睡眠宝胶囊中非法掺入化学药品的检测方法研究

Study on Detection Method of Chemical Drugs Illegally Added in Shuimianbao Capsules

关键词:  氯氮平  地西泮  艾司唑仑  睡眠宝胶囊  超高压液相色谱-质谱联用

Key words:  clozapine  diazepam  estazolam  Shuimianbao capsules  UPLC-MS

摘要:

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，1.8 μm)，流动相20 mmol·L^-1醋酸铵溶液-甲醇(50∶50)，流速0.3 mL·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。

Abstract:

OBJECTIVE To establish a method for detection of diazepam, estazolam and clozapine illegally added in Shuimianbao capsules by TLC combined with UPLC-MS. METHODS Silica gel(GF₂₅₄) TLC was used, a mixture of ethyl acetate-ethanol-ammonium hydroxide(50∶2∶0.5) as developer, detection under 254 nm. Aglient ZORBAX SB C₁₈ column (100 mm×2.1 mm, 1.8 μm) was used, and the mobile phase consisted of 20 mmol·L^-1 ammonium acetate solution-methanol(50∶50), flow rate was 0.3 mL·min^-1; detection wavelength was 225 nm; column temperature was 35?℃, ESI⁺. RESULTS The diazepam, estazolam and clozapine illegally added in Shuimianbao capsules were displayed obvious dots under 254 nm. Then they were verified by UPLC-MS. CONCLUSION The method is simple and accurate. It can be used for rapid screening and rapid identification of diazepam, estazolam and clozapine illegally added in Shuimianbao capsules.