Journal
JOURNAL OF SEPARATION SCIENCE
Volume 35, Issue 20, Pages 2671-2677Publisher
WILEY-V C H VERLAG GMBH
DOI: 10.1002/jssc.201200410
Keywords
Antiretrovirals; Chiralpak AD-H; Darunavir; Stereoisomers; Van't Hoff plots
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Funding
- Council of Scientific and Industrial Research (CSIR), New Delhi, India
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Liquid chromatographic separation of stereoisomers of darunavir on Chiralpak AD-H, a column containing the stationary phase coated with amylose tris(3,5-dimethylphenylcarbamate) as a chiral selector, was studied under normal-phase conditions at different temperatures between 20 and 50 degrees C. The effect of quality and quantity of different polar organic modifiers viz: methanol, ethanol, 1-propanol, and 2-propanol in the mobile phase as well as column temperature on retention, separation, and resolution was investigated and optimized. The optimum separation was accomplished using a mobile phase composed of n-hexane/ethanol/diethyl amine (80:20:0.1 v/v/v) at 40 degrees C. Apparent thermodynamic parameters ?H0 and ?S* were derived from the Van't Hoff plots (lnk' versus 1/T) and used to explain the strength of interactions between the stereoisomers and amylose tris(3,5-dimethylphenylcarbamate) coated chiral stationary phase.
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