液相色谱-质谱联用同时测定芪胶升白胶囊中黄芪甲苷、淫羊藿苷、阿魏酸的含量

Simultaneous determination of the contents of astragaloside Ⅳ,icariin and ferulic acid in Qijiao Shenbai capsules by LC-MS

目的:建立中成药芪胶升白胶囊中黄芪甲苷、淫羊藿苷、阿魏酸的含量测定方法。方法:采用Eclipse XDB-C18色谱柱(150 mm×2.1 mm,5.0μm),流动相A为5 mmol·L^(-1)甲酸铵-0.1%甲酸水溶液,B为乙腈,梯度洗脱,流速0.5 m L·min^(-1);采用电喷雾离子源进行负模式监测,选择离子监测模式用于定量分析,喷雾电压-4 k V,干燥气温度为350℃,干燥气流量为12 L·min^(-1),雾化器压力为310 k Pa,用于定量分析的离子分别是m/z 829.0(黄芪甲苷)、721.3(淫羊藿苷)、193.2(阿魏酸)。结果:黄芪甲苷、淫羊藿苷、阿魏酸质量浓度分别在20.50~1 025、10.38~519.0、10.02~501.0 ng·m L^(-1)范围内与峰面积呈良好线性关系,平均加样回收率在97%~101%之间。3批样品中黄芪甲苷、淫羊藿苷、阿魏酸含量分别在0.499~0.509、0.402~0.405和0.100~0.108 mg·g^(-1)。结论:经方法学验证,本方法可以用于芪胶升白胶囊的含量测定。通过对3个批次的芪胶升白胶囊进行分析测定,各个批次含量无明显差异,可为芪胶升白胶囊的全面质量控制提供依据。

Objective： To develop a method for determination of astragalosideⅣ, icariinand ferulicacid in Chinese patent medicine Qijiao Shenbai capsules.Methods： Separation was carried out at 25℃ on an Eclipse XDB-C18 （150 mm×2.1 mm, 5.0μm） eluted in a gradient program at aflow rate of 0.5 mL·min-1.The mobile phase consisted of water containing 5 mmol·L-1 ammonium formate and 0.1%formic acid （A）-acetonitrile （B）.The mass spectra were obtained by Agilent 6460 triple quad mass spectrometer with electrospray ionization source in negative ion mode by selected ion monitoring （SIM）.The capillary voltage was -4 kV, gas temperature was 350℃, gas flow was 12 L·min-1and nebulizer pressure was set at 310 kPa.The quantitative ions were m/z 829.0 for astragaloside Ⅳ, m/z 721.3 for icariin and m/z193.2 for ferulic acid.Results： The linear ranges for astragalosideIV, icariin and ferulic acid were 10.38-519.0, 20.50-1 025 and 10.02-501.0 ng·mL-1, respectively.The recoveries were between 97%-101%.The content ranges in three batches of Qijiaoshenbai capsules were 0.499-0.509 mg·g-1, 0.402-0.405 mg·g-1 and 0.100-0.108 mg·g-1, respectively.Conclusion： Method validation proves that this method can be used for content determination of Qijiao Shenbai capsules.The determination results of 3 batches of Qijiao Shenbai capsules show the content of each batch has no significant difference.The results may provide a basis for the quality control of Qijiao Shenbai capsules.