Article ID Journal Published Year Pages File Type
1225091 Journal of Pharmaceutical and Biomedical Analysis 2006 5 Pages PDF
Abstract

A high-performance liquid chromatographic method for chiral separation of ketoprofen racemate was developed. (R)- and (S)-ketoprofen enantiomers were separated on a Hypersil BDS C8 column (150 mm × 4.6 mm i.d., 5 μm) at 25 °C, using acetonitrile–triethylamine acetate (TEAA) buffer (pH 5.2, 20 mM) (35:65, v/v) containing 2.0 mM norvancomycin as the mobile phase. Effects of norvancomycin concentration, content of acetonitrile and TEAA buffer pH on the enantioseparation were investigated. The method was validated for linearity, repeatability, limits of detection (LOD) and limits of quantification (LOQ). Calibration curves (r2 = 0.999) were constructed in the range of 2.01–200.8 μg ml−1 for (S)-ketoprofen and 2.04–152.4 μg ml−1 for (R)-ketoprofen, respectively. Repeatability (n = 5) showed less than 2% relative standard deviation (R.S.D.). LOD and LOQ for the two enantiomers were found to be 0.20 and 0.78 ng for (S)-ketoprofen, 0.20 and 0.86 ng for (R)-ketoprofen, respectively. Norvancomycin and vancomycin as chiral mobile phase additives (CMPAs) in the chiral separation showed similar abilities of enantioseparation. However, to obtain the optimum enantioseparation, a lower concentration of norvancomycin than that of vancomycin is required.

Related Topics
Physical Sciences and Engineering Chemistry Analytical Chemistry
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