title: An improved and validated LC method for resolution of bicalutamide enantiomers using amylose tris-(3,5-dimethylphenylcarbamate) as a chiral stationary phase.
abstract: An improved HPLC method for determination of enantiomeric purity of bicalutamide in drugs and pharmaceuticals was developed and validated. Baseline separation with resolution >/=6.0 was achieved within 10 min on Chiralpak AD-H (250 mm x 4.6 mm; particle size 5 microm) column using n-hexane:2-propanol (65:35 v/v) as mobile phase at a flow rate of 1.0 ml/min at 25 degrees C. The detection was made at 270 nm using UV detector while a polarimetric detector connected in series was used for identification of enantiomers. The effects of 2-propanol, ethanol and temperature on enantioselectivity and resolution of enantiomers were evaluated. The method was validated in terms of accuracy, precision and linearity in the range of 10-250 microg/ml and the r(2) was >0.9999. The recoveries were 99.68-100.25% with <1% R.S.D. The limits of detection (LOD) and quantification (LOQ) of enantiomers were (2.4, 3.0 and 7.6, 9.3) x 10(-8)g/ml for (S)-(+)-BCT and (R)-(-)-BCT enantiomers, respectively. The method was found to be suitable for rapid determination of enantiomeric purity of bicalutamide in bulk drugs and pharmaceutical formulations.
authors.affiliation: HPLC/UV Group, Analytical Chemistry Division, Discovery Laboratory, Indian Institute of Chemical Technology, Hyderabad 500007, India. mnrao@iictnet.org
authors.forename: R
authors.initials: R
authors.lastname: Nageswara Rao
authors.forename: A
authors.initials: A
authors.lastname: Narasa Raju
authors.forename: D
authors.initials: D
authors.lastname: Nagaraju
mesh_terms: D000688:Amylose / Q000031:analogs & derivatives; D000813:Anilides / Q000032:analysis* / Q000737:chemistry; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D009570:Nitriles; D048448:Phenylcarbamates; D013237:Stereoisomerism; D013607:Tablets; D013696:Temperature; D014105:Tosyl Compounds
chemical_list: D000813:Anilides; D009570:Nitriles; D048448:Phenylcarbamates; D013607:Tablets; D014105:Tosyl Compounds; C080033:Chiralpak AD; D000688:Amylose; C053541:bicalutamide