液相色谱-串联质谱法对动物源性食品中14种苯二氮类药物及其代谢物残留量的同时检测  

Determination of Benzodiazepines and Metabolites Residues in Foodstuffs of Animal Origin by Liquid Chromatography-Tandem Mass Spectrometry

作　　者：邓晓军[1] 郭德华[1] 朱坚[1] 王敏[1] 盛永刚[1] 樊祥[1] 生茂强[2] 

机构地区：[1]上海出入境检验检疫局,上海200135 [2]上海水产大学食品学院,上海200090

出　　处：《分析测试学报》2008年第11期1162-1166,1170,共6页Journal of Instrumental Analysis

摘　　要：建立了液相色谱-串联质谱(LC-MS/MS)同时检测动物源性食品中14种苯二氮类药物及其代谢物残留量的测定方法。在pH 5.2乙酸铵缓冲溶液中药物残留经酶解后,用氨水调节pH值大于9.5。溶液经乙酸乙酯-异丙醇(体积比5∶1)提取和阳离子交换柱(MCX)净化,并用多反应监测技术所确定的定性离子对检测物进行定性和同位素内标法定量。方法的定量下限为1.0μg/kg,线性范围为1.0～20.0μg/L,各基质的加标平均回收率为64%～117%,相对标准偏差为3.6%～12.3%。A liquid chromatography coulped to tandem mass spectrometry （ LC - MS/MS） method was developed for the determination of benzodiazepines and metabolite residues in foodstuffs of animal origin. The samples were hydrolysised by enzyme in pH 5.2 ammonium acetate buffer followed by an adjustment of pH value more than 9.5 with ammonium hydroxide. The benzodiazepines and metabolite residues were extracted by acetic etherisopropol （5： 1, by volume） and cleaned up by a mixed cation-exchange solid phase extraction column （MCX）. Then the analytes were recognized and quantified by LC -MS/MS with multiple reaction monitoring（MRM） mode using labelled corresponding isotopes as internal standard. The method showed good linearity over the concentration range of 1.0 -20.0 μg/L for all compounds. The limit of quantification （LOQ） of the method was down to 0. 1μg/kg. The spiked recoveries ranged from 64% to 117% with RSD of 3.6% - 12. 3%. The method is reliable and sensitive for daily inspection of benzodiazepine residues.

关 键 词：液相色谱-串联质谱 苯二氮革 残留 食品 

分 类 号：O657.63[理学—分析化学] R971.3[理学—化学]