制备了β-环糊精-6-单取代氨乙基氨丙基三甲氧基硅烷手性单体(β-CD siloxane),以该手性单体和1,2-双(三乙氧基硅基)乙烷(BTEE)为硅源,十六烷基三甲基溴化铵(CTAB)为模板,采用水热合成法直接制得孔道中含有环糊精的手性介孔材料.再对该产物进行苯基异氰酸酯化得到杂合β-环糊精的有机-无机介孔分离材料(β-CD PMOs).在反相-HPLC及正相-HPLC条件下,分别考察该填料柱对常见含氮碱性药物对映体的拆分效果.结果表明,不管在反相或正相分离模式下,采用常见的流动相在pH =4.15条件实现了11个碱性药物的手性分离,手性选择因子(α)最高可达2.42.孔道中直接杂合β-环糊精的手性固定相制备方法简便、快速和成本低,进一步优化成孔条件后有一定应用前景.
参考文献
[1] | CHEN Liren.HPLC Chiral Separations[M].Beijing:Science Press of China,2006:105-136 (in Chinese).陈立仁.液相色谱手性分离[M].北京:科学出版社,2006:105-136. |
[2] | Zhong Q Q,He L F,Beesley T E,et al. Development of Dinitrophenylated Cyclodextrin Derivatives for Enhanced Enantiomeric Separations by High-performance Liquid Chromatography[J].J Chromatogr A,2006,1115 (1/2):19-45. |
[3] | State Food and Drug Administration Information Center[EB/OL].[2009-03-23].http://www.cpi.gov.cn/cpi/jsp/preview_1.jsp? TID =20100323140954005591717(in Chinese).国家食品药品监督管理局信息中心.2009世界畅销药排行榜:立普妥夺冠[EB/OL].[2009-03-23].http://www.cpi.gov.cn/cpi/jsp/preview_1.jsp? TID=20100323140954005591717. |
[4] | YOU Qidong,LIN Guoqiang.Chiral Drugs Research & Application[M].Beijing:Chemical Industry Press,2003:241 (in Chinese).尤启冬,林国强.手性药品研究与应用[M].北京:化学工业出版社,2003:241. |
[5] | Hoffmann F,Cornelius M,Morell J,et al.Periodic Mesoporous Organosilicas (PMOs):Past,Present,and Future[J].J Nanosci Nanotechnol,2006,6(2):265-288. |
[6] | Zhu G R,Jiang D M,Yang Q H,et al.Trans-(1R,2R)-Diamino-cyclohexane Functionalized Mesoporous Organosilica Spheres as Chiral Stationary Phase[J].J Chrornatogr A,2007,1149:219-227. |
[7] | Zhu G R,Zhong H,Yang Q H,et al.Chrial Mesoporous Organosilica Spheres:Synthesis and Chiral Separation Capacity[J].Microporous Mesoporous Mater,2008,116:36-43. |
[8] | Guo Z M,Jin Y,Liang T,et al.Synthesis,Chromatographic Evaluation and Hydrophilic Interaction/Reversed-phase Mixedmode Behavior of a “Click beta-Cyclodextrin” Stationary Phase[J].J Chromatogr A,2009,1216(2):257-263. |
[9] | Han X X,Yao T L,Liu Y,et al.Separation of Chiral Furan Derivatives by Liquid Chromatography Using Cyclodextrin-based Chiral Stationary Phases[J].J Chromatogr A,2005,1063 (1/2):111-120. |
[10] | Berkecz R,Ilisz I,Ivanov-Sztojkov A,et al.HPLC Enantioseparation of 1-(alpha-Aminobenzyl)-2-naphthol and 2-(alphaAminobenzyl)-1-naphthol Analogs on a beta-Cyclodextrin-based Chiral Stationary Phase[J].Chromatographia,2007,65(5/6):337-341. |
[11] | Wang Y,Young D J,Tan T T Y,et al.“ Click” Immobilized Perphenylcarbamated and Permethylated β-Cyclodextrin Stationary Phases for Chiral High-performance Liquid Chromatography Application[J].J Chromatogr A,2010,1217:5103-5108. |
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%