离子淌度质谱法同时测定金芪降糖片中8种成分含量

Simultaneous determination of 8 components in Jinqi jiangtang tablets by ion mobility mass spectrometry method

目的建立离子淌度质谱法同时测定金芪降糖片中表小檗碱、小檗碱、黄连碱、巴马汀、毛蕊异黄酮葡萄糖苷、3,5-二-O-咖啡酰奎宁酸、4,5-二-O-咖啡酰奎宁酸、绿原酸的含量。方法采用离子淌度质谱法进行检测。色谱柱为Waters ACQUITY UPLC HSS T3(2.1 mm×50 mm,1.8μm),流动相为0.1%甲酸溶液-乙腈(梯度洗脱),流速为0.3 mL/min,柱温为40℃,进样量为5μL。采用电喷雾离子源,在正、负离子模式下进行扫描检测,并根据各成分峰响应设置离子淌度参数,对金芪降糖片中8种成分进行含量测定。结果8种成分在各自范围内线性关系良好(r≥0.999);精密度、重复性、稳定性(24 h)试验的RSD均未超过4.0%;平均加样回收率为94.6%~101.2%,RSD为2.6%~3.9%(n=9)。3批金芪降糖片中上述8种成分的含量分别为3.060~3.545、24.50~26.74、2.795~4.149、1.437~2.501、0.204~0.242、0.950~1.281、2.272~2.828、7.314~7.960 mg/g。结论所建方法灵敏度高、重复性好,可为该制剂的质量控制提供参考。

OBJECTIVE To establish the ion mobility mass spectrometry method for simultaneous determination of epiberberine,berberine,coptisine,palmatine,calycosin-7-glucoside,3,5-O-dicaffeoylquinic acid,4,5-O-dicaffeoylquinic acid and chlorogenic acid in Jinqi jiangtang tablets.METHODS Ion mobility mass spectrometry method was used.The determination was performed on Waters ACQUITY UPLC HSS T3(2.1 mm×50 mm,1.8μm)with mobile phase consisted of 0.1% formic acid solution-acetonitrile(gradient elution)at the flow rate of 0.3 mL/min.The column temperature was 40℃,and the injection volume was 5μL.The contents of 8 components in Jinqi jiangtang tablets were determined by scanning detection under positive and negative ion modes with an electric spray ion source,and setting ion mobility mass parameters according to the peak response of each component.RESULTS The results showed that the linear relationship of the eight components was good within their respective ranges(r≥0.999);RSDs of precision,repeatability and stability(24 h)tests were not more than 4.0%;average recoveries were 94.6%-101.2%,RSDs were 2.6%-3.9%(n=9).The contents of the above eight components in three batches of Jinqi jiangtang tablets were 3.060-3.545,24.50-26.74,2.795-4.149,1.437-2.501,0.204-0.242,0.950-1.281,2.272-2.828,7.314-7.960 mg/g,respectively.CONCLUSIONS The established method has high sensitivity and good reproducibility,and can provide reference for the quality control of the preparation.