液相色谱-质谱联用同时测定芪参益气滴丸中黄芪甲苷、丹参素、原儿茶醛、人参皂苷Rg_1和Rb_1含量

Simultaneous Determination of the Contents of Astragaloside Ⅳ,Danshensu,Protocatechualdehyde,Ginsenosides Rg_1 and Rb_1 in Qishenyiqi Dropping Pills by LC-MS

目的建立同时测定芪参益气滴丸中黄芪甲苷、丹参素、原儿茶醛、人参皂苷Rg1和Rb1含量的液相色谱-质谱联用方法。方法采用Wonda Sil C18色谱柱(4.6 mm×150 mm,5μm),流动相A为10 mmol.L-1甲酸铵,0.2%甲酸水溶液,B为0.2%甲酸乙腈溶液,采用线性梯度洗脱;流速为1 mL.min-1,柱温30℃。质谱条件采用电喷雾离子化(ESI)方式,负离子模式,以选择性离子监测(SIM)模式对黄芪甲苷、丹参素、原儿茶醛、人参皂苷Rg1和Rb1进行含量测定。结果黄芪甲苷、丹参素、原儿茶醛、人参皂苷Rg1和Rb1分别在10.72～536.0,89.10～4 455,13.37～668.7,22.60～1 130,23.55～1 177 ng.mL-1内与峰面积呈良好线性关系。芪参益气滴丸中黄芪甲苷、丹参素、原儿茶醛、人参皂苷Rg1和Rb1的平均加样回收率均介于98%～102%之间。结论本法简单、快速、灵敏、准确,可用于芪参益气滴丸中黄芪甲苷、丹参素、原儿茶醛、人参皂苷Rg1和Rb1含量测定,为该药的质量控制提供依据。

OBJECTIVE To establish a LC-MS method for simultaneous determination of 5 compounds （ astragaloside IV, danshensu, protocatechualdehyde, ginsenosides Rg1 and Rb1 ） in Qishenyiqi Dropping Pills. METHODS The chromatographic separation was carried out at 30℃ on a Wonda Sil C18 column （4. 6 mm × 150 mm, 5 μm） eluted in a gradient program. The mobile phase consisted of water containing 10 mmol·L^-1 ammonium formate and 0. 2% formic acid-acrtonitrile containing 0. 2% formic acid. The mass spectra were obtained by Agilent 6410 triple quad mass spectrometer with electrospray ionization source in negative ion mode. RESULTS The linear ranges for astragaloside IV, danshensu, protocatechualdehyde, ginsenosides Rg1 and Rb1 were 10. 72 - 536.0, 89. 10 - 4 455, 1. 337 -66. 87, 22. 60 - 1 130 and 23.55 - 1 177 ng·mL^-1, respectively. The average recoveries ranged between 98% - 102%. CON- CLUSION The established method is convenient, sensitive and accurate. It can be used for the determination of the contents of astragaloside Ⅳ, danshensu, protocatechualdehyde, ginsenosides Rgl and Rb1 in Qishenyiqi Dropping Pills for quality control.