液质联用法定性检测熟大黄配方颗粒中的土大黄苷和番泻苷A  

Identification of Rhaponticin and Sennoside A in Stewed Rhubarb Granule by HPLC-MS/MS

作　　者：王劲 曲国晶 WANG Jin;QU Guo-jing(Heze City Institute for Food and Drug Control,Shandong Heze 274000,China)

机构地区：[1]菏泽市食品药品检验检测研究院,山东菏泽274000

出　　处：《中国药物评价》2024年第3期204-208,共5页Chinese Journal of Drug Evaluation

摘　　要：目的:应用液质联用法定性检测熟大黄配方颗粒中土大黄苷和番泻苷A。方法:采用HPLC-MS/MS法同时检测土大黄苷和番泻苷A,使用Welch UHPLC XB-C_(18)色谱柱(2.1 mm×150 mm,1.8μm),采用0.1%甲酸水-甲醇梯度洗脱,柱温35℃,流速0.3 mL·min^(-1),采用ESI离子源,多反应模式(MRM)模式。结果:该方法对土大黄苷和番泻苷A的检出浓度分别为:2.0 ng·mL^(-1)、8.0 ng·mL^(-1),用该方法检测了山东省内市售的8批熟大黄配方颗粒,均未检出土大黄苷和番泻苷A。结论:该方法专属性强,灵敏度好,能快速定性检查熟大黄配方颗粒中是否含有土大黄苷和番泻苷A,可用于熟大黄(药用大黄)配方颗粒的质量控制。Objective:To found a method for the identification of rhaponticin and sennoside A in Stewed Rhubarb Granule by LC-MS.Methods:An HPLC-MS/MS in MRM mode was adopted.Welch UHPLC XB-C_(18)(2.1 mm×150 mm,1.8μm)column was applied with methanol-0.1%phosphoric acid solution as the mobile phase.The Liquid phase flow velocity was 0.3 mL·min^(-1),The temperature of colum was 35℃.The MS/MS system was operated by using an electrospray ionization probe.Scan mode was in multiple reaction ion monitoring(MRM)mode.Results:Limits of detection were 2.0 ng·mL^(-1)for Rhaponticin and 8.0 ng·mL^(-1)for Sennoside A.Rhaponticin and Sennoside A weren′t found in 8 batches of samples.Conclusion:The method is exclusive and could not only identify the true or false Stewed Rhubarb,but also examine the purity.It′s necessary for the quality control of Stewed Rhubarb Granule.

关 键 词：熟大黄配方颗粒 土大黄苷 番泻苷A 

分 类 号：R284.2[医药卫生—中药学]