以小孔硅胶为载体的纤维素三醋酸酯手性柱的制备及对映体的分离

 合成了纤维素三醋酸酯，并被涂于小孔硅胶上制备成ＨＰＬＣ手性固定相。三种药物、两种富烯和一种哒嗪对映体在柱子上被分离。其中噻马心安使用１．０ｍｏｌ／ＬＮａＣｌＯ４和９５％乙醇为流动相，其它对映体以９５％～９８％乙醇为流动相。自填柱使用４个月后柱效和选择性没有明显降低。

The Preparation of Chiral Column of Cellulose Triacetate Coated on Small Pore Silica Gel and the Separation of Enantiomers

The cellulose triacetate (CTA) prepared by heterogeneous acetylation and coated on small pore 3-aminopropyl silica gel (10 nm) was used as chiral stationary phase for HPLC (OA column). The racemes of three drugs, two fulvenes and one dazine, were separated on this column. Among these racemes, timolol maleas was separated using 1.0 mol/L NaClO4:95% ethanol = 10:90 as mobile phase. Without NaClO4 in mobile phase, the resolution of timolol maleas can not occur. Ethanols of 95%-98% were used as mobile phase for other racemes. The influence of the content of water in mobile phase on the chiral separation of praziquentelum, the retention time and separation factor (alpha) were reduced with the increase of water content in mobile phase. When the content of water in the mobile phase was 13%, praziquentelum could not be separated. It was found that in the case of samples No. 1 and No. 2, when the substituents R1 and R2 or R'1 and R'2 of fulvenes are 4-methoxybenzoyl and 4-methoxyphenyl, the chiral separations of fulvenes can be obtained. For sample No. 4 when R1 and R2 of fulvenes are 2-methylbenzoyl and 2-methylphenyl or in the case of No. 5, when R1 and R2 are 5-bromo-2-furoyl and 5-bromo-2-furan, the chiral separations of fulvenes can not be achieved. For sample No. 6 and No. 7, when R'1 are 4-chlorobenzoyl and benzoyl or R'2 are 4-chlorophenyl and phenyl, the chiral separation also can not be achieved. The column performance and separation factor were not obviously reduced after used for four months.