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建立并验证了一种毛细管电泳法,用于测定氯喹对映异构体的立体异构体纯度。

Development and validation of a capillary electrophoresis assay for the determination of the stereoisomeric purity of chloroquine enantiomers.

机构信息

Department of Pharmaceutical Chemistry, Friedrich Schiller University Jena, Jena, Germany.

出版信息

Electrophoresis. 2011 Oct;32(19):2669-72. doi: 10.1002/elps.201000610. Epub 2011 Sep 8.

DOI:10.1002/elps.201000610
PMID:21905044
Abstract

A stereoselective CE assay for the determination of the enantiomeric purity of (R)-(-)-chloroquine and (S)-(+)-chloroquine was developed and validated. The separations were performed in a 50.2/40 cm uncoated fused silica capillary at 20°C using a 100 mM sodium phosphate buffer, pH 2.5, containing 30 mg/mL sulfobutylether(VII)-β-cyclodextrin as background electrolyte operated at an applied voltage of -25 kV and 20°C. The detection wavelength was 225 nm. Carbamazepine was used as internal standard. The assay was validated in the range of 0.05-1.0% for the respective minor chloroquine enantiomer based on a concentration of 3 mg/mL of the major enantiomer, either (R)-(-)-chloroquine or (S)-(+)-chloroquine. The method was applied to analyze the stereoisomeric purity of synthetic samples of the chloroquine enantiomers.

摘要

建立并验证了一种用于测定(R)-(-)-氯喹和(S)-(+)-氯喹对映体纯度的手性毛细管电泳分析方法。在 20°C 下,使用未涂层的 50.2/40 cm 熔融石英毛细管,以 100 mM 磷酸钠缓冲液(pH 2.5)为背景电解质,其中含有 30 mg/mL 的磺丁基醚(VII)-β-环糊精,施加-25 kV 的电压和 20°C 的温度进行分离。检测波长为 225nm。卡马西平用作内标。该方法基于浓度为 3 mg/mL 的主要对映异构体(R)-(-)-氯喹或(S)-(+)-氯喹,在各自的少量氯喹对映异构体的 0.05-1.0%范围内进行验证。该方法应用于分析合成的氯喹对映异构体样品的立体异构体纯度。

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