UPLC-MS/MS法测定龙胆泻肝丸(水丸)中5种成分的含量

Content Determination of 5 Components in Longdan Xiegan Pills(Water Pills Pills)by UPLC-MS/MS

目的研究可测定龙胆泻肝丸(水丸)中龙胆苦苷、栀子苷、黄芩苷、甘草苷和23-乙酰泽泻醇B含量的超高效液相色谱串联质谱(UPLC-MS/MS)法。方法采用C_(18)色谱柱,以乙腈(A)-0.1%甲酸溶液(B)为流动相,流速为0.2 mL/min,柱温为30℃;质谱采用多反应监测模式(MRM)进行数据采集。结果龙胆苦苷、栀子苷、黄芩苷、甘草苷和23-乙酰泽泻醇B分别在0.6660~13.3200μg/mL、1.0360~10.3600μg/mL、0.4729~4.7290μg/mL、0.1002~2.0030μg/mL和0.0301~0.3011μg/mL浓度范围内,呈良好的线性关系[相关系数(R2)均大于0.9994]。28批样品各成分含量具有一定差异性。结论所建方法简便、高效,能测定龙胆泻肝丸中5种成分的含量,有助于控制该制剂的整体质量。

Objective To study the simultaneous determination of gentiopicroside,gardenoside,baicalin,liquiritin and 23-acetyl alis⁃matol B in Longdan Xiegan pills(Water pills)by UPLC-MS/MS method.Methods The determination was performed on a C_(18)column with acetonitrile-0.1%formic acid solution as the mobile phase at the flow rate of 0.2 mL/min.The column temperature was 30℃.Mul⁃tiple response monitoring mode(MRM)was used for mass spectrometry data acquisition.Results Good linear relationships of gentiopi⁃croside,gardenoside,baicalin,liquiritin and 23-acetyl alismatol B were found in the concentration range of 0.6660~13.32μg·mL,1.036~10.36μg/mL,0.4729~4.729μg/mL,0.1002~2.003μg/mL and 0.03011~0.3011μg/mL(R2>0.9994).The content of each com⁃ponent in 28 batches of samples had certain differences.Conclusion The established method is simple and efficient,and can simulta⁃neously determine the contents of 5 components in Longdan Xiegan pills,which is helpful to control the overall quality of longdan Xie⁃gan pills.