Separation and characterization of active flavonolignans of Silybum marianum by liquid chromatography connected with hybrid ion-trap and time-of-flight mass spectrometry (LC-MS/IT-TOF).
Separation and characterization of active flavonolignans of Silybum marianum by liquid chromatography connected with hybrid ion-trap and time-of-flight mass spectrometry (LC-MS/IT-TOF).
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DOI：
10.1021/np070136b
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发表时间：
2007-09
影响因子：
5.1
通讯作者：
M. Shibano;A. Lin;H. Itokawa;K. Lee
中科院分区：
文献类型：
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作者：
M. Shibano;A. Lin;H. Itokawa;K. Lee
水飞蓟素A（1）和B（2）、水飞蓟素（3）、水飞蓟宾A（4）和B（5）、以及异水飞蓟宾A（6）和B（7）是水飞蓟素中的主要生物活性黄酮木脂体，水飞蓟素是一种来自水飞蓟的草药。采用半微量高效液相色谱法，以Nucleosil 100-3 C 18 HD为固定相，甲醇/水/甲酸移动的为流动相，对7种主要活性黄酮木脂素（包括1/ 2、4/ 5和6/ 7）进行了分离。采用混合离子阱飞行时间质谱（IT-TOF MS）对这些黄酮木脂素的碰撞诱导解离（CID）MS/MS和MS（3）谱进行了系统研究。基于所得CID-MS/MS或MS（3）谱的比较，可以有效区分七种黄酮木脂素（1- 7）。通过IT-TOF高分辨率质谱解析每个特征MS/MS或MS（3）裂解模式。本方法学的结果表明，液相色谱-质谱IT-TOF（LC-MS/IT-TOF）可用于从植物提取物中筛选活性天然产物，并用于水飞蓟素的特定质量控制。
Silychristins A (1) and B (2), silydianin (3), silybins A (4) and B (5), and isosilybins A (6) and B (7) are major bioactive flavonolignans in silymarin, a herbal remedy derived from the milk thistle Silybum marianum. In this study, the seven major active flavonolignans including the diastereomers 1/ 2, 4/ 5, and 6/ 7 were completely separated using semi-micro-high performance liquid chromatography (HPLC) with a Nucleosil 100-3 C 18 HD column and a MeOH/water/formic acid mobile phase system. The collision-induced dissociation (CID) MS/MS and MS (3) spectra of these flavonolignans were studied systematically using hybrid ion-trap and time-of-flight (IT-TOF) mass spectrometry. Efficient differentiation between the seven flavonolignans (1- 7) was possible based on comparison of the resultant CID-MS/MS or MS (3) spectra. Each characteristic MS/MS or MS (3) fragmentation pattern was elucidated with high-resolution mass spectra by IT-TOF. The results with the present methodology show that liquid chromatography-mass spectrometry IT-TOF (LC-MS/IT-TOF) can be useful for general screening of active natural products from plant extracts and for the specific quality control of silymarin.