UPLC-MS/MS检测镇静安神类中成药中违禁添加地西泮、氯硝西泮和艾司唑仑
投稿时间:2011-05-29  修订日期:2011-06-15  点此下载全文
引用本文:陈睿,储忠英,张继春,田兰.UPLC-MS/MS检测镇静安神类中成药中违禁添加地西泮、氯硝西泮和艾司唑仑[J].药学实践杂志,2011,29(6):457~459
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作者单位
陈睿 上海市松江食品药品检验所,上海 201600 
储忠英 上海市松江食品药品检验所,上海 201600 
张继春 上海市松江食品药品检验所,上海 201600 
田兰 上海市松江食品药品检验所,上海 201600 
中文摘要:目的 建立镇静安神类中成药中添加地西泮、氯硝西泮和艾司唑仑的专属检测方法。 方法 采用超高效液相色谱-串联四级杆质谱,C18色谱柱(2.1 mm×50 mm,1.7 μm),10 mmol/L乙酸铵溶液-乙腈(90:10)梯度洗脱,流速0.4 ml/min,检测波长254 nm;离子源为ESI源,正离子检测,对中成药中添加地西泮、氯硝西泮和艾司唑仑定性、定量检测。 结果 地西泮、氯硝西泮和艾司唑仑线性范围分别为109.8~878.4、102.1~816.8、106.9~855.2 ng/ml,地西泮、氯硝西泮和艾司唑仑的检出限为分别0.06、2.5×10-3 、2.8×10-3 ng,定量限分别为0.19、8.2×10-3 、9.2×10-3 ng,3种药物平均回收率在95.7%~103.7%之间。 结论 本方法选择性强、灵敏度高、处理方法简单,测定快速,可用于镇静安神类中成药中添加地西泮、氯硝西泮和艾司唑仑的测定。
中文关键词:超高效液相色谱-串联四级杆质谱  中成药  镇静安神类  违禁添加物
 
Determination of forbidden addition drugs of Diazepam,Clonazepam and Estazolam in tranquilizing mind traditional Chinese medicine by UPLC-MS/MS
Abstract:Objective To establish a specific method for determination of forbidden addition drugs of Diazepam,Clonazepan and Estazolam in tranquilizing mind Traditional Chinese Medicine. Methods Diazepam, Clonazepam and Estazolam were determined and analyzed by UPLC-MS/MS. ACQUITY BEH C18 analysis column(2.1 mm×50 mm,1.7 μm) was used with the mobile phase of 10 mmol/L ammonium acetate and acetonitrile(90:10) with gradient elution. The flow rate was 0.4 ml/min,and the detection wavelength was 254 nm.EIS ion source was used with positive ion monitoring. Results The standard curves of Diazepam,Clonazepam and Estazolam showed good linearity over the concentration rang of 109.8~878.4, 102.1~816.8,106.9~855.2 ng/ml,The detection limits were 0.06,2.5×10-3,2.8×10-3 ng,the quantitation limits were 0.19,8.2×10-3,9.2×10-3 ng,the average recoveries of three chemicals was 95.7%~103.7%. Conclution The method was specific,sensitive,easily and quickly,which could be used to detect Diazepam,Clonazepan and Estazolam in tranquilizing mind traditional Chinese medicine.
keywords:UPLC-MS/MS  traditional Chinese medicine  tranquilizing mind  addition drugs
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