Journal of Chromatography. B, Biomedical Applications

No abstract text is available yet for this article.

The pharmacokinetics and metabolism of synthetic 2-hydroxymesocarb and 4-methyl-2-hydroxymesocarb analyzed by HPLC-DAD and thermospray LC-MS were studied in rats. Multistep liquid-liquid extraction (LLE) was used with diethyl ether at pH 7.0. The major metabolites of 2-hydroxymesocarb in both urine and plasma of the rat were the p-hydroxylated derivative of the phenylcarbamoyl group of the parent drug. The metabolites of 4-methyl-2-hydroxymesocarb in urine of rats may be the oxidized forms at the phenylcarbamoyl group of the parent drug...

Pyrovalerone and its hydroxylated metabolite have been identified by gas chromatography-mass spectrometry in rat urine and plasma. A sensitive gas chromatographic method for the quantitative analysis of pyrovalerone in rat urine and plasma is described. The method also permits the quantitative monitoring of the urinary excretion of the drug and its metabolite. Pyrovalerone and its hydroxylated metabolite are detected up to 18 h after a single oral administration to the rat at a dose of 20 mg/kg.

HPLC in the reversed-phase mode is used to assay methylxanthines including theobromine, paraxanthine, theophylline and caffeine in urine. The calibration graphs show good linearity in the concentration range 0-10 micrograms/ml. The limit for accurate quantitation of theophylline was 0.25 microgram/ml. Between 6 and 20% of the parent drug is recovered in urine (0-12 h) after the oral administration of sustained release preparations containing 150 and 250 mg theophylline to four volunteers. Theophylline levels above 0...

A liquid-solid procedure is proposed for sample clean-up and derivatization of amphetamine and methamphetamine in urine samples. The reagent was 1,2-naphthoquinone 4-sulphonate, and a commercial C18 packing cartridge was used. The samples derivatized at room temperature were chromatographed on a 5-microns Hypersil ODS (250 x 4 mm I.D.) with an elution gradient of acetonitrile-water containing propylamine. Under these conditions, the amines were eluted with short retention times. The procedure was used to determine amphetamine, or methamphetamine with its metabolite amphetamine, in spiked urine samples...

More than 25 years of developing doping control methods have led to comprehensive screening and confirmation procedures for stimulants, narcotics and beta-blockers. Much of this work has been initiated and/or improved by the late Prof. Dr. Manfred Donike. The methodological approach covered in this overview was applied to doping control procedures during the XXV Summer Olympics in Barcelona, Spain, in 1992 and the XVII Winter Olympics in Lillehammer, Norway, in 1994. Urine samples are screened through a combination of two analytical methods that are complementary: (a) gas chromatographic analysis of the parent compound and unconjugated metabolites, following single-step sample extraction and detection by a nitrogen-specific detector based on a retention index identification system and (b) gas chromatographic analysis including also conjugated drugs and metabolites after hydrolysis, solid-phase extraction, derivatisation and mass spectrometric detection...

A method has been developed for confirmation of the glycopeptide human chorionic gonadotropin (hCG) in urine. A solid-phase immunoaffinity trapping technique utilizing a monoclonal antibody recognizing both intact hCG and free hCG beta-subunits was developed for the extraction of hCG from urine. Recovery of hCG from a urine matrix was essentially quantitative. The hCG was quantitatively eluted with 6 M guanidine hydrochloride, reductively alkylated with vinylpyridine, and subjected to tryptic digestion. The tryptic digest was analyzed by HPLC-MS...

The misuse of human growth hormone (hGH) in sport is deemed to be unethical and dangerous because of various adverse effects. Thus, it has been added to the International Olympic Committee list of banned substances. Until now, the very low concentration of hGH in the urine made its measurement difficult using classical methodology. Indeed, for routine diagnosis, only plasma measurements were available. However, unlike blood samples, urine is generally provided in abundant quantities and is, at present, the only body fluid allowed to be analysed in sport doping controls...

A hormone, erythropoietin, mainly produced in adult kidneys and fetal livers, acts on bone marrow erythroid progenitor cells to regulate the production of erythrocyte in mammals. As a result, the oxygen carrying capacity of blood increases and the increased oxygen supply raises the cardiac function and physiological working capacity. Erythropoietin is possibly misused by athletes in sports for the purpose of improving performance. Presently there is no discernible and specific method to identify erythropoietin administration for doping control...

A totally automated procedure has been developed for the preparation and analysis of 34 basic and neutral drugs in urine samples using an integrated HP 7686 PrepStation-HP 6890 gas chromatographic system. The automated preparation of the sample consisted of a liquid-liquid extraction of 250 microliters urine at alkaline pH with 100 microliters of methyl tert.-butyl ether. After phase separation the organic solvent was automatically placed in the injector of the gas chromatograph and analysed. High recoveries of extraction were obtained...

