Development of liquid chromatographic enantiomer separation methods and validation for the estimation of (R)-enantiomer in eslicarbazepine acetate.
Chiral separation method development was carried out for eslicarbazepine acetate and its (R)-enantiomer on diverse chiral stationary phases. Better chiral selectivity was observed on cellulose tris-(3,5-dichlorophenylcarbamate) immobilized column (Chiralpak IC-3). Under polar organic mode (POM), with 100% acetonitrile as mobile phase and 0.5 ml/min flow, a resolution close to three was achieved. With normal phase (NP) mobile phase consisting dichloromethane:ethanol (90:10, v/v) and 1.0 ml/min flow, a resolution close to six was achieved. Detection was done by UV at 220 and 240 nm respectively. Both the methods were found to be robust and were validated with respect to robustness, precision, linearity, limit of detection, limit of quantification and accuracy. The proposed methods are suitable for the accurate estimation of (R)-enantiomer in bulk drug samples up to 0.1% when a 1mg/ml analyte test solution is chromatographed.
Mone
Mahesh Kumar
MK
Drug Discovery Facility, Advinus Therapeutics, Quantum Towers, Plot-9, Rajiv Gandhi Infotech Park, Phase-I, Hinjewadi, Pune 411 057, India. mahesh.mone@advinus.com
Chandrasekhar
K B
KB
D000097:Acetonitriles / Q000737:chemistry; D002623:Chemistry Techniques, Analytical; D002626:Chemistry, Pharmaceutical / Q000379:methods; D002713:Chlorine / Q000737:chemistry; D002845:Chromatography / Q000379:methods; D002853:Chromatography, Liquid / Q000379:methods*; D003984:Dibenzazepines / Q000737:chemistry*; D000431:Ethanol / Q000737:chemistry; D008752:Methylene Chloride / Q000737:chemistry; D009930:Organic Chemicals; D015203:Reproducibility of Results; D012997:Solvents / Q000737:chemistry; D013237:Stereoisomerism; D013696:Temperature
D000097:Acetonitriles; D003984:Dibenzazepines; D009930:Organic Chemicals; D012997:Solvents; D000431:Ethanol; D002713:Chlorine; D008752:Methylene Chloride; C416835:eslicarbazepine acetate; C428744:10,11-dihydro-10-hydroxy-5H-dibenz(b,f)azepine-5-carboxamide; C032159:acetonitrile