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0.0473 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.
Chiral separation of Citalopram(CIT) was performed by capillary zone electrophoresis(CZE) using maltose as ehiral additive. The effeet of the eoneentration of eleetrophoretie running buffer, its pH, eoneentration 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 5.0). Good resolution of eitalopram enantiomers was aehieved and the R, was 2.3 under optimal eonditions. The quantitative analysis of eitalopram was performed. The linear range of eoneentration of R-( - )-CIT to their peak areas was 0.05 ~ 4.00 g/L. The limit of deteetion of two enantiomers were 0. 0453 g/L and 0. 0473 g/L respeetively. The eorrelation eoeffieient was above 0. 9978. The interaetion between CIT and maltose was studied by fluoreseenee speetra and the meehanism of the enantioseparation was also discussed. It was proved that the ehiral reeognition ability of maltose is related to the concentration of maltose. Maltose moleeules begin to aggregate to form hydrophobie cavities, when the concentration of maltose exceeds a critical concentration. The enantioseleetivity is attributed to the stereo recognition of the cavities formed by aggregating maltose molecules.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2006年第10期1384-1388,共5页
Chinese Journal of Analytical Chemistry
基金
国家自然科学基金(No.20375051
20175038)
教育部青年教师奖(No.教人司[2002]123)资助项目
关键词
麦芽糖
西酞普兰
手性分离
毛细管电泳
拆分机理
Citalopram, maltose, chiral separation, capillary eleetrophoresis, enantioseparation mechanism