Quantitation and test of enantiomeric purity of the L-ketohexoses by liquid chromatography with dual refractive index and laser-based chiroptical detection

被引:8
|
作者
Shaw, CJ
Huang, AH
Zhang, XN
机构
[1] Johnson & Johnson Pharmaceut Res & Dev, LLC Analyt Dev Drug Evaluat, Raritan, NJ 08869 USA
[2] Chem Dev Drug Evaluat, Raritan, NJ USA
关键词
chiroptical detection; reaction monitoring; ketohexoses;
D O I
10.1016/S0021-9673(02)01413-9
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
Experimental data for the synthetic methods of preparation of the L-ketohexoses have been lacking an analytical method for monitoring the chemical or enzymatic reactions described. Dual refractive index and laser-based chiroptical detection provides an ideal method for following the reactions, since the refractive index detector quantifies the amount of analyte, while the ratio of optical rotation to refractive index response allows the enantiomer mole fraction to be determined. Sulfonated polystyrenedivinylbenzene resin in the Ca form as the stationary phase with H2O at 80 degreesC as the eluent gives base-line separation of sorbose, fructose, tagatose, and psicose. Dependent on the complexity of the reaction mixture, analysis times range from 20 to 60 min. (C) 2002 Elsevier Science B.V. All rights reserved.
引用
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页码:439 / 443
页数:5
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