromatogr. A, 2010, 1217, 6681-6691.

  • [61] Trufelli H., Palma P., Famiglini G., and Cappiello A., An overview of matrix effects in liquid chromatography-mass spectrometry. Mass Spectrom. Rev., 2011, 30, 491-509.

  • [62] Fernandes V.C., Domingues V.F., Mateus N., and Delerue-Matos C., Determination of pesticides in fruit and fruit juices by chromatographic methods. An overview. J. Chromatogr. Sci., 2011, 49, 715-30.

  • [63] Soler C., Mañes J., and Picó Y., The Role of the Liquid Chromatography-Mass Spectrometry in Pesticide Residue Determination in Food. Crit. Rev. Anal. Chem., 2008, 38, 93-117.

  • [64] Leandro C.C., Hancock P., Fussell R.J., and Keely B.J., Ultra-performance liquid chromatography for the determination of pesticide residues in foods by tandem quadrupole mass spectrometry with polarity switching. J. Chromatogr. A, 2007, 1144, 161-169.


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