超高效液相串联质谱法同时测定二陈汤中4种成分含量

Simultaneous determination of four kinds of components in Erchen Decoction by UPLC-MS/MS

目的建立同时测定二陈汤中橙皮苷、齐墩果酸、麻黄碱、甘草酸含量的超高效液相色谱-串联质谱(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)方法。方法采用Phenomenex Gemini C18色谱柱,流动相为乙腈-2 mmol/L甲酸铵水溶液,等度洗脱。采用电喷雾电离源,多反应离子监测(MRM)。采用外标法定量分析,用于定量分析的橙皮苷、齐墩果酸、麻黄碱及甘草酸检测离子对m/z分别为611.2→303.1、455.2→407.2、166.2→148.2、821.4→350.9。结果橙皮苷、齐墩果酸、麻黄碱及甘草酸分别在0.0100~0.4000、0.0063~0.2500、0.0125~0.5000、0.0025~0.1000 ng范围内与峰面积线性关系良好(r值分别为0.9982、0.9988、0.9994、0.9991)。加样回收率在98.45%~102.60%范围内,RSD均低于1.67%。结论该法专属性强、快速灵敏,可用于二陈汤中橙皮苷、齐墩果酸、麻黄碱及甘草酸的含量测定。

Objective To develop the UPLC-MS/MS method for the determination of hesperidin,oleanolic acid,ephedrine and glycyrrhizic acid in Erchen Decoction.Methods The separation was performed on Phenomenex Gemini C18,isocratic elution was carried out with mobile phase consisting of acetonitrile-2 mmol/L ammonium formate.The mass spectrometer was operated in the positive and negative ionization electrospray(ESI)mode using multiple monitoring(MRM)for analysis of four components.External standard methods fix quantity.The precursor to product ion transitions monitored for hesperidin,oleanolic acid,ephedrine and glycyrrhizic acid were m/z 611.2→303.1,455.2→407.2,166.2→148.2 and 821.4→350.9,respectively.Results Hesperidin,oleanolic acid,ephedrine and glycyrrhizic acid were all analyzed exactly,the linear ranges were 0.0100-0.4000,0.0063-0.2500,0.0125-0.5000,0.0025-0.1000 ng,respectively.The r were 0.9982,0.9988,0.9994 and 0.9991,respectively.The recovery rateof the four analytes ranged from 98.45%to 102.60%and the RSD were all below 1.67%.Conclusion This UPLC-MS/MS method is sensitive,accurate and suitable hwhich could be applied for the determination of hesperidin,oleanolic acid,ephedrine and glycyrrhizic acid in Erchen Decoction.