HPLC-MS/MS法同时测定华山参滴丸中阿托品、山莨菪碱和东莨菪碱的含量(英文)  

Rapid Simultaneous Determination of Atropine,Anisodamine and Scopolamine in Huashanshen Dripping Pill by Liquid Chromatography-tandem Mass Spectrometry

作　　者：侯媛媛[1] 李若洁[2] 彭佳敏[1] 王利强[1] 

机构地区：[1]南开大学药学院,天津300071 [2]南开大学生命科学学院,天津300071

出　　处：《南开大学学报（自然科学版）》2010年第4期29-35,共7页Acta Scientiarum Naturalium Universitatis Nankaiensis

基　　金：Supported by the Fundamental Research Funds for the Central Universities(65011111)

摘　　要：华山参滴丸是含有托烷类生物碱的中药制剂,主要用于治疗哮喘,具有很好的临床疗效,但缺乏较有效的定量方法控制其质量.建立了一种快速、简单、准确的HPLC-MS/MS法同时测定华山参滴丸中阿托品、山莨菪碱和东莨菪碱的含量.首先采用超声的方法对滴丸进行提取来制备样品溶液,然后采用C18色谱柱对样品进行分离.流动相为20 mmol/L醋酸铵水溶液:甲醇(70:30);流速为0.3 mL/min.质谱检测器采用电喷雾正离子模式的多重反应监测方式进行测定,整个分析时间仅耗时1.5 min.阿托品和山莨菪碱在250～4000 ng/mL范围内、东莨菪碱在62.5～1 000 ng/mL范围内均呈良好的线性关系(r^2>0.999).三种成分的日内和日间精密度均小于3.0;平均回收率均大于98%.此方法快速、可靠、重现性好,适用于华山参滴丸的日常质量控制.Huashanshen dripping pill, traditional Chinese medicine （TCM） preparation containing tropane alkaloids, is used for the anti-asthmatic treatment and has good clinical efficacy. But there is not an effective quantification method to assess the quality of Huashanshen dripping pill. In this study, a rapid, simple and ac- curate HPLC-MS/MS method was developed for simultaneous determination of atropine, anisodarnine and scopolamine in Huashanshen dripping pill. After a simple extraction with sonication used for sample preparation, chromatographic separation was performed on a short C18 column with mobile phase of a mixture of 20 mmol/L ammonium acetate in water and methanol （70 ： 30） at a flow rate of 0. 3 mL/min. The mass spectrometer equipped with an electrospray ionization source （ESI） was operated in the positive ion mode using multiple reaction monitoring （MRM）. The whole analytical run time was only 1.5 min and the calibration graphs exhib- ited a linear concentration range of 250-4 000 ng/mL for atropine and anisodamine and 62.5-1 000 ng/mL for scopolamine with correlation coefficients of more than 0. 999 for all the ingredients studied. The intra- and interday precisions were less than 3. 0% and the mean recoveries were more than 98. 0% for all analytes. This method is rapid, reliable, reproducible and suitable for the routine use to control the quality of Huashanshen dripping pill.

关 键 词：托烷类生物碱 HPLC-MS/MS 华山参 定量测定 

分 类 号：R927.2[医药卫生—药学]