[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.
Huang
M
M
Department of Chemistry, Experimental Center, Shandong University, Jinan, 250100.
Sun
J
J
Li
G
G
Yang
G
G
Du
A
A
Gao
Z
Z
Wang
J
J
D002482:Cellulose; D002851:Chromatography, High Pressure Liquid / Q000379:methods; D007536:Isomerism; D011223:Praziquantel / Q000302:isolation & purification*; D020034:Silicone Gels
D020034:Silicone Gels; D011223:Praziquantel; D002482:Cellulose