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采用毛细管电泳分离和二极管阵列检测法测定药品中的氨氯地平对映体。

Determination of amlodipine enantiomers in pharmaceuticals using capillary electrophoresis separation and diode array detection.

作者信息

Mikus P, Maráková K, Valásková I, Havránek E

机构信息

Department of Pharmaceutical Analysis and Nuclear Pharmacy, Faculty of Pharmacy, Comenius University, Odbojárov 10, SK-832 32 Bratislava, Slovak Republic.

出版信息

Pharmazie. 2009 Feb;64(2):76-9.

Abstract

The present work describes a capillary zone electrophoresis (CZE) separation technique coupled with on-capillary diode array detector (DAD) for highly reliable enantioselective determination of amlodipine (AML) in commercial tablets. For the separation of AML enantiomers, (2-hydroxypropyl)-beta-cyclodextrin (HP-beta-CD) was an appropriate chiral selector providing complete enantioresolution. Optimized separation conditions consisted of 50 mmol/l glycine-acetate buffer, pH 3.2, 50 mg/ml HP-beta-CD. Hydroxyethylcellulose (HEC, 0.2% w/v) served as an electroosmotic flow (EOF) suppressor in this buffer. DAD detection was used for the characterization of the composition of separated zones according to differences in corresponding UV-VIS spectra (scanned in interval 200-800 nm). It was demonstrated, comparing reference and real spectra of the analytes, that the proposed separation method was selective enough to produce pure (non-mixed, i.e. spectrally homogeneous) analyte zones without any interfering compound. Successful validation and application of the proposed CZE-DAD method suggest its routine use in enantioselective control of AML in pharmaceuticals.

摘要

本研究描述了一种毛细管区带电泳(CZE)分离技术与毛细管上二极管阵列检测器(DAD)联用的方法,用于可靠地对市售片剂中的氨氯地平(AML)进行对映体选择性测定。对于AML对映体的分离,(2-羟丙基)-β-环糊精(HP-β-CD)是一种合适的手性选择剂,可实现完全的对映体拆分。优化的分离条件包括50 mmol/l甘氨酸-乙酸缓冲液(pH 3.2)、50 mg/ml HP-β-CD。羟乙基纤维素(HEC,0.2% w/v)在该缓冲液中用作电渗流(EOF)抑制剂。根据相应紫外-可见光谱(在200-800 nm区间扫描)的差异,采用DAD检测来表征分离区的组成。通过比较分析物的参考光谱和实际光谱表明,所提出的分离方法具有足够的选择性,能够产生纯的(非混合的,即光谱均匀的)分析物区,且无任何干扰化合物。所提出的CZE-DAD方法的成功验证和应用表明其可常规用于药物中AML的对映体选择性控制。

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