β-环糊精硝基衍生物HPLC柱分离手性药物扑尔敏  

Chiral Separation of Chlorpheniramine by HPLC with β-Cyclodextrin Nitro Group Derivative as Stationary Phase

作　　者：沈静茹[1] 韦慧慰[1] 余学红[2] 朱财延[1] 毛康[1] 

机构地区：[1]中南民族大学化学与材料科学学院分析化学国家民委重点实验室,武汉430074 [2]中南民族大学校医院,武汉430074

出　　处：《中南民族大学学报（自然科学版）》2011年第4期32-35,共4页Journal of South-Central University for Nationalities：Natural Science Edition

基　　金：湖北省自然科学基金资助项目(95J60)

摘　　要：以双[-6-氧-(-3-间硝基苯磺酰基-丁二酸-14,单酯)-4-]-β-环糊精键合全多孔硅胶基质为高效液相色谱固定相,以正相和反相模式对药物扑尔敏进行手性分离.考察了流动相中配比、pH值对分离度的影响.结果表明:正相模式最佳条件下分离度Rs=1.37;反相模式最佳条件下分离度Rs=10.58,扑尔敏浓度为0.000～1.367 mg/mL,前后峰峰高与浓度均呈线性关系,线性相关系数r均为0.9985.峰面积与浓度的线性相关系数r均为0.9998.通过精密度试验考察,以峰高为响应信号,相对标准偏差RSD(n=12)为2.90%～3.77%;以峰面积为响应信号RSD(n=12)为1.05%～3.15%.加标浓度与样品浓度相当时,以峰高为响应信号,回收率94.69%～106.93%.研究表明,采取反相分离模式,易实现扑尔敏两异构体的分离.Chiral separation of chlorpheniramine was investigated by HPLC with silica gels bonded his [ 6-oxygen-（3-m- nitrobenzene sulfonyl-amber acid-I, 4uniester-4） ] - β-CD as stationary phase. The effects of organic phase concentration and buffer pH in mobile phase were discussed. The best conditions for the normal phase mode HPLC separation was obtained with resolution R, of 1.37. Under reversed phase（RP） mode separation, the R, of optimum conditions is 10.58. There were good linear relationship within concentration range of chlorpheniramine from 0. 000 to 1. 367 mg/mL in peak area and peak height, linear correlation coefficients all are 0. 9985 and 0. 9998. Precision test： the relative standard deviation RSD （n = 12） is 2.90 % - 3.77 % （ peak height） and 1.05 % -3.15 % （ peak area）. Recovery test： the percent recovery is 94.69 % - 106.93 % （ peak height） when it is the same concentration of the sample and the addition. The experiment result shows that： in RP mode, enantiomers were separated on baseline.

关 键 词：β-环糊精硝基衍生物 高效液相色谱(HPLC)手性固定相 扑尔敏 手性分离 

分 类 号：O636.12[理学—高分子化学]