García-Ruiz C, Marina M L
Departamento de Química Analítica, Facultad de Ciencias, Universidad de Alcalá, Madrid, Spain.
Electrophoresis. 2000 May;21(8):1565-73. doi: 10.1002/(SICI)1522-2683(20000501)21:8<1565::AID-ELPS1565>3.0.CO;2-2.
Electrokinetic chromatography (EKC) was employed to achieve the enantiomeric separation of a group of chiral 1,4-dihydropyridines (DHPs) with pharmacological activity. Micelles of bile salts alone or mixed with neutral cyclodextrins, micelles of sodium dodecyl sulfate (SDS) mixed with neutral cyclodextrins, and anionic cyclodextrin derivatives, i.e., carboxymethyl-gamma-cyclodextrin (CM-gamma-CD), carboxymethyl-beta-cyclodextrin (CM-beta-CD), and succinylated beta-cyclodextrin (Succ-beta-CD), were employed as pseudostationary phases. The enantiomeric separation ability of these chiral selectors with respect to DHPs was studied in different experimental conditions. CM-beta-CD was shown to be the best chiral selector to perform the enantiomeric separation of DHPs by EKC. Next, the influence of the CM-beta-CD concentration, the pH and nature of the buffer, the temperature, and the applied voltage on the enantiomeric resolution of DHPs was studied. The use of a 50 mM ammonium acetate buffer, pH 6.7, 25 mM in CM-beta-CD together with an applied voltage of 15 or 20 kV, and a temperature of 15 degrees C enabled the individual enantiomeric separation of twelve DHPs, each one into its two enantiomers, and their separation in multicomponent mixtures of up to six DHPs into all their enantiomers.
采用电动色谱法（EKC）对一组具有药理活性的手性1,4 - 二氢吡啶（DHP）进行对映体分离。单独的胆盐胶束或与中性环糊精混合的胶束、十二烷基硫酸钠（SDS）与中性环糊精混合的胶束以及阴离子环糊精衍生物，即羧甲基 - γ - 环糊精（CM - γ - CD）、羧甲基 - β - 环糊精（CM - β - CD）和琥珀酰化β - 环糊精（Succ - β - CD），被用作假固定相。在不同实验条件下研究了这些手性选择剂对DHP的对映体分离能力。结果表明，CM - β - CD是通过EKC对DHP进行对映体分离的最佳手性选择剂。接下来，研究了CM - β - CD浓度、缓冲液的pH值和性质、温度以及施加电压对DHP对映体拆分的影响。使用50 mM醋酸铵缓冲液（pH 6.7）、25 mM的CM - β - CD，外加15或20 kV的电压以及15℃的温度，能够将十二种DHP各自分离为其两种对映体，并将多达六种DHP的多组分混合物中的所有对映体进行分离。
