UFLC-MS/MS法同时测定黄芪中黄芪甲苷和毛蕊异黄酮葡萄糖苷的含量  

Simultaneous Determination of Astragaloside IV and Calycosin-7-O-β-D-Glucopyranoside in Astragali Radix by UFLC-MS/MS

作　　者：崔悦 高兴 韩丽琴 范琢玉 汤鑫淼 冯波 关皎 朱鹤云 CUI Yue;GAO Xing;HAN Liqin;FAN Zhuoyu;TANG Xinmiao;FENG Bo;GUAN Jiao;ZHU Heyun(Schoolof Pharmacy,Jilin Medical University,Jilin 132013 Jilin,China)

机构地区：[1]吉林医药学院药学院,吉林吉林132013

出　　处：《中药新药与临床药理》2021年第12期1855-1858,共4页Traditional Chinese Drug Research and Clinical Pharmacology

基　　金：国家自然科学基金项目(81703683);吉林省科技厅项目(YDZJ202101ZYTS074);吉林省教育厅课题(JJKH20210492KJ;JJKH20191071KJ);吉林省中医药管理局项目(2021168;2021169);吉林省卫生健康科技创新项目(20192c006);吉林省大学生创新创业训练计划项目(202013706016)。

摘　　要：目的建立超快速液相色谱-串联质谱(UFLC-MS/MS)法同时测定黄芪中黄芪甲苷和毛蕊异黄酮葡萄糖苷的含量。方法液相测定采用0.1%甲酸水溶液(A)-乙腈(B)为流动相,梯度洗脱;Shim-Pack XR-ODS柱(75 mm×3.0 mm,2.2μm);流速为0.4 mL·min^(-1)。质谱测定采用三重四极杆串联质谱仪,电喷雾电离源(ESI源),负离子模式检测。结果黄芪甲苷和毛蕊异黄酮葡萄糖苷分别在1~50μg·mL-1(r=0.999 6)、2~100μg·mL^(-1)(r=0.999 8)范围内线性关系良好。黄芪甲苷含量为0.132%~0.140%,毛蕊异黄酮葡萄糖苷含量为0.055 1%~0.064 3%。结论与《中国药典》方法比较,该方法供试品提取简单,分析快速、准确,可用于黄芪的质量控制研究。Objective To develop an ultra-fast liquid chromatography with tandem mass spectrometry(UFLC-MS/MS)method for simultaneous determination of astragaloside IV and calycosin-7-O-β-D-glucopyranoside in Astragali radix.Methods Chromatographic separation was performed on Shim-Pack XR-ODS column(75 mm×3.0 mm,2.2 μm).The mobile phase consisted of 0.1% formic acid in water(A)and acetonitrile(B).The two analytes were determined with gradient elution at a flow rate of 0.4 mL · min-1.Detection was performed on mass spectrometry equipped with electro-spray ionization source under negative ionization mode.Results The linear ranges were 1-50 μg · mL-1(r=0.999 6) for astragaloside IV and 2-100 μg · mL-1(r=0.999 8) for calycosin-7-O-β-Dglucopyranoside.The content ranges of two components in six batches were 0.132%-0.140% for astragaloside IV,0.055 1%-0.064 3% for calycosin-7-O-β-D-glucopyranoside.Conclusion Compared with the content determination methods being included in Pharmacopoeia of the People’s Republic of China,the current method is rapid and accurate,with simple sample preparation,which can be used for the quality control of Astragali radix.

关 键 词：黄芪 黄芪甲苷 毛蕊异黄酮葡萄糖苷 超快速液相色谱-串联质谱法 

分 类 号：R284.1[医药卫生—中药学]