HPLC和UPLC-MS/MS法考察清热解毒口服液中金银花投料规范性  

Research on Standard Feeding of Lonicerae Japonicae Flos in Qingre Jiedu Oral Solution by HPLC and UPLC-MS/MS

作　　者：郑文燕 李哲 冯启宏 许润娟 Zheng Wenyan;Li Zhe;Feng Qihong;Xu Runjuan(Zhongshan Institute for Food and Drug Control,Guangdong Zhongshan 528400,China)

机构地区：[1]中山市食品药品检验所,广东中山528400

出　　处：《中国药师》2022年第1期189-193,共5页China Pharmacist

摘　　要：目的:建立HPLC-ELSD和UPLC-MS/MS法,对清热解毒口服液中金银花投料的规范性进行考察。方法:以山银花的特征成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:SUPELCO DISCOVER C_(18)(250 mm×4.6 mm,5μm);流动相:乙腈-水,梯度洗脱;流速:1.0 ml·min^(-1);柱温:30℃;进样量:10μl;采用UPLC-MS/MS法对结果进行验证,以m/z 1397.5→1073.4、m/z 1397.5→911.3作为检测离子对,离子化模式为ESI-,进行多反应监测。结果:19批次样品中,有7批次检出灰毡毛忍冬皂苷乙,说明市售该制剂品种中存在以山银花替代金银花投料的情况。结论:所建立的方法可以有效地控制清热解毒口服液中金银花投料的规范性。Objective:To study the quality of Lonicerae Japonicae Flos in Qingre Jiedu oral solution by HPLC and UPLC-MS/MS.Methods:An HPLC-ELSD method was used to determine Lonicerae Flos with macranthoidin B as the index.The separation process was performed on a SUPELCO DISCOVER C_(18)(250 mm×4.6 mm,5μm)column with gradient elution.The mobile phase consisted of acetonitrile-water and the flow rate was 1.0 ml·min^(-1).UPLC-MS/MS was applied to verifying the results.The negative electrospray ionization and multi reaction monitoring were adopted with the transitions of m/z 1397.5→1073.4 and m/z 1397.5→911.3.Results:Macranthoidin B was detected out in 7 batches of 19 samples,indicating Lonicerae Flos might be used in the samples.Conclusion:The established methods can be used to control the quality of Lonicerae Japonicae Flos in Qingre Jiedu oral solution.

关 键 词：清热解毒口服液 金银花 高效液相色谱-蒸发光检测器法 超高效液相色谱-串联质谱法 灰毡毛忍冬皂苷乙 

分 类 号：TQ460.72[医药卫生—药物分析学]