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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×0.25μm),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30min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: To establish a qualitative analysis of 10 kinds of benzodiazepines illegally added in improving sleep-type health food and proprietary Chinese medicines by gas chromatography-mass spectrometry. Methods: The samples were extracted and enriched by solvent ultrasonic or liquid-liquid extraction. The samples were determined by gas chromatography-mass spectrometry (GC-MS) and Scan mode. The chromatographic conditions were as follows: DB-5 ms capillary column × 0.25μm). The program temperature was raised: the initial temperature was 120 ℃ (1 min), 10 ℃ .min-1 was raised to 230 ℃, 15 ℃ .min-1 was raised to 270 ℃ 2.5 min, MS scan 40 ~ 350 amu. Results: Under the selected chromatographic conditions, 10 kinds of benzodiazepines were rapidly detected within 30 min, and better separation was obtained. The sample screening results showed that clonazepam and Lazepam. Conclusion: The method is fast, accurate and specific and can be used for rapid screening of illicit drugs.