基于UHPLC-QE Plus-MS/MS法分析柴黄颗粒及柴胡中化学成分  

Analysis of chemical constituents of Chaihuang Granules by UHPLCQE Plus-MS/MS

作　　者：陈晶 傅欣彤 陈有根 郭洪祝 CHEN Jing;FU Xin-tong;CHEN You-gen;GUO Hong-zhu(NMPA Key Laboratory for Quality Evaluation of Traditional Chinese Patent Medicine,Beijing Key Laboratory of Components Analysis and Biological Evaluation on Chinese Medicine,Beijing Institute for Drug Control,Beijing 102206,China)

机构地区：[1]北京市药品检验研究院国家药品监督管理局中成药质量评价重点实验室中药成分分析与生物评价北京市重点实验室,北京102206

出　　处：《中草药》2022年第15期4634-4644,共11页Chinese Traditional and Herbal Drugs

摘　　要：目的 基于UHPLC-QE Plus-MS/MS方法分析柴黄颗粒以及柴胡的化学成分,明确其质量特征。方法 以5%氨甲醇溶液超声提取,采用Luna Omega色谱柱(100 mm×2.1 mm,1.6μm),以乙腈-0.1%甲酸溶液进行梯度洗脱,体积流量0.3m L/min。电喷雾离子源(ESI),负离子模式下采集。根据精确相对分子质量以及二级离子碎片信息,结合相对保留时间,通过查阅文献以及和对照品比对,进行成分指认。结果 鉴定出柴胡药材中化合物50个;柴黄颗粒中71个化合物,其中36个峰归属于黄芩,33个归属于柴胡。结论 建立的方法能快速、准确分析柴黄颗粒和柴胡化学成分,归纳各主要成分裂解规律,并通过与两者成分比较,发现柴胡配伍前后化学成分的变化,提示柴黄颗粒及柴胡中的质控成分。Objective To analyze and identify the chemical components and characteristic components of Chaihuang Granules(柴黄颗粒)and Chaihu(Bupleuri Radix)by UHPLC-QE Plus-MS/MS.Methods The samples were extracted with 5%ammonia-methanol solution by ultrasonic.The analyses was performed on a Luna Omega C18 column(100 mm×2.1 mm,1.6μm),the mobile phase was acetonitrile−0.1%formic acid solution with gradient elution mode at the flow rate of 0.3 mL/min.Electrospray ion source(ESI)was applied in negative ion mode.The chemical constituents were analyzed by exact relative molecular weight,fragment ion and the relative retention time and comparation with the related literature and reference standards.Results A total of 50 chemical compounds were identified from Bupleuri Radix,71 chemical compounds in Chaihuang Granules were identified,among which 36 compounds were attributed to Huangqin(Scutellariae Radix)and 33 compounds were attributed to Bupleuri Radix.Conclusion The method is fast and highly sensitive for the screening and confirmation of the chemical constituents from Chaihuang Granules and Bupleuri Radix.The fragmentation characteristics were summarized in this paper.By comparing the chemical constituents in Chaihuang Granules and Bupleuri Radix,the chemical composition changes before and after compatibility can be found,which suggested a reference for the quality control components of Chaihuang Granules and Bupleuri Radix.

关 键 词：柴黄颗粒 柴胡 黄芩 UHPLC-QE Plus-MS/MS 柴胡皂苷v 柴胡皂苷p 柴胡皂苷a 野黄芩苷 

分 类 号：R284.1[医药卫生—中药学]