| 引用本文: | 刘静,董宇,姜鑫,王震红.LC-MS测定止咳平喘类中成药中非法添加的8种化学药物[J].中国现代应用药学,2021,38(7):851-855. |
| LIU Jing,DONG Yu,JIANG Xin,WANG Zhenhong.Determination of 8 Chemical Drugs Illegally Added into Cough and Asthma Traditional Chinese Medicine by LC-MS[J].Chin J Mod Appl Pharm(中国现代应用药学),2021,38(7):851-855. |
|
| 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。 |
| 关键词: 液质联用法 止咳平喘 非法添加 中成药 |
| DOI：10.13748/j.cnki.issn1007-7693.2021.07.014 |
| 分类号:R927.11 |
| 基金项目: |
|
| Determination of 8 Chemical Drugs Illegally Added into Cough and Asthma Traditional Chinese Medicine by LC-MS |
|
LIU Jing, DONG Yu, JIANG Xin, WANG Zhenhong
|
|
Liaoning Institute for Drug Control, Shenyang 110036, China
|
| 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. |
| Key words: LC-MS cough and asthma illegal addition traditional Chinese medicine |
