摘要
目的:建立止咳平喘类中成药中非法添加的8种化学药品的检测方法。方法:采用超高效液相色谱-四级杆-琶行时间质谱(UPLC-Q-TOF),MS模式进行检测。采用Waters Acquity BEH C18色谱柱(2.1mm×100mm,1.7μm),流动相甲醇-0.1%甲酸的10mmol·L^-1甲酸铵溶液梯度洗脱,流速0.4mL·min^-1;离子源ESI源,正离子检测,扫描范同m/z 100-600。对茶碱、磺胺甲噁唑、氯苯那敏、苯海拉明、喷托维林、苯丙哌林、醋酸泼尼松、地西泮进行定量俭测。结果:8种化学药品的线性范围分别为1.251-62.55,1.043-52.15,1.057-52.85,1.002-50.10,1.147-57.35,1.069-53.45,0.991-49.55,1.111-55.55mg·L^-1,8种化学药品平均回收率和97.8%-103.2%。结论:该方法快速、简便、准确,可用于止咳平喘类中成药中非法添加8种化学药品的快速检测。
Objective: To establish an UPLC-Q-TOF method for the determination of 8 kinds of chemical medicines illegally added in traditional Chinese medicines for relieving cough and asthma. Method: UPLC-Q-TOF and MS mode was adopted to perform the quantitative determination with the Waters Acquity BEH C18 column (2.1 mm×100mm,1.7μm), methanol -10 mmol·L^-1 ammonium formate (containing 0.1% formie acid) for the gradient elution, and the flow rate was 0.4 mL·min^-1 The ion source was eleetrospray ionization (ESI) with the positive ion detection. The scan range was m/z 100-600. Theophylline, sulfamethoxazole, chlorphenamine, diphenhydramine, pentoxyverine, benproperine, prednisone acetate and diazepam added in the traditional Chinese medicines were quantitatively identified. Result: The linear ranges of 8 kinds of chemical medicines were 1.251-62.55, 1.043-52.15, 1.057-52.85, 1.002-50.10, 1.147-57.35, 1.069-53.45, 0.991-49.55, 1.111-55.55 mg·L^-1 The average recovery rate of 8 kinds of chemical medicines was 97.8%-103.2%. Conclusion : This method is rapid, simple and accurate, and could be used to detect 8 kinds of chemical medicines added in traditional Chinese medicines for relieving cough and asthma.
出处
《中国实验方剂学杂志》
CAS
CSCD
北大核心
2015年第4期64-67,共4页
Chinese Journal of Experimental Traditional Medical Formulae
基金
重庆市科技攻关项目(CSTC2012gg B10001)