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Licensed Unlicensed Requires Authentication Published by De Gruyter September 17, 2013

Simultaneous determination of 32 antibiotics in aquaculture products using LC-MS/MS

Ganna Fedorova, Vaclav Nebesky, Tomas Randak and Roman Grabic
From the journal Chemical Papers

Abstract

An analytical multiclass, multi-residue method for the determination of antibiotics in aquaculture products was developed and validated. A fast, cheap, and straightforward extraction procedure followed by liquid chromatography-tandem mass spectrometry analysis was proposed. This method covers 32 antibiotics of different classes, which are frequently used in aquaculture. Three different extraction procedures were compared, and the extraction with acetonitrile (0.1 vol. % formic acid) showed the best results. The selected extraction procedure was validated at four different fortification levels (10 μg kg−1, 25 μg kg−1, 50 μg kg−1, and 100 μg kg−1). Recoveries of the tested antibiotics ranged from 70 % to 120 %, with the relative standard deviation (RSD) of triplicates lower than 20 %. The limits of quantification (LOQ) ranged from 0.062 μg kg−1 to 4.6 μg kg−1, allowing for the analysis of trace levels of these antibiotics in aquaculture products. The method was applied to the analysis of selected antibiotics in fish and shrimp meat available in the Czech market.

[1] Bilandžić, N., Kolanović, B. S., Varenina, I., Scortichini, G., Annunziata, L., Brstilo, M., & Rudan, N. (2011). Veterinary drug residues determination in raw milk in Croatia. Food Control, 22, 1941–1948 DOI: 10.1016/j.foodcont.2011.05.007. http://dx.doi.org/10.1016/j.foodcont.2011.05.00710.1016/j.foodcont.2011.05.007Search in Google Scholar

[2] Cabello, F. C. (2006). Heavy use of prophylactic antibiotics in aquaculture: a growing problem for human and animal health and for the environment. Environmental Microbiology, 8, 1137–1144. DOI: 10.1111/j.1462-2920.2006.01054.x. http://dx.doi.org/10.1111/j.1462-2920.2006.01054.x10.1111/j.1462-2920.2006.01054.xSearch in Google Scholar

[3] Cañada-Cañada, F., Muñoz de la Peña, A. M., & Espinosa-Mansilla, A. (2009). Analysis of antibiotics in fish samples. Analytical and Bioanalytical Chemistry, 395, 987–1008. DOI: 10.1007/s00216-009-2872-z. http://dx.doi.org/10.1007/s00216-009-2872-z10.1007/s00216-009-2872-zSearch in Google Scholar

[4] Dasenaki, M. E., & Thomaidis, N. S. (2010). Multi-residue determination of seventeen sulfonamides and five tetracyclines in fish tissue using a multi-stage LC-ESI-MS/MS approach based on advanced mass spectrometric techniques. Analytica Chimica Acta, 672, 93–102. DOI: 10.1016/j.aca.2010.04.034. http://dx.doi.org/10.1016/j.aca.2010.04.03410.1016/j.aca.2010.04.034Search in Google Scholar

[5] De Alwis, H., & Heller, D. N. (2010). Multiclass, multiresidue method for the detection of antibiotic residues in distillers grains by liquid chromatography and ion trap tandem mass spectrometry. Journal of Chromatography A, 1217, 3076–3084. DOI: 10.1016/j.chroma.2010.02.081. http://dx.doi.org/10.1016/j.chroma.2010.02.08110.1016/j.chroma.2010.02.081Search in Google Scholar

[6] European Commision (2003). Commission Decision of 13 March 2003 amending Decision 2002/657/EC as regards the setting of minimum required performance limits (MRPLs) for certain residues in food of animal origin. Official Journal of the European Communities, 2003(L71), 17–18. Search in Google Scholar

[7] European Commision (2010). Commission Decision (EU) No 37/2010 of 22 December 2009 on pharmacologically active substances and their classification regarding maximum residue limits in foodstuffs of animal origin. Official Journal of the European Communities, 2010(L15), 1–72. Search in Google Scholar

[8] European Council (1996). Council Directive 96/23/EC of 29 April 1996 on measures to monitor certain substances and residues thereof in live animals and animal products and repealing Directives 85/358/EEC and 86/469/EEC and Decisions 89/187/EEC and 91/664/EEC (1996). Official Journal of the European Communities, 1996(L125), 10–32. Search in Google Scholar

[9] Greenlees, K. J. (2003). Animal drug human food safety toxicology and antimicrobial resistance-The square peg. International Journal of Toxicology, 22, 131–134. DOI: 10.1080/10915810305091. http://dx.doi.org/10.1080/1091581030509110.1080/10915810305091Search in Google Scholar

[10] Heuer, O. E., Kruse, H., Grave, K., Collignon, P., Karunasagar, I., & Angulo, F. J. (2009). Human health consequences of use of antimicrobial agents in aquaculture. Clinical Infectious Diseases, 49, 1248–1253. DOI: 10.1086/605667. http://dx.doi.org/10.1086/60566710.1086/605667Search in Google Scholar

[11] Jo, M. R., Lee, H. J., Lee, T. S., Park, K., Oh, E. G., Kim, P. H., Lee, D. S., & Horie, M. (2011). Simultaneous determination of macrolide residues in fish and shrimp by liquid chromatography-tandem mass spectrometry. Food Science and Biotechnology, 20, 823–827. DOI: 10.1007/s10068-011-0114-6. http://dx.doi.org/10.1007/s10068-011-0114-610.1007/s10068-011-0114-6Search in Google Scholar

