title: Liquid chromatographic separation and thermodynamic investigation of stereoisomers of darunavir on Chiralpak AD-H column.
abstract: 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°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°C. Apparent thermodynamic parameters ΔH(0)  and ΔS* 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.
authors.affiliation: Analytical Chemistry Division, Indian Institute of Chemical Technology, Tarnaka, Hyderabad, India. rnrao55@yahoo.com
authors.forename: Ramisetti Nageswara
authors.initials: RN
authors.lastname: Rao
authors.forename: Kandukuri Nagesh
authors.initials: KN
authors.lastname: Kumar
authors.forename: Bompelli Sravan
authors.initials: BS
authors.lastname: Kumar
mesh_terms: D000327:Adsorption; D000688:Amylose / Q000031:analogs & derivatives* / Q000737:chemistry; D002853:Chromatography, Liquid / Q000295:instrumentation / Q000379:methods*; D000069454:Darunavir; D048448:Phenylcarbamates / Q000737:chemistry*; D013237:Stereoisomerism; D013449:Sulfonamides / Q000737:chemistry*; D013816:Thermodynamics
chemical_list: D048448:Phenylcarbamates; D013449:Sulfonamides; C080033:Chiralpak AD; D000688:Amylose; D000069454:Darunavir