UFLC-MS/MS法同时测定黄芪建中汤中6个活性成分的含量  

Simultaneous determination of six active components in Huangqi Jianzhong decoction by UFLC-MS/MS

作　　者：关皎 王悦 廖宇 高兴 周新新 冯波 崔悦 朱鹤云 GUAN Jiao;WANG Yue;LIAO Yu;GAO Xing;ZHOU Xin-xin;FENG Bo;CUI Yue;ZHU He-yun(School of Pharmacy,Jilin Medical University,Jilin 132013,China)

机构地区：[1]吉林医药学院药学院,吉林132013

出　　处：《药物分析杂志》2022年第1期133-139,共7页Chinese Journal of Pharmaceutical Analysis

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);吉林省大学生创新创业训练计划项目(S202113706075;202013706016)。

摘　　要：目的:建立一种同时测定黄芪建中汤中6个活性成分(毛蕊异黄酮-7-O-β-D-吡喃葡萄糖苷、桂皮酸、芍药苷、芍药内酯苷、甘草苷和甘草酸)含量的超快速液相色谱-串联质谱法。方法:采用Shim-Pack XR-ODS色谱柱(75 mm×3.0 mm,2.2μm),以0.1%甲酸水溶液(A)-乙腈(B)为流动相,梯度洗脱(0~6.0 min,12%B→25%B;6.0~7.0 min,25%B→45%B;7.0~11.0 min,45%B→60%B;11.0~13.0 min,60%B→70%B),平衡时间5 min,流速0.4 mL·min^(-1),柱温30℃,进样量5μL;采用电喷雾电离源(ESI源),负离子模式检测,多反应监测(MRM)。结果:毛蕊异黄酮-7-O-β-D-吡喃葡萄糖苷、桂皮酸、芍药苷、芍药内酯苷、甘草苷和甘草酸质量浓度分别在0.2~10μg·mL^(-1)(r=0.9996)、0.5~25μg·mL^(-1)(r=0.9995)、2~100μg·mL^(-1)(r=0.9996)、0.5~25μg·mL^(-1)(r=0.9998)、0.5~25μg·mL^(-1)(r=0.9997)和0.5~25μg·mL^(-1)(r=0.9996)范围内与峰面积呈良好线性关系;平均回收率(n=9)分别为98.3%、98.4%、98.9%、98.0%、98.8%和99.2%。6批样品中上述6个成分的含量分别为0.114~0.128、0.118~0.144、4.19~4.52、1.03~1.12、0.277~0.345、0.679~0.798 mg·mL^(-1)。结论:本方法灵敏度高,稳定性好,可用于黄芪建中汤的质量控制。Objective:To establish an ultra-fast liquid chromatography with tandem mass spectrometry(UFLC-MS/MS)method for simultaneous determination of six active components(calycosin-7-O-β-D-glucopyranoside,cinnamic acid,paeoniflorin,albiflorin,liquiritin and glycyrrhizic acid)in Huangqi Jianzhong decoction.Methods:Chromatographic separation was performed on a Shim-Pack XR-ODS column(75 mm×3.0 mm,2.2μm).The mobile phase consisted of 0.1%formic acid in water(A)and acetonitrile(B)at a flow rate of 0.4 mL·mL^(-1).The six analytes were determined with gradient elution(0-6 min,12%B→25%B;6-7 min,25%B→45%B;7-11 min,45%B→60%B;11-13 min,60%B→70%B),and the equilibration time was 5 min.The column temperature was maintained at 30℃,and the injection volume was 5μL.Detection was performed with electrospray ionization source in negative ionization mode.Quantification was performed using multiple reactions monitoring(MRM)mode.Results:The linear ranges of calycosin-7-O-β-D-glucopyranoside,cinnamic acid,paeoniflorin,albiflorin,liquiritin and glycyrrhizic acid were 0.2-10μg·mL^(-1)(r=0.9996),0.5-25μg·mL^(-1)(r=0.9995),2-100μg·mL^(-1)(r=0.9996),0.5-25μg·mL^(-1)(r=0.9998),0.5-25μg·mL^(-1)(r=0.9997)and 0.5-25μg·mL^(-1)(r=0.9996),respectively.The average recoveries(n=9)of the above-mentioned six components were 98.3%,98.4%,98.9%,98.0%,98.8%and 99.2%,respectively.The content ranges of six components in six batches were 0.114-0.128 mg·mL^(-1)for calycosin-7-O-β-D-glucopyranoside,0.118-0.144 mg·mL^(-1)for cinnamic acid,4.19-4.52 mg·mL^(-1)for paeoniflorin,1.03-1.12 mg·mL^(-1)for albiflorin,0.277-0.345 mg·mL^(-1)for liquiritin and 0.679-0.798 mg·mL^(-1)for glycyrrhizic acid.Conclusion:The established method is accurate,stable and reproducible,and can provide a research method for the quality control of Huangqi Jianzhong decoction.

关 键 词：黄芪建中汤 毛蕊异黄酮-7-O-β-D-吡喃葡萄糖苷 桂皮酸 芍药苷 芍药内酯苷 甘草苷 甘草酸 超快速液相色谱-串联质谱法 

分 类 号：R917[医药卫生—药物分析学]