UPLC-MS/MS法同时测定黄芪水提液中3种成分的含量  

Simultaneous Determination of Three Components in Astragalus membranaceus Aqueous Extact Solution by UPLC-MS/MS Method

作　　者：胡燕梨[1] 谭丽盈[1] 胡国辉[1] HU Yan-li;TAN Li-ying;HU Guo-hui(NO.1 Affiliated Hospital of Guangzhou University of Traditional Chinese Medicine,Guangzhou 510400,China)

机构地区：[1]广州中医药大学第一附属医院,广东广州510400

出　　处：《海峡药学》2022年第2期66-69,共4页Strait Pharmaceutical Journal

摘　　要：目的建立UPLC-MS/MS法同时测定黄芪水提液中毛蕊异黄酮葡萄糖苷、毛蕊异黄酮和黄芪甲苷含量的方法。方法黄芪药材经水进行提取后采用UPLC-MS/MS法进行测定,色谱条件:安捷伦SB-C_(18)色谱柱(2.1 mm×100 mm,1.8μm)用于进行分离,采用梯度洗脱方式进行分离,乙腈和0.1%甲酸水溶液作为流动相,流速为0.3 mL·min^(-1);柱温设为40℃,进样体积:1μL,质谱测定条件:检测器为电喷雾离子源,正离子模式采集,多反应监测(MRM)方式定量。结果毛蕊异黄酮葡萄糖苷、毛蕊异黄酮和黄芪甲苷的浓度分别在1.012~50.6 ng(r=0.9989)、1.656~82.8 ng(r=0.9996)和2.404~120.2 ng(r=0.9998)范围内线性关系良好;平均回收率分别为96.78%、96.95%和101.86%,相对标准偏差分别为4.28%、2.39%和1.56%。结论该方法操作简单、分析速度速、灵敏度高,可以用于黄芪水提液中三种成分的质量控制。OBJECTIVE To propose an UPLC-MS/MS method for the simultaneous determination of calycosin-7-O-β-D-glucoside,calycosin and astragaloside IV in aqueous extracts of Astragalus membranaceus.METHODS The samples were extracted by water and Agilent SB-C_(18) column(2.1 mm×100 mm,1.8μm)was used to perform separation with acetonitrile-0.1%formic acid as mobile phase by gradient elution.The condition of flow rate at 0.3 mL·min^(-1),column temperature of 40℃and 1μL was the injection volume.The detected sample with ion source was adopted with ESI positive ion mode acquisition and MRM scanning was used for quantification.RESULTS The linear range of calycosin-7-O-β-D-glucoside,calycosin and astragaloside IV were 1.012-50.6 ng(r=0.9989),1.656-82.8 ng(r=0.9996)and 2.404-120.2 ng(r=0.9998),respectively.The average recoveries of this three compounds were 96.78%,96.95%and 101.86%,with RSD of 4.28%,2.39%and 1.56%,respectively.CONCLUSION The method is simple,fast and sensitive,and can be used for the quality control of the three components in the aqueous extract of Astragalus membranaceus.

关 键 词：黄芪 水提液 毛蕊异黄酮葡萄糖苷 毛蕊异黄酮 黄芪甲苷 含量测定 液质联用 

分 类 号：R284.1[医药卫生—中药学]