Quantitation and test of enantiomeric purity of the L-ketohexoses by liquid chromatography with dual refractive index and laser-based chiroptical detection.
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 degrees C 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.
Shaw
Charles J
CJ
Johnson & Johnson Pharmaceutical Research and Development, L.L.C.-Analytical Development/Drug Evaluation, 1000 Route 202, Raritan, NJ 08869, USA. cshaw@prius.jnj.com
Huang
Aihua
A
Zhang
Xini
X
D002138:Calibration; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D006601:Hexoses / Q000032:analysis* / Q000302:isolation & purification; D012031:Refractometry; D013237:Stereoisomerism
D006601:Hexoses