Cyclodextrin-modified monolithic columns for resolving dansyl amino acid enantiomers and positional isomers by capillary electrochromatography

被引:61
作者
Chen, ZL
Ozawa, H
Uchiyama, K
Hobo, T
机构
[1] NTT Corp, Microsyst Integrat Labs, Ubiquitous Interface Lab, Biosensing Res Grp, Kanagawa 2430198, Japan
[2] Tokyo Metropolitan Univ, Grad Sch Engn, Dept Appl Chem, Tokyo 158, Japan
关键词
capillary electrochromatography; chiral separation; cyclodextrin; dansyl amino acids; monolithic column; positional isomers; sol-gel process;
D O I
10.1002/elps.200305403
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
We describe beta- and gamma-cyclodextrins (beta- and gamma-CD)-modified monolithic columns prepared by sol-gel process and chemical modifications. The monolithic silica column was fabricated inside a fused-silica capillary with 100 gm inner diameter by sol-gel process. The monolithic silica matrix was chemically modified chiral selectors of beta- or gamma-CDs with a spacer of 3-glycidoxypropyltrimethoxysilane by on-column reactions. gamma-CD-modified monolithic column has successfully been applied for the separation of dansyl amino acid enantiomers. beta-CD-modified monolithic column has been used for the separation of the positional isomers of o-, m-, and p-cresols and the enantioseparation of racemates of benzoin and several dansyl amino acids by capillary electrochromatography, respectively. For the separation of neutral positional isomers, a positive electric field was applied. However, for the separation of negatively charged analytes, a negative electric field was applied at the inlet of column. The separation efficiency of 5.0 x 10(4) theoretical plates/m for dansyl-L-threonine was obtained at electric field strength of -300 V/cm in the mobile phase of 50 mm 2-(N-morpholino)ethanesulfonic acid (MES)-Tris/methanol (70/30) buffer at pH 7.0. L-Enantiomers were eluted as the first peak. Scanning electron micrograph showed that monolithic columns have the morphology of continuous skeleton and large through-pores.
引用
收藏
页码:2550 / 2558
页数:9
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