基于LC-MS联用的杜仲主要化学成分定性及定量分析
投稿时间:2019-01-29     点此下载全文
引用本文:雒晓梅,宿美凤,常晓燕,王小明,李壮壮,王卫华,孙桂波,石钺.基于LC-MS联用的杜仲主要化学成分定性及定量分析[J].中国现代中药,2019,21(8):1029-1040
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作者中文名作者英文名单位中文名单位英文名E-Mail
雒晓梅 LUO Xiao-mei 北京协和医学院 中国医学科学院 药用植物研究所,北京100193 Institute of Medicinal Plant Development,Chinese Academy of Medical Science,Peking Union Medical College,Beijing 100193,China  
宿美凤 SU Mei-feng 北京协和医学院 中国医学科学院 药用植物研究所,北京100193 Institute of Medicinal Plant Development,Chinese Academy of Medical Science,Peking Union Medical College,Beijing 100193,China  
常晓燕 CHANG Xiao-yan 北京协和医学院 中国医学科学院 药用植物研究所,北京100193 Institute of Medicinal Plant Development,Chinese Academy of Medical Science,Peking Union Medical College,Beijing 100193,China  
王小明 WANG Xiao-ming 北京协和医学院 中国医学科学院 药用植物研究所,北京100193 Institute of Medicinal Plant Development,Chinese Academy of Medical Science,Peking Union Medical College,Beijing 100193,China  
李壮壮 LI Zhuang-zhuang 北京协和医学院 中国医学科学院 药用植物研究所,北京100193 Institute of Medicinal Plant Development,Chinese Academy of Medical Science,Peking Union Medical College,Beijing 100193,China  
王卫华 WANG Wei-hua 清华大学 药学技术中心,北京100084 Center of Pharmaceutical Technology,Tsinghua University,Beijing 100084,China  
孙桂波 SUN Gui-bo 北京协和医学院 中国医学科学院 药用植物研究所,北京100193 Institute of Medicinal Plant Development,Chinese Academy of Medical Science,Peking Union Medical College,Beijing 100193,China  
石钺 SHI Yue 北京协和医学院 中国医学科学院 药用植物研究所,北京100193 Institute of Medicinal Plant Development,Chinese Academy of Medical Science,Peking Union Medical College,Beijing 100193,China 石钺,研究员,研究方向:中药及复方药效物质基础及其质量控制方法;Tel:(010)57833255,E-mail:shiyue1029@126.com 
基金项目:中医药行业科研专项(201507004)
中文摘要:目的:建立超高效液相串联质谱(UPLC-MS/MS)对杜仲主要成分定量及定性的方法。方法:采用UPLC-QE高分辨质谱负离子监测模式进行定性分析;采用UPLC-MS/MS法,负离子多反应监测(MRM)模式进行含量测定,分析杜仲中松脂醇二葡萄糖苷、松脂醇单葡萄糖苷、丁香脂素二葡萄糖苷、桃叶珊瑚苷、京尼平苷、京尼平苷酸、车叶草苷共7个主要成分的含量。结果:定性共鉴定出98个化合物,包括木脂素类38个,环烯醚萜类13个,黄酮类9个,苯丙素类15个,酚类7个,其余化合物共16个;定量分析在考察的浓度范围内测定的成分线性关系良好(r>0.995 7),精密度RSD<3.42%,重复性RSD<4.32%,回收率(n=9)均在91.04%~108.15%,RSD均小于4.89%。结论:该方法灵敏度高、重复性好,分析快速、准确、可靠,可用于定性、定量检测杜仲中主要化学成分,为综合评价杜仲的质量提供参考。
中文关键词:杜仲  超高效液相串联质谱  化学成分  含量测定
 
Qualitative and Quantitative Analysis of Main Chemical Constituents in Eucommia ulmoides by LC-MS
Abstract:Objective:The study is aimed at establishing a method for quantitative and qualitative determination of main components of Eucommia ulmoides by ultrahigh performance liquid phase tandem mass spectrometry(UPLC-MS/MS).Methods:UPLC-QE method was used for qualitative analysis with negative ion detection model.UPLC-MS/MS method with negative ion MRM detection mode were used to determine the contents of 7 main components in the E.ulmoides(pinoresinol diglucoside,pinoresinol-4-O-glucoside,geniposidic acid,liriodendrin,asperuloside,geniposide).Results:A total of 99 chromatographic peaks were identified,including 38 lignin,13 iridoterpenes,9 flavonoids,15 phenylalexins,7 phenols and 17 other compounds.The linear relationship of the components measured in the concentration range examined was good(r>0.995 7),the precision RSD<3.42%,the reproducible RSD<4.32%,and the recoveries rate(n=9)were ranged from 91.04% to 108.15%,and the RSD was smaller than 4.89%.Conclusion:The UPLC-MS/MS method has high sensitivity and good reproducibility,and the analysis is fast,accurate and reliable.It can be used to qualitatively and quantitatively detect the main chemical components in E.ulmoides,and provide a reference for comprehensive evaluation of E.ulmoides quality.
keywords:Eucommia ulmoides Oliv.  UPLC-MS/MS  chemical constituent  content determination
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