The hardware and software facilities for electronic storage, transfer and handling of data is such that multipurpose databases can be made accessible without geographic restriction at low cost. The versatile and flexible underlying structures allow for ease of access and retrieval of data and gives presentation formats fully comparable to printed counterparts. Because of the apparent ease of use and because of the wider distribution of the information, misinterpretation is more likely to occur than in oral or written presentation for more restricted and more culturally homogeneous audiences...

Regression equation modelling was used for the correlation of gas chromatographic relative retention times tRR of anabolic steroids, stimulants and narcotics with their molecular characteristics in order to create a model for the prediction of tRR values of unanalyzed molecules. Predicting chromatographic retention parameters is one of the main goals of the quantitative structure-retention relationships (QSRR) methodology. To be performed, QSRR studies require two tools; a methodology for the extraction of the structural characteristics and a statistical program for the correlation of these characteristics with the chromatographic data...

Four diuretic drugs banned in sport (amiloride, triamterene, bendroflumethiazide and bumetanide) have been separated by capillary zone electrophoresis (CZE) and detected using conventional fluorescence spectrometry. The effect of pH on electrophoretic parameters such as migration time, peak efficiency and peak height is discussed. Complete separation of the four drugs is achieved in less than 8 min at pH 8. No interference due to endogenous urine components is observed and thus direct urine analysis is feasible...

Since the inclusion of diuretics in the list of banned substances in sports in 1988, a large number of screening and confirmation procedures to detect the presence of these substances in urine samples have been developed. In this paper, a review of the analytical methodology described to analyze diuretics is presented. The paper has been focused on the needs of doping control and mainly screening procedures including sample preparation and liquid or gas chromatographic separation have been considered. More relevant papers using capillary zone electrophoresis have been also considered...

Knowledge of the effects of episodic or short-term exercise-stress on endogenous testosterone and luteinizing hormone levels still remains fragmentary and inconclusive. In this study, an approach based on the absolute concentrations of urinary total testosterone (T), luteinizing hormone (LH) and the T/LH concentration ratios, was used to profile short-term exercise-stress responses in healthy drug-free male athletes. Testosterone and luteinizing hormone concentrations were measured using gas chromatography-mass spectrometry (GC-MS) and microparticle enzyme immunoassay (MEIA) techniques, respectively...

The effect of alcohol (1.2 and 2.0 g/kg) on the urinary testosterone-to-epitestosterone (T/E) ratio was studied by two experiments each conducted with four healthy females and males. The intake of 2.0 g/kg of ethanol within 5 h in the evening significantly increased plasma testosterone concentration and ratio of T/E in urine collected next morning in females. The results suggest that alcohol increases the T/E ratio more in females than in males. The effect of high doses of alcohol on urinary T/E ratio must be kept in mind when doping tests are performed during training periods...

The misuse of anabolic androgenic steroids (AAS) in human sports is controlled by gas chromatography-mass spectrometric analysis of urine specimens obtained from athletes. The analysis is improved with modern high-resolution mass spectrometry (HRMS). The detection and identification of metabolites of stanozolol (I) [3'-hydroxystanozolol (II) and 4 beta-hydroxystanozolol (III)] and metandienone (IV) I17 beta-methyl-5 beta-androst-1-ene-3 alpha,17 alpha-diol (V) and 18-nor-17,17-dimethyl-5 beta-androsta-1,13-dien-3 alpha-ol (VI)] with GC-HRMS at 3000 resolution yielded a large increase in the number of positive specimens...

An analytical screening procedure has been developed for the estimation of total androgen conjugates in post-competition urine, using gas chromatography-mass spectrometry with computerized data acquisition and concentration calculation. Rapid acid-catalyzed methanolysis is a key feature of the method, which allows simultaneous cleavage of glucuronides and sulfates. Analytical data generated by this method for testosterone and epitestosterone are in accordance with our previous results obtained by more accurate isotope dilution mass spectrometry...

Furazabol and 16-hydroxyfurazabol represented the most abundant peaks in urinary metabolic profiles for two men obtained by gas chromatography-mass spectrometry (GC-MS) after oral administration of 5 mg furazabol. The excreted amounts of unchanged furazabol were determined and its response in GC-MS was compared with that of the 16-hydroxy metabolite. The maximum excretion rates of these compounds were reached 2-3 h after oral administration. The half-lives of unchanged furazabol for two human subjects, were 1...

Gas chromatography-mass spectrometry (GC-MS) is the method of choice for separation and detection of anabolic steroids in urine. Recently, there have been advances in the areas of gas chromatography columns, tandem mass spectrometry using ion traps, and large volume sample injection that have promise for lowering detection limits and extending the utility of GC-MS for steroid analysis. In this work, a Varian Saturn III GC-MS system has been used in its tandem mass spectrometry mode to detect low picogram levels of model steroids in standard solution and the urine matrix...