高效液相色谱–串联质谱测定动物源性食品中硝基咪唑类药物及其代谢物残留量

Determination of nitroimidazoles and their metabolites in animal-borne food by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  硝基咪唑  高效液相色谱–串联质谱  甲硝唑  地美硝唑  洛硝哒唑  羟基甲硝唑  1-甲基-5-硝基-2-羟甲基咪唑

英文关键词:nitroimidazole  high performance liquid chromatography-electrospray ionization triple?quadruple tandem mass spectrometric  metronidazole  dimetridazole  ronidazole  hydroxyl metronidazole  2-hyd??ro?xy-methyl-1-methyl-5-nitroimidazole

中文摘要:

      目的 建立高效液相色谱–电喷雾电离串联四级杆质谱测定动物源性食品中甲硝唑(MNZ)、地美硝唑(DMZ)、洛硝哒唑(RNZ)3种硝基咪唑类化合物及2种代谢物羟基甲硝唑MNZOH(甲硝唑代谢物)、1-甲基-5-硝基-2-羟甲基咪唑HMMNI(地美硝唑代谢物)残留量的检测方法。方法 样品采用乙酸乙酯提取, 甲醇和正己烷分配除脂, 再经HLB固相萃取柱净化, 采用高效液相色谱–串联质谱法在选择离子监测(MRM)正离子模式(ESI+)下检测。结果 该方法在0.1~100.0 μg/L范围内具有良好的线性关系, 相关系数r >0.99。在添加水平为0.1、0.5、10.0 μg/kg时, 方法的回收率在61.1 %~108.0 %之间, 相对标准偏差为1.9 %~6.3 % ; 定量下限(S/N=10)为0.1 μg/kg。结论 该方法适合动物源性食品中硝基咪唑类药物及其代谢物残留量的检测。

英文摘要:

      Objective To establish a high performance liquid chromatography-electrospray ionization triple?quadruple tandem mass spectrometric (HPLC-MS/MS) method for the determination of metronidazole ?(MNZ), dimetridazole (DMZ), ronidazole (RNZ), hydroxyl metronidazole (MNZOH) and 2-hydroxymethyl-1-methyl?5-nitroimidazole (HMMNI) in animal-borne food. Methods Animal tissue samples were extracted by ethyl acetate, and the fat was removed by methanol-hexane distribution. The extract was cleaned-up by HLB SPE cartridge. Identification of nitroimidazoles and their metabolites was achieved by electrospray ionization tandem mass spectrometer under multiple reaction monitoring (MRM) mode. Results The calibration curves showed a good linearity in the range of 0.1~100.0 μg/kg with r >0.99. The average recoveries of spiked samples at three spiked levels of 0.1, 0.5 and 10.0 μg/kg were between 61.1% to 108.0% with the relative standard deviations (RSDs) of 1.9%~6.3%. The limits of quantitation (LOQs) were 0.1 μg/kg for MNZ, DMZ, RNZ, MNZOH and HMMNI. Conclusion The method could be used to simultaneously confirm the multi-residue of nitromidazoles and their metabolites in animal-borne food.