使用基于环糊精的手性固定相从药物剂型中高效液相色谱法拆分硫利达嗪对映体。

HPLC resolution of thioridazine enantiomers from pharmaceutical dosage form using cyclodextrin-based chiral stationary phase.

作者信息

Bhushan R, Gupta Deepak

机构信息

Department of Chemistry, Indian Institute of Technology Roorkee, Roorkee 247 667, India.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2006 Jun 6;837(1-2):133-7. doi: 10.1016/j.jchromb.2006.03.042. Epub 2006 May 3.

DOI:10.1016/j.jchromb.2006.03.042

PMID:16675310

Abstract

Resolution of racemic thioridazine obtained from Thioril tablets (Cipla Ltd., Goa, India) into its enantiomers has been achieved by HPLC using a beta-cyclodextrin (CD)-bonded stationary phase. Thioridazine was isolated from commercial formulations and was purified using preparative TLC. The purity was ascertained by RP-HPLC. For the resolution of rac-thioridazine using cyclodextrin based CSP and mobile phase of 0.05 M phosphate buffer (pH 6.5)-acetonitrile (50:50) was found to be successful. The optimum conditions of resolution were established by systematically studying the effect of organic modifier, concentration of buffer, pH and flow rate of mobile phase. The detection limit was found to be 10 microg (5 microg of each enantiomer). The enantiomeric purity of each of the resolved isomers was verified by optical rotation.

摘要

通过使用β-环糊精（CD）键合固定相的高效液相色谱法（HPLC），实现了从硫利达嗪片（印度果阿西普拉有限公司）获得的外消旋硫利达嗪拆分为其对映体。硫利达嗪从市售制剂中分离出来，并使用制备薄层层析法进行纯化。纯度通过反相高效液相色谱法确定。发现使用基于环糊精的手性固定相和0.05 M磷酸盐缓冲液（pH 6.5）-乙腈（50:50）的流动相拆分外消旋硫利达嗪是成功的。通过系统研究有机改性剂、缓冲液浓度、pH值和流动相流速的影响，确定了最佳拆分条件。检测限为10微克（每种对映体5微克）。通过旋光法验证了每种拆分异构体的对映体纯度。