ABSTRACT
A sensitive and specific quantitative assay for the determination of dextromoramide in human fluids and tissues is described. Dextromoramide and an internal standard, SKF 525 A, are isolated by a basic extraction and back-extraction process. The final extract is separated on a 25-m capillary column B.P. 1 and drugs are detected by selected ion monitoring at m/z 100 and m/z 86 for dextromoramide and the internal standard, respectively. The minimum detectable quantities are 0.5 and 0.3 ng/mL, for dextromoramide in plasma and urine, respectively. Coefficients of variation for within-run data were less than 6%.
Subject(s)
Dextromoramide/metabolism , Dextromoramide/blood , Dextromoramide/urine , Gas Chromatography-Mass Spectrometry/methods , Humans , Reproducibility of ResultsABSTRACT
Dextromoramide (Palfium) was given by intravenous injection to a Thoroughbred horse at a dosage of 20 mg and urine was collected 2, 4, 6 and 8 h after drug administration. Enzymatic hydrolysis of the urine followed by solvent extraction gave a residue which was back-extracted into 0.1 M sulphuric acid. After basification to pH 9 and solvent extraction, the resulting residue was submitted to gas chromatographic-mass spectrometric analysis. Both electron-impact and ammonia chemical-ionization mass spectra were recorded and, based on the observed fragmentation patterns, the principal metabolites in horse urine were shown to be 2,2-diphenyl-3-methyl-4-morpholinobutyramide (compound 2) and the product of hydroxylation of one phenyl ring in dextromoramide (compound 3), respectively. The electron-impact mass spectra of compounds 2 and 3, and of their derivatisation products from oncolumn methylation in the gas chromatograph, are reported.
Subject(s)
Dextromoramide/urine , Doping in Sports , Horses/urine , Animals , Chemical Phenomena , Chemistry , Gas Chromatography-Mass SpectrometryABSTRACT
A rapid method is described for the extraction and identification of a number of basis drugs and their metabolites in urine. Gas chromatography is used as the primary source of identification, and characteristic chromatograms and retention times for a number of drug metabolites are outlined.
