Separation and characterization of silybin, isosilybin, silydianin and silychristin in milk thistle extract by liquid chromatography-electrospray tandem mass spectrometry
Separation and characterization of silybin, isosilybin, silydianin and silychristin in milk thistle extract by liquid chromatography-electrospray tandem mass spectrometry
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DOI：
10.1016/j.chroma.2006.03.053
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发表时间：
2006-05-26
影响因子：
4.1
通讯作者：
Barrett, Jeffrey S.
中科院分区：
文献类型：
--
作者：
Lee, James I.;Hsu, Bih H.;Barrett, Jeffrey S.
建立了一种高效液相色谱/串联质谱（LC/MS/MS）分析水飞蓟提取物中水飞蓟素的方法。本研究采用醋酸铵-甲醇/水/甲酸梯度流动相体系，在YMC ODS-AQ高效液相色谱柱上完全分离水飞蓟苷、水飞蓟素、水飞蓟宾的非对映体（水飞蓟宾A和B）和异水飞蓟宾的非对映体（异水飞蓟宾A和B） 6种主要活性成分。主要成分的鉴定和表征不仅基于产物离子扫描，它提供了所选分子离子的独特碎片化信息，而且基于多反应监测（MRM）数据的特定碎片化，这证实了LC色谱峰的保留时间。该方法应用于水飞蓟素存在的人血浆样品的分析，似乎适用于药代动力学研究，其中水飞蓟素成分的区分是必不可少的。(c) 2006 Elsevier B.V.版权所有
A selective and sensitive liquid chromatography/tandem mass spectrometry (LC/MS/MS) method has been developed for the characterization of silymarin in commercially available milk thistle extract. In this study, six main active constituents, including silydianin, silychristin, diastereomers of silybin (silybin A and B) and diastereomers of isosilybin (isosilybin A and B) in silymarin, were completely separated on a YMC ODS-AQ HPLC column using a gradient mobile phase system comprised of ammonium acetate and methanol/water/formic acid. Identification and characterization of the major constituents were based not only on the product ion scan, which provided unique fragmentation information of a selected molecular ion, but also on the specific fragmentation of multiple reaction monitoring (MRM) data, which confirmed the retention times of LC chromatographic peaks. The method was applied in the analysis of human plasma samples in the presence of silyrnarin and appeared to be suitable for the pharmacokinetic studies in which the discrimination of silymarin constituents is essential. (c) 2006 Elsevier B.V. All rights reserved.