Multi-residue determination of veterinary drugs in cheese by QuEChERS and liquid chromatography- tandem mass spectrometry

doi:10.3724/SP.J.1123.2014.10022

Abstract

Abstract:

A rapid and sensitive method has been developed for the simultaneous determination of 50 veterinary drugs (including macrolides, quinolones, sulfonamides, and tetracyclines) in cheese using a modified QuEChERS method coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS). After adding Na₂EDTA buffer solution and ceramic homogenizer, the cheese sample was extracted by 5% (v/v) acetic acid-acetonitrile, sodium chloride and anhydrous sodium sulfate were used for salting-out process. The resulting supernatant solution was purified by C₁₈ sorbent and the re-dissolved solution was analyzed by LC-MS/MS under dynamic multi-reaction monitoring (dynamic MRM) mode via positive electrospray ionization with a ZORBAX-SB-C₁₈ column. The limits of quantification (LOQ, S/N=10) of the target compounds ranged from 0.05 μg/kg to 20 μg/kg in cheese. At spiked levels of 20, 50, 100 μg/kg (n=6), the percentages of drug with a recovery between 70% and 120% were 94%, 92%, and 96%, respectively. The relative standard deviations (RSDs) were between 1% and 14%. This method has been applied to determine seven real samples from markets. Roxithromycin and flumequine have been detected in two samples separately. The results demonstrated that this simple, rapid and accurate method is suitable for the detection of multi-class veterinary drugs in cheese.

Key words: cheese, liquid chromatography-tandem mass spectrometry (LC-MS/MS), multi-residues, QuEChERS, veterinary drug

CLC Number:

O658

CAO Yafei, KANG Jian, CHANG Qiaoying, HU Xueyan, WANG Zhibin, FAN Chunlin, WANG Minglin. Multi-residue determination of veterinary drugs in cheese by QuEChERS and liquid chromatography- tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2015, 33(2): 132-139.

References

[1] Stolker A A M, Brinkman U A T. J Chromatogr A, 2005, 1067(1/2): 15
[2] Electronic Code of Federal Regulations. Tolerances for Residues of New Animal Drugs in Food. (2011-07-28) [2014-07-10]. http://ecfr.gpoaccess.gov/cgi/t/text/text-idx?c=ecfr&sid=407e94c4cd1bff327c7146f42bcc0d56&tpl=/ecfrbrowse/Title21/21cfr556_main_02.tpl
[3] European Union. Commision Regulation. (2009-12-22) [2014-06-20]. http://ec.europa.eu/health/files/mrl/mrl_20101212_consol.pdf
[4] The Japan Food Chemical Research Foundation. Maximum Residue Limits (MRLs) List of Agricultural Chemicals in Foods. (2011-09-30) [2014-06-21]. http://www.m5.ws001.squarestart.ne.jp/foundation/search.html
[5] Ministry of Agriculture. No. 235 Bulletin of the Ministry of Agriculture of the People's Republic of China (农业部. 中华人民共和国农业部公告第235号). (2002-12-24) [2014-08-20]. http://www.moa.gov.cn/zwllm/tzgg/gg/200302/t20030226_59300.htm
[6] Anastasio A, Esposito M, Amorena M, et al. J Agric Food Chem, 2002, 50 (18): 5241
[7] Berardi G, Bogialli S, Curini R, et al. J Agric Food Chem, 2006, 54(13): 4537
[8] Bogialli S, Coradazzi C, Di Corcia A, et al. J AOAC Int, 2007, 90(3): 864
[9] Anastassiades M, Lehotay S J, Stajnbaher D, et al. J AOAC Int, 2003, 86(2): 412
[10] Lehotay S J, Mastovska K, Yun S J. J AOAC Int, 2005, 88(2): 630
[11] Lehotay S J. J AOAC Int, 2007, 90(2): 485
[12] Li Y, Zheng F, Wang M L, et al. Chinese Journal of Chromatography (李岩, 郑锋, 王明林, 等. 色谱), 2009, 27(2): 127
[13] Zhao Z Y, Shi Z H, Kang J, et al. Chinese Journal of Chromatography (赵志远, 石志红, 康健, 等. 色谱), 2013, 31(4): 372
[14] Huang H H, Zhang J, Xu D M, et al. Chinese Journal of Chromatography (黄何何, 张缙, 徐敦明, 等. 色谱), 2014, 32(7): 707
[15] Chen L, Song F, Liu Z, et al. J Chromatogr A, 2012, 1225: 132
[16] Cherta L, Portoles T, Beltran J, et al. J Chromatogr A, 2013, 1314: 224
[17] Stubbings G, Bigwood T. Anal Chim Acta, 2009, 637(1/2): 68
[18] Aguilera-Luiz M M, Vidal J L M, Romero-Gonzalez R, et al. J Chromatogr A, 2008, 1205(1/2): 10
[19] Gao F D, Zhao Y, Shao B, et al. Chinese Journal of Chromatography (高馥蝶, 赵妍, 邵兵, 等. 色谱), 2012, 30(6): 560
[20] Yan X F. China Journal of Veterinary Medicine (闫小峰. 中国兽药杂志), 2010, 44(5): 47
[21] Bo H B, Chen L R. Chinese Journal of Health Laboratory Technology (薄海波, 陈立仁. 中国卫生检验杂志), 2004, 14(6): 699
[22] Tsai W H, Huang T C, Chen H H, et al. J Chromatogr A, 2010, 1217(3): 415
[23] Taylor P J. Clin Biochem, 2005, 38(4): 328
[24] Gomez Perez M L, Romero-Gonzalez R, Martinez Vidal J L, et al. J Sep Sci, 2013, 36(7): 1223