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建立了高效液相色谱-串联质谱(HPLC/MS/MS)测定鱼类样品中地西泮及其代谢物去甲地西泮、替马西泮和奥沙西泮的分析方法。样品用1%氨化乙酸乙酯提取,HLB固相萃取柱净化,乙酸乙酯洗脱。在正离子模式下以电喷雾串联质谱仪进行测定,以氘代地西泮、氘代去甲地西泮、氘代替马西泮和氘代奥沙西泮为内标物,内标法定量。以大菱鲆和鳜鱼为研究对象,在1.0、10.0和50.0μg/kg添加水平下,方法平均回收率为85.7%～105.6%(批内),相对标准偏差为2.1%～7.6%(批内),方法定量限为1.0μg/kg(S/N>10)。实验结果表明:该方法简单、快速、准确度高、重复性好,适合于鱼类样品中地西泮及其代谢物残留的检测。
A method for the determination of diazepam and its metabolites n-diazepam, temazepam and oxazepam in fish samples by high performance liquid chromatography-tandem mass spectrometry (HPLC / MS / MS) was established. Samples were extracted with 1% ammoniated ethyl acetate, purified by HLB solid phase extraction cartridge, and eluted with ethyl acetate. In the positive ion mode electrospray tandem mass spectrometry determination, deuterated diazepam, deuterated desazepam, deuterium instead of macrazone and deuterated oxazepam as internal standard, internal standard method. Taking turbot and anchovy as the research objects, the average recoveries were between 85.7% and 105.6% at the 1.0, 10.0 and 50.0 μg / kg levels, with relative standard deviations between 2.1% and 7.6% ), The limit of quantification was 1.0 μg / kg (S / N> 10). The experimental results show that the method is simple, rapid, accurate and reproducible. It is suitable for the determination of diazepam and its metabolites in fish samples.