HPLC-ELSD和UPLC-MS/MS法考察复方金银花颗粒中金银花投料规范性  

Research on Standard Feeding of Lonicerae Japonicae Flos in Compound Honeysuckle Granules by HPLC-ELSD and UPLC-MS/MS

作　　者：王舒 姚奕然 黄赛燕 刘欢欢 徐丹洋 周谧 WANG Shu;YAO Yiran;HUANG Saiyan;LIU Huanhuan;XU Danyang;ZHOU Mi(Nantong Food and Drug Control Center,Nantong Jiangsu 226006,China.)

机构地区：[1]南通市食品药品监督检验中心,江苏南通226006

出　　处：《药品评价》2022年第24期1485-1489,共5页Drug Evaluation

基　　金：南通市市级科技项目(JCZ20171)。

摘　　要：目的:建立高效液相-蒸发光散射法(HPLC-ELSD)和超高效液相-质谱联用法(UPLC-MS/MS)对复方金银花颗粒中山银花成分灰毡毛忍冬皂苷乙进行检查,对制剂中金银花投料的规范性进行研究。方法:以山银花的特征组分灰毡毛忍冬皂苷乙为检测指标,采用HPLC-ELSD法进行限度检查,色谱柱:Agilent Zorbax Eclipse Plus C18(250 mm×4.6 mm,5μm);流动相:乙腈-0.4%乙酸溶液,梯度洗脱;流速:1.0 mL/min;蒸发光散射检测器。采用UPLCMS/MS法对结果进行验证,以m/z 1399.8→633.2和m/z 1399.8→795.2作为检测离子对,电喷雾正离子模式(ESI+),多反应监测(MRM)。结果:30批次样品中,有15批次检出灰毡毛忍冬皂苷乙特征组分,说明市售的该制剂品种中存在以山银花替代金银花投料的情况。结论:建立的该方法可以很好地控制复方金银花颗粒中金银花投料的规范性。Objective:To establish HPLC-ELSD and UPLC-MS/MS methods for the detection of macranthoidin B of lonicerae flos in compound honeysuckle granules,and to investigate the phenomenon of illegal feeding.Methods:An HPLCELSD method was used to determine lonicerae flos with macranthoidin B as the index.HPLC-ELSD method was used with Agilent Zorbax Eclipse Plus C18(250 mm×4.6 mm,5μm)as analytical column.Acetonitrile and 0.4%acetic acid were used as mobile phase for gradient elution,the flow rate was 1.0 mL/min and ELSD detector was used.UPLC-MS/MS method was applied to verifying the results.The positive electrospray ionization and multiple reaction monitoring were adopted with the transitions of m/z 1399.8→633.2 and m/z 1399.8→795.2.Results:The characteristic component of macranthoidin B was detected in 15 batches of 30 samples,which indicated that there was a situation of replacing lonicerae japonicae flos with lonicerae flos in the market.Conclusion:The established method can well control the standard feeding of lonicerae japonicae flos in compound honeysuckle granules.

关 键 词：复方金银花颗粒 金银花 灰毡毛忍冬皂苷乙 高效液相-蒸发光散射法 超高效液相-质谱联用法 

分 类 号：R286.0[医药卫生—中药学] O657.63[医药卫生—中医学]