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摘 要:以乙醇-水为流动相,用纤维素-三(苯甲酰酯)(CTB)作为手性固定相对外消旋体托品酸进行了高效液相色谱手性分离。考察了不同比例的乙醇-水流动相、不同流速以及用不同醇类酯化对托品酸酯在手性色谱柱上的色谱行为。实验表明,流动相中水的比例、流速以及酯化所用醇类均对托品酸酯衍生物分离有很大影响。以流动相为乙醇-水(95∶5),流速为0.1 mL/min的色谱体系,使托品酸乙酯在CTB柱上得到基线分离。对托品酸乙酯在CTB手性固定相上反相手性识别机理进行了讨论。
Abstract:Reverse-phase
chromatography was employed for chiral separation of tropine acid enantiomers on
the cellulose tribenzoate (CTB) chiral stationary phases coated on a
small-particle spherical silica support in an eluant system consisting of a
mixture of alcohol and water. The influence of water proportion in mobile phase,
flow rate of chromatography, derivatives of various kinds of alcohol were
systematically examined. The result showed that the mobile phase strength, flow
rate of chromatography and the structure of chiral compounds were dominant
factors to retention and resolution of the analytes. Meanwhile, the steric
effects of alcohol seemed to be a certain factor. We observed that a good
separation of enantiomers of tropine acid ethyl ester derivatives could be
obtained under the conditions of chromatography, which was mobile phase:
alcohol-water (95∶5);
flow rate: 0.1 mL/min; stationary phase: cellulose tribenzoate.
Keywords:Enantiomeric separation, chiral stationary phase, tropine acid, high performance liquid chromatography |
作者单位:严建伟(浙江大学化学系,杭州
310027) 施介华(浙江大学化学系,杭州 310027) 徐秀珠(浙江大学化学系,杭州 310027) 参考文献: [1]Allenmark S G.
Chromatographic Enantioseparation, Methods and Applications. Eillis
Horwood, Chirchester, 1988
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原载于《分析化学》2001 Vol.29 No.1 P.53-56
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