苯二氮_类药物的气相色谱-质谱联用法定性分析方法研究

目的: 建立气相色谱-质谱联用法定性分析在改善睡眠类保健食品及中成药中非法添加的苯二氮草类10种药物。 方法: 采用溶剂超声或液-液萃取方式对样品进行提取富集,气相色谱-质谱联用(GC-MS),Scan模式进行定性检测,采用DB-5 ms毛细管色谱柱(30 m×0.25 mm×0.25 μm),程序升温:初始温度120 ℃(1 min),10 ℃·min^-1升至230 ℃,15 ℃·min^-1升至270 ℃(20 min),选择EI离子源,溶剂延迟2.5 min,质谱扫描40～350 amu。 结果: 在选定的色谱条件下,能够在30 min内快速检测苯二氮 类10种药物,并得到较好的分离;样品筛查结果发现2批样品中分别添加了氯硝西泮和劳拉西泮。 结论: 该法快速﹑准确,专属性强,可用于快速筛查违禁药物。

Objective: The research aimed to establish a GC-MS method for detection of 10 kinds benzodiazepine drugs added illegally in health foods and traditional Chinese medicines of improve sleeping. Method: Using solvent extraction or liquid-liquid extraction method to get the enrichment of samples.Qualitative analysis by GC-MS and scan mode was carried out .The analytical capillary column was DP-5 ms (30 m×0.25 mm,0.25 μm ).The oven temperature was set at 120 ℃ (1 min) initially,it was programmed rising by 10 ℃·min^-1 up to 230 ℃,rising by 15 ℃·min^-1 up to 270 ℃(20 min).The EI ion source was selected and the solvent was delayed by 2.5 min.The MS scanning was set at the range of 40-350 amu. Result: At the selected chromatographic conditions,10 kinds of chemical drugs could get a better separation within 30 min.Clonazepam and lorazepam were detected in two batches of samples. Conclusion: This method is rapid,accurate,selective and suitable for fast qualitative detection of drugs added illegally.

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