UPLC-Q-TOF-MS/MS法定性分析丹膝颗粒的化学成分  

Qualitative Analysis on Chemical Constituents from Danxi Granules by UPLC-Q-TOF-MS/MS

作　　者：刘灿黄 章泽恒[2] 汪辉 何清彦 蒋桃 黄胜 LIU Canhuang;ZHANG Zeheng;WANG Hui;HE Qingyan;JIANG Tao;HUANG Sheng(Inslitute for Drug and Food Contrl of Changsha,Changsha Hunan 410208,China;Hunan drug evaluation and ADRmonitoring center,Changsha Hunan 410013,China;Hunan food and Drug Vocational College,Changsha Hunan 410208,China;JIUZHITANG co.,ltd.Changsha Hunan 410205,China)

机构地区：[1]长沙市食品药品检验所,湖南长沙410208 [2]湖南省药品审评认证与不良反应监测中心,湖南长沙410013 [3]湖南食品药品职业学院,湖南长沙410208 [4]九芝堂股份有限公司,湖南长沙410205

出　　处：《药品评价》2022年第4期201-209,共9页Drug Evaluation

基　　金：2020年湖南省自然科学基金科药联合项目(2020JJ9056)。

摘　　要：目的:采用超高效液相色谱-飞行时间质谱联用技术(UPLC-Q-TOF-MS/MS)对丹膝颗粒中的化学成分进行定性分析。方法:采用Atlantis®T3色谱柱(2.1 mm×250 mm,5μm),以乙腈-0.1%甲酸溶液为流动相进行梯度洗脱,流速为0.4 mL/min,柱温35℃,进样量2μL。质谱采用电喷雾(ESI)离子源,正、负离子模式监测,通过保留时间、相对分子质量、质谱碎片等信息,结合对照品碎片裂解规律及文献数据对检测到的化学成分进行定性分析。结果:由一级MS、二级MS/MS高分辨质谱数据共鉴定和推测出102个化合物。结论:首次利用UPLC-Q-TOF MS/MS技术对丹膝颗粒的主要成分进行定性分析,为其质量控制、药效物质基础、药理作用机制研究提供了参考。Objective:To analyze and identify the chemical constituents from danxi granules by UPLC-Q-TOF-MS/MS.Methods:Using Atlantis®T3 chromatographic column(2.1 mm×250 mm,5μm)with the temperature of 35℃,the mobile phase was acetonitrile-0.1%formic acid solution with gradient elution at a flow rate of 0.4 mL/min,the column temperature was 35℃,the injection volume was 2μL.The MS spectrum was acquired in both negative and positive ion modes using ESI ion source.The compounds were identified by retention time,relative molecular mass and mass spectrometry pyrolysis fragments,as well as fragmentation regularity sum-marized from reference substance and the literature.Results:Combining literature reports and high-resolution mass spectrometry data of MS and MS/MS.102 compounds from danxi granules were successfully identified and predicted.Conclusion:The study is the first to use UPLC-Q-TOF MS/MS technology to analyze the main components of danxi granules,which provides a reference for the overall quality,basis of medicinal materials and pharmacological mechanism of action.

关 键 词：丹参 丹膝颗粒 超高效液相色谱-飞行时间质谱 定性分析 

分 类 号：R284.1[医药卫生—中药学]