Identification and determination of the enantiomers of moprolol and their metabolites in human urine by high-performance liquid chromatography and gas chromatography-mass spectrometry.
A simple and sensitive high-performance liquid chromatographic (HPLC) method using chiral derivatization was developed to screen and determine the enantiomers of moprolol and their metabolites in human urine. The recovery of (+)- and (-)-moprolol from urine was 70.8-81.1% at different concentrations. The coefficients of variation (C.V.) were less than 3.2 and 6.5% for intra- and inter-assays, respectively. Moprolol could be detected in urine up to 24 h after oral administration of a 50-mg dose of moprolol. Unconjugated and conjugated enantiomers of moprolol and their metabolites were analyzed by gas chromatography (GC). A gas chromatographic-mass spectrometric (GC-MS) confirmatory method was established to identify the metabolites of moprolol. The double derivation procedure for moprolol and their metabolites with S-(-)-methyl chloroformate [(-)-MCF] and N-methyl(trimethylsilyl)trifluoroacetamide (MSTFA) gave very good GC-MS properties of the derivatized compounds and provided reliable structural information for their confirmation analysis. This is the first published report on the use of a GC-MS method for the detection of the enantiomers of moprolol and their metabolites in human urine.
Li
F
F
Institut National de la Recherche Scientifique, INRS-Santé, Université du Québec, Pointe-Claire, Canada.
Bi
H
H
Côté
M
M
Cooper
S
S
D000081:Acetamides; D000319:Adrenergic beta-Antagonists / Q000652:urine*; D000328:Adult; D002851:Chromatography, High Pressure Liquid; D005463:Fluoroacetates; D005561:Formates; D008401:Gas Chromatography-Mass Spectrometry; D006801:Humans; D006868:Hydrolysis; D007202:Indicators and Reagents; D008297:Male; D050198:Phenoxypropanolamines; D011412:Propanolamines / Q000652:urine*; D013237:Stereoisomerism; D014297:Trimethylsilyl Compounds
D000081:Acetamides; D000319:Adrenergic beta-Antagonists; D005463:Fluoroacetates; D005561:Formates; D007202:Indicators and Reagents; D050198:Phenoxypropanolamines; D011412:Propanolamines; D014297:Trimethylsilyl Compounds; C059663:menthyl chloroformate; C086665:N-methyl-N-(trimethylsilyl)trifluoroacetamide; C009976:moprolol