Separation of amlodipine besilate enantiomers by biphasic recognition recycling high-speed counter-current chromatography
Separation of amlodipine besilate enantiomers by biphasic recognition recycling high-speed counter-current chromatography
复制标题
双相识别循环高速逆流色谱分离苯磺酸氨氯地平对映体
DOI：
10.1016/j.seppur.2015.03.053
复制
发表时间：
2015-05
影响因子：
8.6
通讯作者：
Yang Weijun
中科院分区：
文献类型：
--
作者：
Zhang Panliang;Sun Genlin;Tang Kewen;Zhou Congshan;Yang Changan;Yang Weijun
采用两相识别循环高速逆流色谱法分离苯磺酸对映体。在水移动的相中加入亲水性磺丁基醚-β-环糊精（SBE-β-CD），在有机相中加入亲脂性酒石酸异丁酯（d-IBTA），建立了双相识别体系，该体系能分别优先识别（+）-对映体和（-）-对映体。根据ADB对映体的分配比和分离因子，选择了乙酸乙酯-水溶液（1：1，v/v）和上述手性选择剂组成的两相溶剂体系。考察了手性选择剂的种类、浓度、水溶液的pH值以及温度对分离效果的影响。通过制备型高速逆流色谱分离，30 mg外消旋体得到纯的对映体，纯度大于97.5%，回收率在80%~ 84%之间。实验结果表明，双相识别循环高速逆流色谱提供了一个有前途的手段，以低分离因子的外消旋体在一个高效的方式分离。
Biphasic recognition recycling high-speed counter-current chromatography (HSCCC) was applied for the separation of amlodipine besilate (ADB) enantiomers. The biphasic recognition system was established by adding hydrophilic sulfobutyl ether-β-cyclodextrin (SBE-β-CD) in the aqueous mobile phase and lipophilicd-iso-butyl tartrate (d-IBTA) in the organic stationary phase, which is capable of preferentially recognizing (+)-enantiomer and (−)-enantiomer respectively. The two-phase solvent system, which was composed of ethyl acetate–aqueous solution (1:1, v/v) plus the above chiral selectors, was selected as per the distribution ratios and separation factor of ADB enantiomers. Impacts of the type and concentration of chiral selectors, pH value of the aqueous solution as well as temperature on the separation efficiency were investigated. By means of preparative HSCCC, pure enantiomers were obtained through the separation of 30 mg racemates with a purity greater than 97.5% and a recovery rate between 80% and 84%. Experimental results revealed that biphasic recognition recycling high-speed counter-current chromatography offers a promising means to separate racemates with a low separation factor in a highly efficient manner.
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影响因子：
4.1
作者：
Maria Perez, Anna;Minguillon, Cristina
通讯作者：
Minguillon, Cristina
影响因子：
4.1
作者：
Tong, Shengqiang;Guan, Yi-Xin;Zhao, Liying
通讯作者：
Zhao, Liying
影响因子：
16.6
作者：
Afonso, CAM;Crespo, JG
通讯作者：
Crespo, JG
DOI：
10.1080/10826070701277133
发表时间：
2007-04
影响因子：
1.3
作者：
Y. Cai;Z. Yan;M. Zi;L. Yuan
通讯作者：
Y. Cai;Z. Yan;M. Zi;L. Yuan
影响因子：
7.4
作者：
Franco, P;Blanc, J;Minguillón, C
通讯作者：
Minguillón, C