UPLC-MS/MS测定大黄蛰虫丸中的9种成分

Simultaneous Determination of 9 Components in Dahuang Zhechong Pills by Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry

目的建立超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定大黄蛰虫丸中黄芩素、黄芩苷、苦杏仁苷、大黄酚、大黄素甲醚、甘草苷、芍药苷、毛蕊花糖苷、甘草酸铵含量的分析方法。方法采用Agilent Technologies Infinity Lab Poroshell 120 EC-C18(4.6 mm×100 mm,2.7μm)色谱柱,以乙腈-0.1%甲酸水溶液为流动相,梯度洗脱,流速0.3 ml/min;电喷雾离子源正负同时检测,多反应监测(MRM)扫描模式,通过比较供试品与对照品的色谱保留时间、色谱峰面积,同时进行黄芩素、黄芩苷、苦杏仁苷、大黄酚、大黄素甲醚、甘草苷、芍药苷、毛蕊花糖苷、甘草酸铵的定量测定。结果9种成分线性范围的相关系数(r)均不低于0.998,回收率为93.77%~101.27%,RSD为0.57%~1.79%。结论该法快速简便、高通量、选择性好、灵敏度高,能为大黄蛰虫丸的质量控制提供依据。

Objective To establish an ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method for the simultaneous determination of baicalein,baicalin,amygdalin,chrysophanol,physcion,liquiritin,paeoniflorin,verbascoside and monoammonium glycyrrhizinate in Dahuang Zhechong Pills.Methods An Agilent Technologies Infinity Lab Poroshell 120 EC-C18 column(4.6 mm×100 mm,2.7μm)was used with acetonitrile-0.1%formic acid aqueous solution as mobile phase for gradient elution.The flow rate was 300 ml/min.The electrospray ion source detection was performed at the same time under multiple reaction monitoring(MRM)scanning mode.The chromatographic retention time and chromatographic peak area of the samples and the reference were compared,and the contents of baicalein,baicalin,amygdalin,chrysophanol,physcion,liquiritin,paeoniflorin,verbascoside and monoammonium glycyrrhizinate were determined.Results The correlation coefficients(r)were not less than 0.998,the recoveries were 93.77%-101.27%,and the RSDs were 0.57%-1.79%for the nine compositions.Conclusion The method is quick and simple,and has high flux,good selectivity and high sensitivity.It can provide evidence for quality control of Dahuang Zhechong Pills.