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采用超高效液相色谱串联质谱联用仪分析猪肉的地西泮、去甲羟地西泮和去甲地西泮。猪肉先经过β-盐酸葡萄糖醛苷酶水解,然后用乙酸乙酯振荡提取酶解液,分离上层有机溶剂并蒸干,用乙腈溶解残渣,溶液过滤后用超高效液相色谱串联质谱法(UPLC-MS/MS)进行检测。通过对提取方式和液相色谱分离条件的优化,建立猪肉中地西泮、去甲羟地西泮和去甲地西泮的UPLC-MS/MS检测方法。方法中空白样品的加标回收率为80.8%～90.3%,相对标准偏差(RSD)在5.9%～13.4%,定量限为1.0μg/kg。
Analysis of pork diazepam, nor-hydroxy-diazepam and nor-diazepam by ultra performance liquid chromatography-tandem mass spectrometry. The pork is first hydrolyzed by β-HCI glucosidase, then the enzyme solution is extracted by shaking with ethyl acetate, the upper organic solvent is separated and evaporated to dryness, the residue is dissolved in acetonitrile, the solution is filtered and characterized by ultra performance liquid chromatography tandem mass spectrometry (UPLC -MS / MS). UPLC-MS / MS method was established for the determination of diazepam, nor-hydroxy-diazepam and nor-diazepam in pork by optimizing the extraction method and liquid chromatography separation conditions. The spiked recoveries of blank samples in the method ranged from 80.8% to 90.3%, the relative standard deviations (RSDs) ranged from 5.9% to 13.4%, and the limits of quantitation was 1.0 μg / kg.