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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-飞行时间质谱(UPLC-Q-TOF),MS模式进行检测。采用Waters Acquity BEH C18色谱柱(2.1 mm×100 mm,1.7μm),流动相甲醇-0.1%甲酸的10 mmol·L-1甲酸铵溶液梯度洗脱,流速0.4 m L·min-1;离子源ESI源,正离子检测,扫描范围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、地西泮进行定量检测。结果:8种化学药品的线性范围分别为1.251~62.55,1.043~52.15,1.057~52.85,1.002~50.10,1.147~57.35,1.069~53.45,0.991~49.55,1.111~55.55 mg·L-1,8种化学药品平均回收率在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 a method for the determination of eight chemicals illegally added in proprietary Chinese medicines for cough and asthma. Methods: Ultra-performance liquid chromatography-quadrupole-time-of-flight mass spectrometry (UPLC-Q-TOF) The mobile phase was eluted with a gradient of methanol-0.1% formic acid in 10 mmol·L-1 ammonium formate with a flow rate of 0.4 mL · min-1 on a Waters Acquity BEH C18 column (2.1 mm × 100 mm, 1.7 μm) ESI source, positive ion detection, scanning range m / z 100 ~ 600. Theophylline, sulfamethoxazole, chlorpheniramine, diphenhydramine, pentovirin, benproperine, prednisone acetate, diazepam for quantitative detection. Results: The linear ranges of the eight chemicals ranged from 1.251 to 62.55, from 1.043 to 52.15, from 1.057 to 52.85, from 1.002 to 50.10, from 1.147 to 57.35, from 1.069 to 53.45, from 0.991 to 49.55 and from 1.115 to 55.55 mg · L -1 The average recovery rate of chemicals ranged from 97.8% to 103.2%. Conclusion: The method is rapid, simple and accurate and can be used for the rapid detection of 8 kinds of illegal drugs added to cough and asthma medicines.