[12] Johnston, L., Mackay, L., & Croft, M. (2002). Determination of quinolones and fluoroquinolones in fish tissue and seafood by high-performance liquid chromatography with electrospray ionisation tandem mass spectrometric detection. Journal of Chromatography A, 982, 97–109. DOI: 10.1016/s0021-9673(02)01407-3. http://dx.doi.org/10.1016/S0021-9673(02)01407-310.1016/S0021-9673(02)01407-3Search in Google Scholar

[13] Kaufmann, A., Butcher, P., Maden, K., & Widmer, M. (2008). Quantitative multiresidue method for about 100 veterinary drugs in different meat matrices by sub 2-μm particulate high-performance liquid chromatography coupled to time of flight mass spectrometry. Journal of Chromatography A, 1194, 66–79. DOI: 10.1016/j.chroma.2008.03.089. http://dx.doi.org/10.1016/j.chroma.2008.03.08910.1016/j.chroma.2008.03.089Search in Google Scholar PubMed

[14] Li, L. Z., Fu, J. L., Qiu, Y. X., & Wang, J. L. (2011). Analysis of streptolydigin degradation and conversion in cultural supernatants of Streptomyces lydicus AS 4.2501. Chemical Papers, 65, 652–659. Doi: 10.2478/s11696-011-0050-1. http://dx.doi.org/10.2478/s11696-011-0050-110.2478/s11696-011-0050-1Search in Google Scholar

[15] Martínez Vidal, J. L., Aguilera-Luiz, M. M., Romero-González, R., Ĝarrido Frenich, A. (2009). Multiclass analysis of antibiotic residues in honey by ultraperformance liquid chromatography-tandem mass spectrometry. Journal of Agricultural and Food Chemistry, 57, 1760–1767. DOI: 10.1021/jf8034572. http://dx.doi.org/10.1021/jf803457210.1021/jf8034572Search in Google Scholar

[16] Monko, M. (2011). Selective phospholipid extractions for cleanup or enrichment using HybridSPE®-Phospholipid. Reporter, 45(March), 16–17. Search in Google Scholar

[17] Nakazawa, H., Ino, S., Kato, K., Watanabe, T., Ito, Y., & Oka, H. (1999). Simultaneous determination of residual tetracyclines in foods by high-performance liquid chromatography with atmospheric pressure chemical ionization tandem mass spectrometry. Journal of Chromatography B: Biomedical Sciences and Applications, 732, 55–64. DOI: 10.1016/s0378-4347(99)00260-1. http://dx.doi.org/10.1016/S0378-4347(99)00260-110.1016/S0378-4347(99)00260-1Search in Google Scholar

[18] Niessen, W. M. A., Manini, P., & Andreoli, R. (2006). Matrix effects in quantitative pesticide analysis using liquid chromatography-mass spectrometry. Mass Spectrometry Reviews, 25, 881–899. DOI: 10.1002/mas.20097. http://dx.doi.org/10.1002/mas.2009710.1002/mas.20097Search in Google Scholar PubMed

[19] Peters, R. J. B., Bolck, Y. J. C., Rutgers, P., Stolker, A. A. M., & Nielen, M. W. F. (2009). Multi-residue screening of veterinary drugs in eg, fish and meat using high-resolution liquid chromatography accurate mass time-of-flight mass spectrometry. Journal of Chromatography A, 1216, 8206–8216. DOI: 10.1016/j.chroma.2009.04.027. http://dx.doi.org/10.1016/j.chroma.2009.04.02710.1016/j.chroma.2009.04.027Search in Google Scholar PubMed

[20] Romero-González, R., López-Martínez, J. C., Gómez-Milán, E., Garrido-Frenich, A., & Martínez-Vidal, J. L. (2007). Simultaneous determination of selected veterinary antibiotics in gilthead seabream (Sparus Aurata) by liquid chromatographymass spectrometry. Journal of Chromatography B, 857, 142–148. DOI: 10.1016/j.jchromb.2007.07.011. http://dx.doi.org/10.1016/j.jchromb.2007.07.01110.1016/j.jchromb.2007.07.011Search in Google Scholar PubMed

[21] Villar-Pulido, M., Gilbert-López, B., García-Reyes, J. F., Ramos Martos, N., & Molina-Díaz, A. (2011). Multiclass detection and quantitation of antibiotics and veterinary drugs in shrimps by fast liquid chromatography time-of-flight mass spectrometry. Talanta, 85, 1419–1427. DOI: 10.1016/j.talanta.2011.06.036. http://dx.doi.org/10.1016/j.talanta.2011.06.03610.1016/j.talanta.2011.06.036Search in Google Scholar PubMed

[22] Yu, H. A., Tao, Y. F., Chen, D.M., Wang, Y. L., Huang, L. L., Peng, D. P., Dai, M. H., Liu, Z. L., Wang, X., & Yuan, Z. H. (2011). Development of a high performance liquid chromatography method and a liquid chromatography-tandem mass spectrometry method with the pressurized liquid extraction for the quantification and confirmation of sulfonamides in the foods of animal origin. Journal of Chromatography B, 879, 2653–2662. DOI: 10.1016/j.jchromb.2011.07.032. http://dx.doi.org/10.1016/j.jchromb.2011.07.03210.1016/j.jchromb.2011.07.032Search in Google Scholar PubMed

Published Online: 2013-9-17
Published in Print: 2014-1-1

© 2013 Institute of Chemistry, Slovak Academy of Sciences