采用毛细管电泳技术,以α-环糊精、β-环糊精和β-环糊精聚合物为手性选择剂,对4种不对称合成物3-(二乙基氨基)-1-苯基-1-丙醇(a)、1-苯基-3-(1-哌啶)-1-丙醇(b)、3-吗啉-1-对甲苯基-1-丙醇(c)和1-(4-氯苯基)-3-吗啉-1-丙醇(d)的消旋体和光学活性异构体进行了手性分离.结果发现,使用20 kV的分离电压.以浓度为30 g/L的β-环糊精聚合物的80 mmol/L三羟甲基氨基甲烷缓冲溶液(pH=3.2)为背景电解质溶液,4种化合物在40 min内均可得到基线分离.根据对映异构体峰面积和保留时间的比值确定了4种不对称化合物的光学纯度.测定的RSD均不大于1.5%.
参考文献
| [1] | Kreidler D,Czesla H,Schurig V.A Mixed Stationary Phase Containing Two Versatile Cyclodextrin-Based Selectors for the Simultaneous Gas Chromatographic Enantioseparation of Racemic Alkanes and Racemic a-Amino Acid Derivatives[J].J Chromatogr 5,2008,875(1):208-216. |
| [2] | ZHU Zhijia,WANG Qianqian,KANG Jingwu.Enantioseparation with a Chiral Micro-HPLC System[J].Acta Chim Sin,2008,66(15):1845-1849(in Chinese).朱智甲,王倩倩,康经武.手性微柱高效液相色谱用于对映体的分离[J].化学学报,2008,66(15):1845-1849. |
| [3] | Ward T J,Ward K D.Chiral Separations:Fundamental Review 2010[J].Anal Chem,2010,82(12):4712-4722. |
| [4] | Simo C,Garcia-Canas V,Cifuentes A.Chiral CE-MS[J].Eleclrophoresis,2010,31(9):1442-1456. |
| [5] | Chen B,Du Y X,Li P.Investigation of Enantiomeric Separation of Basic Drugs by Capillary Electrophoresis Using Clindamycin Phosphate as a Novel Chiral Selector[J].Electrophoresis,2009,30(15):2747-2754. |
| [6] | LIU Dan,WEI Ruixia,XIE Tianyao.Simple and Efficient Enantioseparation of Ofloxacin by Capillary Electrophoresis with Contactless Conductivity Detedction Using Binary Chiral Selectors[J].Chinese J Anal Chem,2009,37 (11):1687-1690(in Chinese).刘丹,魏瑞霞,谢天尧.毛细管电泳/非接触式电导法分离检测氧氟沙星对映体[J].分析化学,2009,37(11):1687-1690. |
| [7] | Renard E,Deratani A,Volet G,et al.Preparation and Characterization of Water Soluble High Molecular Weight β-Cyclodextrin-Epichlorohydrin Polymers[J].Eur Polym,1997,33(1):49-57. |
| [8] | Ma L Y,Gu J L,Han J H,et al.Capillary Electrophoresis Enantioseparation of Drugs Using β-Cyclodextrin Polymer:Intramolecular Synergistic Effect[J].Electrophoresis,1999,20(9):1900-1903. |
上一张
下一张
上一张
下一张
计量
- 下载量()
- 访问量()
文章评分
- 您的评分：
-
10%
-
20%
-
30%
-
40%
-
50%