Enantiomeric separation of beta-blockers by HPLC using (R)-1-naphthylglycine and 3,5-dinitrobenzoic acid as chiral stationary phase.
Direct liquid chromatographic separations of the enantiomers of metoprolol and bisoprolol have been developed, using (R)-1-naphthylglycine and 3,5-dinitrobenzoic acid as chiral stationary phase (CSP). The separations were achieved in a normal phase system employing a mobile phase containing n-hexane, 1,2-dichloroethane and methanol. Column efficiency was strongly dependent on the composition of the mobile phase. The eluent contents of methanol and of 1,2-dichloroethane were optimized, and so was flow-rate and column temperature. Under the optimal conditions, linear responses for (R)-metoprolol and (S)-metoprolol are obtained in the range of 0.079-1.38 and 0.015-5.80 mg/ml, with detection limits of 0.008 and 0.002 mg/ml, respectively. As for bisoprolol, the linear ranges of (R)-isomer and (S)-isomer are 0.05-1.31 and 0.02-1.00 mg/ml with detection limits of 0.001 and 0.008 mg/ml, respectively. The relative standard deviation (R.S.D.) of each enantiomer did not exceed 0.90%. The method has been successfully applied to the determination of enantiomers in pharmaceuticals.
Zhang
Xianhua
X
Department of Chemistry, Beijing Normal University, Beijing 100875, People's Republic of China.
Ouyang
Jin
J
Baeyens
W R G
WR
Zhai
Suodi
S
Yang
Yiping
Y
Huang
Guangming
G
D000319:Adrenergic beta-Antagonists / Q000032:analysis* / Q000737:chemistry; D000473:Alkanes / Q000032:analysis / Q000737:chemistry; D002851:Chromatography, High Pressure Liquid / Q000379:methods; D005998:Glycine / Q000031:analogs & derivatives* / Q000032:analysis*; D009579:Nitrobenzoates / Q000032:analysis*; D013237:Stereoisomerism
D000319:Adrenergic beta-Antagonists; D000473:Alkanes; D009579:Nitrobenzoates; C026017:3,5-dinitrobenzoic acid; C004544:naphtha; D005998:Glycine