β-环糊精毛细管电色谱法拆分和测定马尼地平、尼卡地平对映体  

Preparation of β-Cyclodextrin Capillary Column for Enantioseparation and Determination of Nicardipine and Manidipine by Capillary Electrochromatography

作　　者：聂桂珍[1] 李来生[1] 程彪平[1] 周仁丹[1] 张宏福[1] 

机构地区：[1]南昌大学分析测试中心,南昌330047

出　　处：《应用化学》2014年第12期1472-1480,共9页Chinese Journal of Applied Chemistry

基　　金：国家自然科学基金(21165012);江西省自然科学基金(2010GZH0089);江西省教育厅科技项目(GJJ11274)资助~~

摘　　要：采用溶胶-凝胶法制备对硝基苯氨基甲酸酯化β-环糊精毛细管开管柱（NCDP）,建立了分别拆分钙离子阻滞剂盐酸马尼地平和盐酸尼卡地平对映体的毛细管电色谱方法。采用红外光谱、扫描电子显微镜对其进行了必要的结构及形态表征。在极性有机模式下,考察了有机溶剂的组成及含量、三乙胺和冰醋酸的含量、运行电压、温度对手性分离的影响。优化的条件为：温度20℃,检测波长236 nm,压力进样（3.448 k Pa×3 s）,盐酸马尼地平在乙腈-甲醇-三乙胺-冰醋酸（体积比57∶43∶0.05∶0.07）流动相中,运行电压25 k V时,分离度（RS）为1.39;盐酸尼卡地平在乙腈-甲醇-三乙胺-冰醋酸（体积比55∶45∶0.05∶0.08）流动相中,运行电压20 k V时,分离度为1.30。上述两种地平对映体保留时间和峰面积的RSD分别小于1.2%和5.6%（n=5）,表明所制备的电色谱柱有良好的稳定性。盐酸马尼地平的拆分时间〈5 min,盐酸尼卡地平的拆分时间〈7 min,有利于建立快速测定其对映体含量的方法。盐酸马尼地平和盐酸尼卡地平在5.2~125 mg/L范围内线性关系良好（r≥0.9969）,检测限分别为1.8和2.3 mg/L（S/N=3）。初步将NCDP柱用于盐酸马尼地平片和盐酸尼卡地平缓释胶囊中对映体含量的测定。The separation and determination methods of calcium antagonists manidipine hydrochloride and nicardipine hydrochloride enantiomers were developed by open-tubular capillary electrochromatography （ CEC）, respectively. A new capillary column with p-nitrophenylcarbamation fl-eyclodextrin was prepared by sol-gel method. The sol-gel modified with cyelodextrin derivative was characterized by infrared spectroscopy （IR） and scanning electron microscopy（SEM）. In polar organic mode, the effect of the volume fraction and concentration of added triethylamine and glacial acetic acid, the content of organic solvents, the operating voltage, and temperature on the resolution （Rs） were investigated. The optimized conditions were at 20℃, detection wavelength at 236 nm, and injection pressure at 3.448 kPa x 3 s. The compositions of mobile phases were V （ MeOH ） ： V （ ACN ） ： V （TEA） ： V （ HOAc ） = 57 ： 43 ： 0. 05： 0. 07 for manidipine hydrochloride and V（MeOH） ： V（ ACN ） ： V（ TEA ） ： V（ HOAe ） = 55： 45： 0. 05 ： 0. 08 for nicardipine hydrochloride. The resolution （Rs ） of manidipine hydrochloride was 1.39 at 25 kV. The resolution （RS） of nieardipine hydrochloride was 1.30 at 20 kV. The RSDs of retention time and peak area were less than 1.2% and 5.6% （ n = 5 ） for the drugs, respectively. It was indicated that new column has stable electrochromatography performance. The single run time were less than 5 min for manidipine hydroehloride and less than 7 min for nicardipine hydrochloride. Good linearity were observed in the concentration range of 5.2 ~ 125.0 mg/L with correlation coefficients 0. 9969 or more for both drug enantiomers. The limit of detection values were 1.8 mg/L for manidipine and 2. 3 mg/L for nicardipine, respectively. The nitrophenyl carbamated β-cyelodextrin phase （NCDP） column were preliminarily used for determinations of manidipine hydrochloride and nicardipine hydrochloride tablet and capsule. Keywords opened-tubular capillar

关 键 词：开管毛细管电色谱法 溶胶-凝胶法 Β-环糊精衍生物 手性分离 盐酸尼卡地平和盐酸马尼地平 

分 类 号：O657[理学—分析化学]