UFLC-MS/MS法同时测定黄芩汤中8个活性成分的含量  

Simultaneous Determination of Eight Active Components in Huangqin Decoction by UFLC-MS/MS

作　　者：崔悦 钟思雨 汤鑫淼 苗青 郎鹏超 关皎 朱鹤云 冯波 CUI Yue;ZHONG Siyu;TANG Xinmiao;MIAO Qing;LANG Pengchao;GUAN Jiao;ZHU Heyun;FENG Bo(School of 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》2022年第8期1108-1112,共5页Traditional Chinese Drug Research and Clinical Pharmacology

基　　金：吉林省大学生创新创业训练计划项目(S202113706052)。

摘　　要：目的建立超快速液相色谱-串联质谱法(UFLC-MS/MS)同时测定黄芩汤中黄芩苷、汉黄芩苷、黄芩素、汉黄芩素、芍药苷、芍药内酯苷、甘草苷和甘草酸8个活性成分的含量。方法采用Shim-Pack XRODS色谱柱(75 mm×3.0 mm,2.2μm),流动相为0.1%甲酸水溶液(A)-乙腈(B),梯度洗脱(0~15 min,10%→70%B);流速:0.4 mL·min^(-1);柱温:35℃;进样量:5μL;电喷雾电离源(ESI源)负离子检测,多反应检测(MRM)。结果黄芩汤中8个成分质量浓度分别在浓度范围内与峰面积线性关系良好,平均回收率为98.5%~100.3%。黄芩汤中黄芩苷、汉黄芩苷、黄芩素、汉黄芩素、芍药苷、芍药内酯苷、甘草苷和甘草酸的含量范围分别为0.124~0.135、0.057~0.067、0.259~0.282、0.145~0.158、0.077~0.085、0.0061~0.0064、0.030~0.035、0.0157~0.189 mg·mL^(-1)。结论本方法分析时间短、灵敏度高、稳定性好,可用于黄芩汤的质量控制。Objective To develop an ultra-fast liquid chromatography-tandem mass spectrometry for the determination of eight active components,including baicalin,wogonoside,baicalein,wogonin,paeoniflorin,paeoniflorin,liquirtin and glycyrrhizic acid in Huangqin Decoction.Methods Shim-Pack XR-ODS column(75 mm×3.0 mm,2.2μm)was used for separation.The mobile phase consisted of 0.1%formic acid aqueous solution(A)and acetonitrile(B).The gradient elution(0-15 min,10%-70%B)was carried out at the flow rate of 0.4 mL·min^(-1) with the column temperature of 35℃.The injection volume was 5μL.Electrospray ionization source and multiple reaction detection(MRM)were used for detection.Results Within the concentration ranges of baicalin,wogonoside,baicalein,wogonin,paeoniflorin,albiflorin,liquiritin and glycyrrhizic acid,the contents and peak areas showed good linearities.The average recoveries(n=9)were 99.2%-100.3%.The content ranges of the eight components were 0.124-0.135,0.057-0.067,0.259-0.282,0.145-0.158,0.077-0.085,0.0061-0.0064,0.030-0.035,0.0157-0.189 mg·mL^(-1),respectively.Conclusion The method is sensitive,accurate and stable,and can be used for the quality control of Huangqin Decoction.

关 键 词：黄芩汤 黄芩苷 黄芩素 芍药苷 超快速液相色谱-串联质谱法 含量测定 质量控制 

分 类 号：R284.1[医药卫生—中药学]