β氨基酸__(期刊论文)

β氨基酸对映体在键合型配体交换色谱固定相上的分离

http://www.100md.com 《分析化学》 2006年第5期

β氨基酸,,β氨基酸，对映体分离，手性固定相，配体交换色谱，硅胶基质,摘要,关键词,1引言,2实验部分,3结果与讨论,References

     摘要

    制备了以Lα氨基酸为手性配体和球型多孔硅胶为基质的键合型手性配体交换色谱固定相，用于β氨基酸对映体的拆分。考察了硅胶基质、配体、流动相pH值、中心金属离子浓度和流动相阴离子等因素对5种β苯丙氨酸对映体分离的影响，由此确立最佳色谱分离条件为：以 BaseLine 硅胶为基质键合L羟脯氨酸的手性固定相， 5.0 mmol/L和pH 4.6 的CuSO4溶液为流动相，紫外检测波长为254 nm。在此条件下5种β氨基酸对映体均可在35 min内得到分离，分离因子在1.49～1.77之间。结果表明：该方法操作简便，成本低廉，可用于β氨基酸对映体的分离和分析。

     关键词 β氨基酸，对映体分离，手性固定相，配体交换色谱，硅胶基质

    Enantiomeric Separation of βAmino Acids on Chemically Bonded Ligand Exchange Stationary Phases

    Li Ruifen, Wan Qianhong

    (College of Pharmaceutical Science and Technology, Tianjin University, Tianjin 300072)

    Abstract βAmino acid enantiomers are important pharmaceutical intermediates and generally obtained by resolution of synthetic racemates. A simple resolution method based on chiral ligand exchange chromatography with Lαamino acid chemically bonded to spherical silica as the stationary phase and aqueous solution containing cupric ions as the mobile phase is described. With βphenylalanine and its analogous as model compounds, the effects of the silica support, chiral ligand, mobile phase composition and pH on enantiomeric separation of βamino acids were examined. Optimum separation conditions such as chiral stationary phase, Lhydroxyproline bonded silica (BaseLine Sil, 5 μm); mobile phase, aqueous solution of 5 mmol/L CuSO4, pH 4.6; flow rate of 1 mL/min; detection wavelength 254 nm; column temperature and ambient were obtained. A baseline separation of the enantiomers was obtained for all 5 βamino acids tested (βphenylalanine, 3hydroxyβphenylalanine, 3fluoroβphenylalanine, 3hydroxy 4methylβphenylalanine, 3,4dimethoxyβphenylalanine) with elution times less than 35 min and separation factors in the range of 1.49-1.77. Compared with similar chiral stationary phases prepared by coating silica with Lhydroxyproline derivatives, the chemically bonded phases described in the present work are advantageous in that they allow the use of organic solvents without worrying about the leach out of the chiral ligand and thus prolong the columns service life. ......

百拇医药网 http://www.100md.com/html/DirDu/2006/06/20/01/47/21.htm

您现在查看是摘要页，全文长 10371 字符。