麦芽糖作选择剂西酞普兰手性毛细管电泳分析及拆分机理研究
麦芽糖,西酞普兰,手性分离,毛细管电泳,拆分机理,,麦芽糖,西酞普兰,手性分离,毛细管电泳,拆分机理,1引言,2实验部分,3结果与讨论,R
摘 要 研究了以麦芽糖为选择剂的毛细管电泳手性拆分方法。以抗抑郁药物西酞普兰对映体的分离和定量测定为实例,考察了分离条件,在40%(m/m)麦芽糖、8.0×10-2 mol/L磷酸盐运行缓冲液(pH 5.0)中,分离电压20 kV时,西酞普兰对映体分离度达2.3。测定S (+)西酞普兰中R(-)异构体的含量,在0.05~4.00 g/L浓度范围内线性关系良好。R(-)西酞普兰与S(+)西酞普兰的检出限分别为0.0453 g/L和00473 g/L,线性相关系数均>0.9978。以荧光光谱法对西酞普兰与麦芽糖的相互作用进行了考察,并较系统地对拆分机理进行了研究。证明麦芽糖的手性识别能力与其浓度有关,当麦芽糖达到一定浓度后将形成聚集体,而麦芽糖的拆分作用就主要体现在其聚集体疏水空腔的立体作用上。关键词 麦芽糖,西酞普兰,手性分离,毛细管电泳,拆分机理
Enantioseparation and Quantitative Analysis of Citalopram by Capillary Electrophoresis with Maltose as Chiral Selector and Its Separation Mechanism
Zhang Rong, Xiao Shangyou, Xu Hongmei, Huang Rui, Xia Zhining
1Department of Pharmaceutics, College of Chemistry and Chemical Engineering, Chongqing University, Chongqing 400044
2College of Bioengineering, Chongqing University, Chongqing 400044
3College of Bioinformation,University of Posts and Telecommunications, Chongqing 400065
Abstract Chiral separation of Citalopram(CIT) was performed by capillary zone electrophoresis(CZE) using maltose as chiral additive. The effect of the concentration of electrophoretic running buffer, its pH, concentration of maltose, and the applied running voltage were investigated. The optimized conditions were obtained with 20 kV as running voltage, and a running buffer of 40%(m/m)maltose in 0.08 mol/L phosphate(pH 50). Good resolution of citalopram enantiomers was achieved and the Rs was 2.3 under optimal conditions. The quantitative analysis of citalopram was performed. The linear range of concentration of R(-)CIT to their peak areas was 0.05~4.00 g/L. The limit of detection of two enantiomers were 0.0453 g/L and 0.0473 g/L respectively. The correlation coefficient was more than 0.9978. The interaction between CIT and maltose was studied by fluorescence spectra and the mechanism of the enantioseparation was also discussed. It was proved that the chiral recognition ability of maltose is related to the concentration of maltose. Maltose molecules begin to aggregate to form hydrophobic cavities, when the concentration of maltose exceeds a critical concentration. The enantioselectivity is attributed to the stereo recognition of the cavities formed by aggregating maltose molecules. ......
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