Chromatographic separation of chlorthalidone enantiomers using β-cyclodextrins as chiral additives
Chromatographic separation of chlorthalidone enantiomers using β-cyclodextrins as chiral additives
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DOI：
10.1016/s0378-4347(00)00103-1
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发表时间：
2000-04-14
期刊：
影响因子：
--
通讯作者：
Campíns-Falcó, P
中科院分区：
文献类型：
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作者：
Herráez-Hernández, R;Campíns-Falcó, P
用不同的β-环糊精作为流动相手性添加剂，在C-18LiChrospher(125×4 mm i.d.)色谱柱上进行了氯苯醚酮对映体的色谱分析。纵队。考察了流动相组成(有机溶剂比例、缓冲液类型、pH值)、流动相流速、β-环糊精的种类和浓度对拆分的影响。甲醇和0.1M磷酸盐缓冲液，pH 4，含2%三乙胺(v/v)和12.5 mMβ-环糊精的25：75混合溶液，流速为0.8ml/min，是拆分氯替利酮对映体的最佳选择。在此条件下，检测波长为230 nm，线性范围为0.5-20微克/毫升。两种异构体的检出限均为50 ng/ml。通过对不同药物制剂中氯苯醚酮的分析，验证了该方法的实用性。文中还给出了生物样品的应用实例。(C)2000 Elsevier Science B.V.保留所有权利。
Different beta-cyclodextrins have been tested as chiral additives in the mobile phase for the chromatographic analysis of chlorthalidone enantiomers in a C-18 LiChrospher (125x4 mm I.D.) column. The effect on enantioresolution of different parameters was studied: composition of the mobile phase (percentage of organic solvent, type of buffer and pH), mobile phase flow-rate, and type and concentration of beta-cyclodextrin. A 25:75 mixture of methanol and 0.1 M phosphate buffer, pH 4, containing 2% triethylamine (v/v), and 12.5 mM beta-cyclodextrin, at a flow-rate of 0.8 ml/min, was found to be the best option for the resolution of chlorthalidone enantiomers. Under such conditions, linear calibration curves were obtained in the 0.5-20-mu g/ml interval using UV detection at 230 nm. The limit of detection for both isomers was 50 ng/ml. The utility of the described assay has been tested by analyzing chlorthalidone in different pharmaceutical preparations. Examples of application to biological samples are also given. (C) 2000 Elsevier Science B.V. All rights reserved.