止咳平喘类中成药中9种非法添加化学成分的定性定量检验方法研究

【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。

Qualitative and Quantitative Method for Detection of 9 Chemicals Illegally Added into Cough-checking and Asthma-relieving Chinese Patent Medicines

Objective To establish a qualitative and quantitative method for the detection of 9 chemicals illegally added into cough-checking and asthma-relieving Chinese patent medicines.Methods Qualitative screening of 9 chemicals illegally added into cough-checking and asthma-relieving Chinese patent medicines was performed by ultra-performance liquid chromatography quadrupole time-of-flight mass spectrometry(UPLC-Q-TOF).And then the quantitative detection of the positive samples showed by UPLC-Q-TOF was carried out with high performance liquid chromatography(HPLC).Chromatographic separation was achieved on a Kromasil C18 column(250 mm × 4.6 mm,5 μm) with the mobile phase of acetonitrile and ammonium formate buffer (pH 3.65) by gradient elution.The flow rate was 1.0 mL/min,and the detection wavelength was 225 nm and 360 nm respectively.Results Five batches of samples had been tested,and codeine phosphate was detectable in one batch of the samples,the content being 0.84 mg/mL.Conclusion The established method is simple,accurate and highly-sensitive for the determination of 9 chemicals illegally added into cough-checking and asthma-relieving Chinese patent medicines.