Mikus P, Maráková K, Valásková I, Havránek E
Department of Pharmaceutical Analysis and Nuclear Pharmacy, Faculty of Pharmacy, Comenius University, Odbojárov 10, SK-832 32 Bratislava, Slovak Republic.
Pharmazie. 2009 Feb;64(2):76-9.
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.
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。