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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 method for simultaneous determination of 14 benzodiazepines and their metabolites in animal-derived foods by liquid chromatography-tandem mass spectrometry (LC-MS / MS) was developed. In pH 5.2 ammonium acetate buffer solution after the drug residues by enzymolysis, with ammonia to adjust the pH value is greater than 9.5. The solution was extracted with ethyl acetate-isopropanol (5: 1 by volume) and purified by cation exchange column (MCX). Qualitative and isotopic internal standard was used to quantify the test substance by qualitative ions determined by multiple reaction monitoring. The lower limit of quantitation was 1.0 μg / kg with the linear range of 1.0 ~ 20.0 μg / L. The average recoveries for each substrate ranged from 64% to 117% with relative standard deviations of 3.6% to 12.3%.