Heart-cut achiral-chiral LC-LC method development using factorial design: application to the chiral separation of ketoprofen
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- 作者：Miguel Peñín-Ibáñez ; María Jesús Santos-Delgado…
- 关键词：Two ; dimensional LC ; LC direct chiral liquid chromatography ; Enantiomer determination ; Ketoprofen ; Pharmaceuticals
- 刊名：Analytical and Bioanalytical Chemistry
- 出版年：2017
- 出版时间：February 2017
- 年：2017
- 卷：409
- 期：4
- 页码：1135-1144
- 全文大小：
- 刊物类别：Chemistry and Materials Science
- 刊物主题：Analytical Chemistry; Biochemistry, general; Laboratory Medicine; Characterization and Evaluation of Materials; Food Science; Monitoring/Environmental Analysis;
- 出版者：Springer Berlin Heidelberg
- ISSN：1618-2650
- 卷排序：409
文摘
A two-dimensional achiral-chiral LC-LC method in heart-cut mode for ketoprofen and its enantiomeric fraction determination was proposed. A C8 column was used in the first dimension, and the chiral column was an α1-acid glycoprotein. The mobile phase of the chiral system was optimized by a factorial design. The effect of temperature on retention and on enantiomeric resolution was studied. Particular attention was paid to mobile phase compatibility for the two columns and to transferring time, using ketoprofen standards. The R-(−) and S-(+)-ketoprofen retention times were 9 and 11 min, respectively; the resolution was higher than 1.1 and enantiomeric fraction close to 0.5. The method was applied to capsules and gels containing ketoprofen. Factorial design was also used to establish the best conditions for gel sample preparation. Recoveries were 84 and 105 % for capsules and gels, respectively.