LC-MS测定止咳平喘类中成药中非法添加的8种化学药物

Determination of 8 Chemical Drugs Illegally Added into Cough and Asthma Traditional Chinese Medicine by LC-MS

关键词:  液质联用法  止咳平喘  非法添加  中成药

Key words:  LC-MS  cough and asthma  illegal addition  traditional Chinese medicine

摘要:

目的 建立LC-MS检测止咳平喘类中成药中的8种非法添加化学药物（茶碱、磺胺甲噁唑、醋酸泼尼松、地西泮、氯苯那敏、苯海拉明、喷托维林、苯丙哌林）。方法 采用高效液相色谱-离子阱质谱，ESI离子源，在正负离子扫描方式下，以一级全扫描模式和二级全扫描模式进行检测。采用资生堂CAPCELL-PAK C₁₈色谱柱（4.6 mm×150 mm，5 μm），乙腈-0.02 mol·L^-1乙酸铵溶液为流动相进行梯度洗脱，流速0.5 mL·min^-1。通过比较对照品和样品的色谱图和质谱图，对样品中非法添加的化学成分进行定性鉴别。结果 8种化合物色谱峰分离良好，检出限为0.1~0.4 μg·mL^-1。21批样品中，3批检出茶碱。结论 该方法操作简单，专属性强，灵敏度高，适用于止咳平喘类中成药中非法添加的8种化学类物质的快速分析检测。

Abstract:

OBJECTIVE To establish a LC-MS method for the determination of 8 chemicals(including theophylline, sulfamethoxazole, prednisone acetate, diazepam, chlorpheniramine, diphenhydramine, pentoxyverine, benproperine) illegally added into cough and asthma traditional Chinese medicine. METHODS A high performance liquid chromatography-ion trap mass spectrometry and electrospray ionization source were adopted to perform the analysis operated in positive and negative ion modes with full scan MS and full scan MS² modes. Chromatographic separation was performed on a SHISEIDO CAPCELL-PAK C₁₈ column(4.6 mm×150 mm, 5 μm) with the mobile phase consisted of acetonitrile-0.02 mol·L⁻¹ ammonium acetate solution by gradient elution at a flow rate of 0.5 mL·min⁻¹. The qualitative identification of chemical components illegally added in samples was performed by comparing the chromatograms and mass spectrograms of the reference substances and samples. RESULTS A good chromatographic resolution of 8 compounds was obtained under the LC-MS condition. Out of 21 batches of samples, 3 samples contained theophylline with the detection limit of the method of 0.1-0.4 μg·mL⁻¹. CONCLUSION The method is simple, selective and rapid. It is suitable for the rapid analysis and detection of 8 chemical substances illegally added in Chinese patent medicines for relieving cough and asthma.