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目的建立薄层色谱结合超高压液相色谱-质谱联用法快速筛查及鉴定睡眠宝胶囊中非法掺加的氯氮平、地西泮、艾司唑仑。方法采用硅胶GF254板,乙酸乙酯-无水乙醇-氨水(50∶2∶0.5)为展开剂,在254 nm下检视。色谱条件为:Aglient ZORBAX SB C18柱(100 mm×2.1 mm,1.8μm),流动相20 mmol·L-1醋酸铵溶液-甲醇(50∶50),流速0.3 m L·min-1,检测波长225 nm,柱温35℃,正离子扫描检测。结果睡眠宝胶囊非法掺入氯氮平、地西泮、艾司唑仑在254 nm下显明显的斑点,通过UPLC-PDA-Q TOF MS可进一步快速确证。结论本方法操作简便,结果可靠,可用于快速筛查及确证睡眠宝胶囊中非法掺入氯氮平、地西泮及艾司唑仑。
OBJECTIVE To establish a rapid screening and identification of clozapine, diazepam and estazolam illegally added to Siberian Capsules by TLC and UHPLC-MS. Methods silica gel GF254 plate, ethyl acetate - absolute ethanol - ammonia (50: 2: 0.5) as a developing agent, at 254 nm view. The chromatographic conditions were: Aglient ZORBAX SB C18 column (100 mm × 2.1 mm, 1.8 μm), mobile phase of 20 mmol·L -1 ammonium acetate solution (50:50), flow rate of 0.3 m L · min -1, detection wavelength 225 nm, column temperature 35 ℃, positive ion scan detection. Results Sleeping capsule was illegally mixed with clozapine, diazepam and estazolam at 254 nm, which was confirmed by UPLC-PDA-Q TOF MS. Conclusion The method is simple and reliable, and can be used for rapid screening and confirmation of clozapine, diazepam and estazolam.