Determination of nitroimidazoles and their metabolites in animal-derived foods by liquid chromatography-tandem mass spectrometry coupled with dispersive solid phase extraction

doi:10.3724/SP.J.1123.2017.12028

Abstract

Abstract:

A method for the quantitative analysis of nitroimidazoles and their metabolites in four kinds of animal-derived foods by liquid chromatography-tandem mass spectrometry (LC-MS/MS) coupled with dispersive solid phase extraction (dSPE) was established. The samples (2.0 g) were extracted with ethyl acetate. The extracts were degreased with hexane and purified with 50 mg primary-secondary amine (PSA), and then filtered through a hydrophilic polytetrafluoroethylene (PTFE) membrane. The analytes were separated on a C18 column, and detected in selected reaction monitoring (SRM) mode via positive electrospray ionization. The matrix matching and internal standard method was used. The nitroimidazoles and their metabolites showed good linearity in the range of 0.5-20.0 μg/L with correlation coefficients greater than 0.99. The limits of detection of the nitroimidazoles and their metabolites in animal-derived foods were between 0.1 and 0.5 μg/kg. The recoveries varied between 84.2% and 120.8%, with relative standard deviations (n=6) ranging from 2.0% to 16.2% at spiked levels of 1.0, 3.0, and 10.0 μg/kg. The proposed method is accurate, fast, cheap, easy, and can satisfy the requirements of monitoring nitroimidazoles and their metabolites in animal-derived foods.

Key words: animal derived foods, dispersive solid phase extraction (dSPE), liquid chromatography-tandem mass spectrometry (LC-MS/MS), nitroimidazoles and their metabolites

CLC Number:

O658

FANG Li, QIU Fengmei, YU Xinwei, ZHANG Zhichao. Determination of nitroimidazoles and their metabolites in animal-derived foods by liquid chromatography-tandem mass spectrometry coupled with dispersive solid phase extraction[J]. Chinese Journal of Chromatography, 2018, 36(5): 431-438.

References

[1] Cronly M, Behan P, Foley B, et al. J Chromatogr A, 2009, 1216(46):8101
[2] Xia X, Li X W, Zhang S X, et al. J Chromatogr A, 2008, 1208(1/2):101
[3] Ministry of Agriculture. No. 235 Bulletin of the Ministry of Agriculture of the People's Republic of China. (2002-12-24)[2017-12-20]. http://www.moa.gov.cn/zwllm/nybz/200803/t20080304_1028649.htm 农业部. 中华人民共和国农业部公告第235号. (2002-12-24)[2017-12-20]. http://www.moa.gov.cn/zwllm/nybz/200803/t20080304_1028649.htm
[4] Zhang C, Pan J R, Shuai R Q, et al. Journal of Nuclear Agricultural Sciences, 2016, 30(2):323 张弛, 潘家荣, 帅瑞琪, 等. 核农学报, 2016, 30(2):323
[5] Wang Y B, He F Y, Wan Y P, et al. Food Addit Contam A, 2011, 28(5):619
[6] Thompson C S, Traynor I M, Fodey T L, et al. Anal Chim Acta, 2009, 637(1/2):259
[7] Wang J C, Ma S Y, Wang D J, et al. Chinese Journal of Animal and Veterinary Sciences, 2008, 39(12):1772 汪纪仓, 马素英, 王大菊, 等. 畜牧兽医学报, 2008, 39(12):1772
[8] He D, Li X Y, Xian Y P, et al. Journal of Instrumental Analysis, 2015, 34(8):911 何东, 李秀英, 冼燕萍, 等. 分析测试学报, 2015, 34(8):911
[9] Hernandez-Mesa M, Garcia-Campana A M, Cruces-Blanco C. Food Chem, 2014, 145(4):161
[10] Wang Y, Zheng C Y, He F, et al. Food Science, 2011, 32(20):197 王杨, 郑重莺, 何丰, 等. 食品科学, 2011, 32(20):197
[11] Lu K, Tong Q Y. Journal of Instrumental Analysis, 2011, 30(11):1320 卢坤, 童群义. 分析测试学报, 2011, 30(11):1320
[12] Li C Y, Wu M, Yan L J, et al. Journal of Food Safety and Quality, 2012, 3(1):17 黎翠玉, 吴敏, 严丽娟, 等. 食品安全质量检测学报, 2012, 3(1):17
[13] Guo X C, Xia Z Y, Wang H H, et al. Talanta, 2017, 166:101
[14] Zhang L, Kong X H, Wang H, et al. Chinese Journal of Analytical Chemistry, 2014, 42(12):1735 张璐, 孔祥虹, 王菡, 等. 分析化学, 2014, 42(12):1735
[15] Liu Y M, Gao Y Z, Li J, et al. Chinese Journal of Chromatography, 2010, 28(6):596 刘永明, 曹彦忠, 李金, 等. 色谱, 2010, 28(6):596
[16] Zhang Y, Yue Z F, Lan F, et al. Chinese Journal of Analytical Chemistry, 2012, 40(5):724 张毅, 岳振峰, 蓝芳, 等. 分析化学, 2012, 40(5):724
[17] Cui C Y, Zhang H Y, Wu X Q, et al. Chinese Journal of Chromatography, 2017, 35(5):487 崔春艳, 张红医, 吴兴强, 等. 色谱, 2017, 35(5):487
[18] Luo H T, Huang X L, Wu H Q, et al. Chinese Journal of Chromatography, 2017, 35(8):816 罗辉泰, 黄晓兰, 吴慧勤, 等. 色谱, 2017, 35(8):816