Development and validation of a chiral liquid chromatographic method for the determination of atenolol and metoprolol enantiomers in tablet preparations.
Atenolol (AT) and metoprolol (MT) are predominantly used in the treatment of angina pectoris, certain arrhythmias, systemic hypertension, and several other cardiovascular disorders. Both compounds are produced commercially in the racemic form, although the S-form is responsible for the desired biological effect. This paper describes a simple, rapid, precise, and accurate method for separating the enantiomers of AT and MT. AT isomers are separated by using a Chiralcel OD column (250 x 4.6 mm, 10 microm), hexane-ethanoldiethylamine-acetic acid (60 + 40 + 0.2 + 0.2, v/v/v/v) as the mobile phase, and a flow rate of 1.0 mL/min. MT isomers are separated by using a mobile phase with the same components in the following proportions (40 + 60 + 0.2 + 0.2, v/v/v/v) and a flow rate of 0.8 mL/min. Ultraviolet detection was at 276 nm for both analytes. The coefficients of variation (CVs) and average recoveries (ARs) for the R-enantiomers in samples A, B, C, D, and E were 1.15 and 101.06%, 0.74 and 99.25%, 1.05 and 102.57%, 0.84 and 101.57%, and 0.86 and 98.62%, respectively. The CVs and ARs for the S-enantiomers in samples A, B, C, D, and E were 1.33 and 98.87%, 0.99 and 100.76%, 1.17 and 101.69%, 1.26 and 100.39%, and 1.40 and 99.39%, respectively. The standard curves of R-AT, S-AT, R-MT, and S-MT showed good linearity over the concentration range studied with correlation coefficients of 0.9991, 0.998, 0.9988, and 0.999, respectively.
Singh
A K
AK
University of São Paulo, Department of Pharmacy, Faculty of Pharmaceutical Sciences, SP, Brazil.
Kedor-Hackmann
E R
ER
Santoro
M I
MI
D000319:Adrenergic beta-Antagonists / Q000008:administration & dosage / Q000032:analysis* / Q000737:chemistry / Q000592:standards; D001262:Atenolol / Q000008:administration & dosage / Q000032:analysis* / Q000737:chemistry / Q000592:standards; D002219:Carbamates; D002482:Cellulose / Q000031:analogs & derivatives; D002853:Chromatography, Liquid / Q000379:methods*; D006801:Humans; D008790:Metoprolol / Q000008:administration & dosage / Q000032:analysis* / Q000737:chemistry / Q000592:standards; D048448:Phenylcarbamates; D012015:Reference Standards; D013237:Stereoisomerism; D013607:Tablets
D000319:Adrenergic beta-Antagonists; D002219:Carbamates; D048448:Phenylcarbamates; D013607:Tablets; C065943:cellulose tris-3,5-dimethylphenyl-carbamate; D001262:Atenolol; D002482:Cellulose; D008790:Metoprolol