Lee James I, Hsu Bih H, Wu Di, Barrett Jeffrey S
Division of Clinical Pharmacology & Therapeutics, The Children's Hospital of Philadelphia, Abramson Research Center 916H, Philadelphia, PA 19104-4399, USA.
J Chromatogr A. 2006 May 26;1116(1-2):57-68. doi: 10.1016/j.chroma.2006.03.053. Epub 2006 Apr 24.
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 silymarin and appeared to be suitable for the pharmacokinetic studies in which the discrimination of silymarin constituents is essential.
已开发出一种选择性和灵敏的液相色谱/串联质谱（LC/MS/MS）方法，用于表征市售水飞蓟提取物中的水飞蓟素。在本研究中，水飞蓟素中的六种主要活性成分，包括水飞蓟宁、水飞蓟宾、水飞蓟宾的非对映异构体（水飞蓟宾A和B）以及异水飞蓟宾的非对映异构体（异水飞蓟宾A和B），在YMC ODS-AQ高效液相色谱柱上使用由醋酸铵和甲醇/水/甲酸组成的梯度流动相系统完全分离。主要成分的鉴定和表征不仅基于产物离子扫描，其提供了选定分子离子的独特碎片信息，还基于多反应监测（MRM）数据的特定碎片，其确认了液相色谱峰的保留时间。该方法应用于存在水飞蓟素的人体血浆样品分析，似乎适用于区分水飞蓟素成分至关重要的药代动力学研究。
