| With the rapid development of life science and chiral technology, more and more people pay attention to the development of chiral drugs with a single enantiomer. In the numerous chiral separation technology of optical isomers, HPLC chiral stationary phase(CSP) method has achieved a breakthrough development, and occupied a dominant position in the chiral separation filed. The CSPs based on the β-cyclodextrin derivatives have been recognized as the one of most powerful for both analytical and preparative separations, and had widely application prospect.4-Chlorophenycarbamate β-CD derivative was synthesized using 4-chlorophenyl isoyanate as derivative reagent. Two novel β-CD-CSPs were prepared(β-CD-CSP1 and β-CD-CSP2) by coating 4-chlorophenylcarbamate β-CD derivative on aminopropyl silica and silica gel, respectively. A novel bonded 4-chlorophenylcarbamate β-CD CSP3 were prepared using γ-(triethoxysilyl)propyl isoyanate as the bonding reagents, silica gel as support, 4-chlorophenyl isoyanate as derivative reagent. The chiral recognition abilities of the obtained three β-CD-4-chlorophenylcarbamate-based CSPs were evaluated through enantioseparation of the thirteen racemates under the HPLC normal-phase mode. The results show that the three CSPs exhibit chiral recognition ability for the thirteen enantiomers. the results showed that the chiral recognition ability of coated silica gel β-CD-CSP2 is better to the coated aminopropyl silica gel β-CD-CSP1, and β-CD-CSP1 than the same quality bonded type β-CD-CSP3.Using γ-(triethoxysilyl)propyl isoyanate as the bonding reagents, a novel bonded hp-β-CD-(phenylcarbamate)-CSP4 were prepared and evaluated through the enantiomeric separation of the racemates. The hp-β-CD-CSP4 show a high chiral resolution abilities, especially for compounds 1, 7 and 11.Finally, nitrophenol positional isomers were separated on four self-made chiral columns. The four novel β-CD-CSPs had good recognition ability for nitrophenol positional isomers. |
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