UPLC-MS/MS法测定右归丸中毛蕊花糖苷的含量

The Content Determination of Verbascoside in Yougui Pills by UPLC-MS/MS

目的:建立右归丸中毛蕊花糖苷的含量测定方法。方法:采用Waters ACQUITY UPLC BEH C_(18)色谱柱(2.1 mm×100 mm,1.7μm),以乙腈-0.1%甲酸溶液为流动相,梯度洗脱,流速0.3 mL/min,柱温30℃;质谱条件以623→161和623→133为特征离子对,采用电喷雾离子源(ESI)和负离子扫描方式,进行多反应离子监测(MRM)定量分析。结果:毛蕊花糖苷在质量浓度175.739 2~1 757.392 0 ng/mL范围内呈良好线性关系,方法学考察良好。9批样品中毛蕊花糖苷的含量范围为33.40~53.20μg/g。结论:所建方法能测定右归丸中熟地黄的主要化学成分的含量,可用于右归丸的质量控制。

Objective:To establish a method for the content determination of verbascoside in Yougui pills.Methods:The liquid chromatography was performed using acetonitrile-0.1%formic acid as mobile phase in gradient elution at a flow rate of 0.3 mL/min and column temperature of 30℃.The mass spectrometry conditions were characterized by ion pairs 623→161 and 623→133,electrospray ion source and positive ion scanning,and multiple reactive ion monitoring(MRM)quantitative analysis.Results:A good linear relationship was found in the mass concentration range of 175.7392-1757.3920 ng/mL.The content of verbascoside in 9 batches of samples ranged from 33.40μg/g to 53.20μg/g.Conclusion:The method can be used to determine the content of main chemical components of Radix rehmanniae praeparata in Yougui pills and to control the quality of Yougui pills.