基于诱导圆二色性技术的高速逆流色谱法拆分外消旋反式-δ-viniferin。
Enantioseparation of racemic trans-δ-viniferin using high speed counter-current chromatography based on induced circular dichroism technology.
机构信息
State Key Laboratory of Natural Medicines, Department of Natural Medicinal Chemistry, China Pharmaceutical University, 24 Tong Jia Xiang, Nanjing 210009, Jiangsu, China.
State Key Laboratory of Natural Medicines, Department of Natural Medicinal Chemistry, China Pharmaceutical University, 24 Tong Jia Xiang, Nanjing 210009, Jiangsu, China.
出版信息
J Chromatogr A. 2014 Jan 10;1324:164-70. doi: 10.1016/j.chroma.2013.11.037. Epub 2013 Nov 23.
A preparative chiral high speed counter-current chromatography (HSCCC) method based on induced circular dichroism (ICD) spectrum was developed to separate trans-δ-viniferin (TVN) enantiomers successfully. The important parameters for the chiral HSCCC separation process, including the type of chiral selector (CS), the concentration of chiral selector and the equilibrium temperature, were optimized using induced circular dichroism spectrum. The final separation procedure was established with a biphasic solvent system composed of n-hexane-ethyl acetate-25 mmol L(-1) hydroxypropyl-β-cyclodextrin aqueous solution (5:5:10, v/v/v) in the head-to-tail elution mode at 5 °C. Under optimum chiral HSCCC separation conditions, 8.2mg of (7S, 8S)-TVN (1) and 9.4 mg of (7R, 8R)-TVN (2) were successfully separated from 20mg TVN enantiomers with the purity of 99.51% and 99.36%, respectively.
一种基于诱导圆二色性（ICD）光谱的制备性手性高速逆流色谱（HSCCC）方法被开发出来，成功地分离反式-δ-viniferin（TVN）对映体。手性 HSCCC 分离过程的重要参数，包括手性选择器（CS）的类型、手性选择器的浓度和平衡温度，均使用诱导圆二色性光谱进行了优化。最终的分离程序采用两相溶剂系统建立，在头对尾洗脱模式下，在 5°C 下，由正己烷-乙酸乙酯-25mmolL(-1)羟丙基-β-环糊精水溶液（5:5:10，v/v/v）组成。在最佳手性 HSCCC 分离条件下，从 20mg TVN 对映体中成功分离出 8.2mg（7S,8S）-TVN（1）和 9.4mg（7R,8R）-TVN（2），纯度分别为 99.51%和 99.36%。
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