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【目的】建立检测止咳平喘中成药中9种非法添加化学成分的定性定量检验方法。【方法】采用超高效液相色谱—四级杆—飞行时间串联质谱(UPLC-Q-TOF)联用技术对止咳平喘类中成药中非法添加的9种化学成分进行定性筛查,经筛查为阳性的样品用高效液相色谱法(HPLC)对止咳平喘中成药中非法添加的9种化学成分进行含量检测。色谱柱采用Kromasil C18(250 mm×4.6 mm,5μm),流动相为乙腈及甲酸铵缓冲液(p H 3.65),梯度洗脱,流速为1.0 m L/min,检测波长为225 nm和280 nm。【结果】通过对5批止咳平喘类中成药进行检测,检出1批样品含有磷酸可待因,含量为0.84 mg/m L。【结论】本法简便准确,灵敏度高,适用于止咳平喘类中成药中9种非法添加化学成分的检测。
【Objective】 To establish a qualitative and quantitative test method to detect nine kinds of illicitly added chemical constituents in proprietary Chinese medicines for relieving cough and asthma. 【Method】 Nineteen chemical constituents illegally added to proprietary Chinese medicines for relieving cough and asthma were qualitatively screened by UPLC-Q-TOF combined with ultra-performance liquid chromatography-quadrupole-time-of-flight mass spectrometry Positive samples were detected by high performance liquid chromatography (HPLC) on cough and asthma patent medicines illegally added to the content of nine chemical constituents. The column was eluted with a gradient of Kromasil C18 (250 mm × 4.6 mm, 5 μm) with acetonitrile and ammonium formate buffer (p H 3.65) at a flow rate of 1.0 mL / min at 225 nm and 280 nm . 【Result】 Five batches of cough and asthma-type Chinese patent medicines were tested. One batch of samples containing codeine phosphate was detected, with a content of 0.84 mg / m L. 【Conclusion】 This method is simple, accurate and sensitive. It is suitable for the detection of 9 kinds of illicitly added chemical constituents in proprietary Chinese medicines for relieving cough and asthma.