UFLC-MS/MS法同时测定龙胆中7个活性成分的含量  

Simultaneous Determination of Seven Active Components in Gentianae Radix Et Rhizoma by UFLC-MS/MS

作　　者：关皎 舒欣洋 吴燕 张雯钰 娄云 范琢玉 汤鑫淼 朱鹤云 崔悦 冯波 GUAN Jiao;SHU Xin-yang;WU Yan;ZHANG Wen-yu;LOU Yun;FAN Zhuo-yu;TANG Xin-miao;ZHU He-yun;CUI Yue;FENG Bo(School of Pharmacy, Jilin Medical University, Jilin 132013,China;Shenzhen Institute of Technology, Shenzhen 518116,China)

机构地区：[1]吉林医药学院药学院,吉林吉林132013 [2]深圳技师学院,广东深圳518116

出　　处：《中国兽药杂志》2022年第6期31-39,共9页Chinese Journal of Veterinary Drug

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);国家级大学生创新创业训练计划项目(202013706017)。

摘　　要：建立可同时测定龙胆中7个活性成分(马钱苷酸、獐牙菜苦苷、6'-O-β-D-葡萄糖基龙胆苦苷、龙胆苦苷、獐牙菜苷、异荭草苷和异牡荆素)含量的超快速液相色谱-串联质谱方法。流动相采用0.1%甲酸水溶液(A)-乙腈(B),色谱柱Shim-Pack XR-ODS(75 mm×3.0 mm,2.2μm),梯度洗脱;采用三重四极杆串联质谱仪,电喷雾电离源,正离子模式监测。上述7个成分线性浓度范围分别为2.5~100μg·mL^(-1)(r=0.9996)、1~40μg·mL^(-1)(r=0.9995)、1~40μg·mL^(-1)(r=0.9995)、5~200μg·mL^(-1)(r=0.9996)、0.1~4μg·mL^(-1)(r=0.9995)、0.05~2μg·mL^(-1)(r=0.9998)和0.01~0.4μg·mL^(-1)(r=0.9995)。6批龙胆样品中上述7个成分的含量分别为0.894%~1.072%、0.260%~0.285%、0.223%~0.268%、3.88%~4.05%、0.00726%~0.00898%、0.000840%~0.00195%和0.000779%~0.00104%。该方法灵敏、稳定,可用于龙胆药材的质量控制。To establish an ultra-fast liquid chromatography with tandem mass spectrometry(UFLC-MS/MS)method for simultaneous determination of seven active components(loganic acid,swertiamarin,6'-O-β-D-glucosylgentiopicroside,gentiopicroside,swertioside,isoorientin and isovitexin)in Gentianae Radix Et Rhizoma.Chromatographic separation was performed on 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).The seven analytes were determined with gradient elution.Detection was performed on 3200 QTRAP mass spectrometry equipped with electrospray ionization source in positive ionization mode.Quantification was performed using multiple reactions monitoring(MRM)mode.The linear ranges of the seven analytes were 2.5~100μg·mL^(-1)(r=0.9996),1~40μg·mL^(-1)(r=0.9995),1~40μg·mL^(-1)(r=0.9995),5~200μg·mL^(-1)(r=0.9996),0.1~4μg·mL^(-1)(r=0.9995),0.05~2μg·mL^(-1)(r=0.9998)and 0.01~0.4μg·mL^(-1)(r=0.9995),respectively.The content ranges of seven components in six batches were 0.894%~1.072%,0.260%~0.285%,0.223%~0.268%,3.88%~4.05%,0.00726%~0.00898%,0.000840%~0.00195%and 0.000779%~0.00104%,respectively.The established method is sensitive and stable,and can provide a research method for the quality control of Gentianae Radix Et Rhizoma.

关 键 词：龙胆 环烯醚萜苷 黄酮 超快速液相色谱-串联质谱法 

分 类 号：S859.79[农业科学—临床兽医学]