| 引用本文: | 申兰慧,彭耀文,杨敏智.睡眠宝胶囊中非法掺入化学药品的检测方法研究[J].中国现代应用药学,2015,32(6):724-727. |
| SHEN Lanhui,PENG Yaowen,YANG Minzhi.Study on Detection Method of Chemical Drugs Illegally Added in Shuimianbao Capsules[J].Chin J Mod Appl Pharm(中国现代应用药学),2015,32(6):724-727. |
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| 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。 |
| 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 |
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| Study on Detection Method of Chemical Drugs Illegally Added in Shuimianbao Capsules |
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SHEN Lanhui1, PENG Yaowen1,2, YANG Minzhi1
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1.Jiangsu Wuxi Institute for Drug Control, Wuxi 214028, China;2.School of Pharmaceutical Sciences, Jiangnan University, Wuxi 214122, China
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| 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. |
| Key words: clozapine diazepam estazolam Shuimianbao capsules UPLC-MS |
