Qiao Hong-mei
2013
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Journal
Applied Chemical Industry
Abstract
A high performance liquid chromatography method was established for the enantiomeric separation of important medicine intermediate 2-hydroxy-3-methoxy-3,3-diphenylpropionic acid.Baseline separation of 2-hydroxy-3-methoxy-3,3-diphenylpropionic acid was achieved under normal phase chromatographic mode using the chiral stationary phase.Effects of the types of chiral stationary phase,isopropanol modifier concentration,column temperature and flow rate were investigated.Ultimately,the optimized chromatographic conditions were as follows:the chromatographic column was Chiralpak ID(250 mm×4.6 mm,5 μm),the mobile phase were hexane-isopropanol-trifluoroacetic acid(97 ∶ 3 ∶ 0.1,v/v/v),the flow rate was 1.0 mL/min,the detection wavelength was 220 nm,the column temperature was 25 ℃.Under this condition,the resolution of 2-hydroxy-3-methoxy-3,3-diphenylpropionic acid enantiomer was 2.3.The detection limit and quantity limit of R-impurity were 0.5 μg/mL,1.0 μg/mL,respectively.It was good linear(r=0.999 6) over the range of 1~100 μg/mL.The average recoveries of standard addition of R-impurity were 98.4%~104.5%,and the related standard deviations of peak areas was 1.5%.R-impurity in the three batches of 2-hydroxy-3-methoxy-3,3-diphenylpropionic acid were in line with the requirements.The method using for detection of(S)-2-hydroxy-3-methoxy-3,3-diphenylpropionic acid isomer is simple,rapid and reproducible.