中国中药杂志

2017, v.42(20) 3945-3956

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基于UPLC技术的吴茱萸定性定量一体化研究
Qualitative and quantitative analysis of Evodiae Fructus based on the UPLC technology

樊小瑞;刘梓晗;冯伟红;刘晓谦;杨立新;王智民;李春;
FAN Xiao-rui;LIU Zi-han;FENG Wei-hong;LIU Xiao-qian;YANG Li-xin;WANG Zhi-min;LI Chun;National Engineering Laboratory for Quality Control Technology of Chinese Herbal Medicines,Institute of Chinese Materia Medica,China Academy of Chinese Medical Sciences;

摘要(Abstract):

采用UPLC建立吴茱萸指纹图谱和多成分同步测定方法。采用Waters Acquity BEH C_(18)色谱柱(2.1 mm×50 mm,1.7μm)色谱柱,0.2%甲酸乙腈-0.2%甲酸水为流动相,梯度洗脱,检测波长320 nm。以去氢吴茱萸碱为参照峰,通过对29批吴茱萸进行测定,建立了吴茱萸的UPLC指纹图谱,该指纹图谱可同时对24个共有峰进行检测,采用对照品对新绿原酸、绿原酸、隐绿原酸、金丝桃苷、异鼠李素-3-O-β-D-芸香糖苷、去氢吴茱萸碱、吴茱萸碱、吴茱萸次碱、吴茱萸卡品碱和二氢吴茱萸卡品碱共10个色谱峰进行了指认。采用国家药典委员会"中药色谱指纹图谱相似度评价软件"2008A版进行相似度评价,29批药材中有19批药材相似度大于0.9。此外,采用同一色谱条件对吴茱萸中的9个成分进行了同步测定。所测定的9个成分新绿原酸、隐绿原酸、金丝桃苷、异鼠李素-3-O-β-D-芸香糖苷、去氢吴茱萸碱、吴茱萸碱、吴茱萸次碱、吴茱萸卡品碱和二氢吴茱萸卡品碱分别在0.000 46~0.138,0.000 146~0.175,0.000 412~0.124,0.000 448~0.134,0.000 452~0.136,0.003 38~0.169,0.000 44~0.132,0.001 07~0.128,0.001 71~0.128μg与各自峰面积积分值成良好线性关系,9种成分的平均加样回收率分别为100.3%,100.4%,101.6%,97.51%,102.9%,101.4%,103.8%,104.0%,95.99%,RSD分别为2.4%,2.0%,3.0%,0.80%,1.9%,2.1%,1.1%,2.2%,2.4%。该文建立的UPLC方法在20 min内实现了对吴茱萸化学成分的全谱分离,与文献报道方法相比,该文在一个色谱条件下同时实现了吴茱萸指纹图谱测定和多成分同步测定,而且所建方法具有专属性强、分离度高、色谱峰纯度高、方法简单易行的特点,为吴茱萸药材同步进行定性和定量分析提供了依据。
An UPLC method was developed for the studies of fingerprint and quantification of multi-components for Evodiae Fructus. The chromatographic separation was performed on a C_(18) column( 2. 1 mm × 50 mm,1. 7 μm) with mobile phase of 0. 2% formic acid-acetonitrile and 0. 2% formic acid-water in gradient mode,and the detection wavelength was set at 320 nm. Dehydroevodiamine was used as the reference peak,there were 24 common peaks in the fingerprint of 29 samples were detected,and among them 10 chromatographic peaks were identified with the reference substance and they were neochlorogenic acid,chlorogenic acid,cryptochlorogenic acid,hyperin,isorhamnetin-3-O-β-D-rutinoside,dehydroevodiamine,evodiamine,rutaecarpine,evocarpine and dihydroevocarpine.The fingerprint data was evaluated with similarity evaluation system for chromatographic fingerprint of traditional Chinese medicine( Version 2008 A),and the similarity of 19 batches of Evodiae Fructus was greater than 0. 9 in the 29 samples. In addition,9 components including neochlorogenic acid,chlorogenic acid,hyperin,isorhamnetin-3-O-β-D-rutinoside,dehydroevodiamine,evodiamine,rutaecarpine,evocarpine and dihydroevocarpine were simultaneously determined at the same chromatographic conditions,whose peak area integral values showed good linear relationship at the range of 0. 000 46-0. 138,0. 000 146-0. 175,0. 000 412-0. 124,0. 000 448-0. 134,0. 000 452-0. 136,0. 003 38-0. 169,0. 000 44-0. 132,0. 001 07-0. 128,0. 001 71-0. 128,respectively. Their average recoveries were 100. 3%,100. 4%,101. 6%,97. 51%,102. 9%,101. 4%,103. 8%,104. 0%,95. 99%,and RSD were 2. 4%,2. 0%,3. 0%,0. 80%,1. 9%,2. 1%,1. 1%,2. 2%,2. 4%,respectively. The established UPLC method not only realized the full separation of all chemical constituents of Evodiae Fructus within 20 minutes,but also achieved the chromatographic fingerprint determination and simultaneous multi-components determination of Evodiae Fructus at the same chromatographic conditions. Compared with other methods in literatures,the method has the following characteristics of strong specificity,good separation,high purity of chromatographic peaks,simplity and feasibility,which provides better means for the simultaneous qualitative and quantitative analysis of Evodiae Fructus.

关键词(KeyWords): 吴茱萸;指纹图谱;多成分同步测定;超高效液相色谱
Evodiae Fructus;chromatographic fingerprint;simulataneous multi-component determination;UPLC

Abstract:

Keywords:

基金项目(Foundation): 国家科技支撑计划项目(2011BAI07B08)

作者(Author): 樊小瑞;刘梓晗;冯伟红;刘晓谦;杨立新;王智民;李春;
FAN Xiao-rui;LIU Zi-han;FENG Wei-hong;LIU Xiao-qian;YANG Li-xin;WANG Zhi-min;LI Chun;National Engineering Laboratory for Quality Control Technology of Chinese Herbal Medicines,Institute of Chinese Materia Medica,China Academy of Chinese Medical Sciences;

Email:

DOI: 10.19540/j.cnki.cjcmm.20170807.007

参考文献(References):

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