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Analytical findings of unannounced doping control in body builders in Flanders during 1988-1993 are reported. In some federations between 38 and 58% of the controlled athletes were found positive during this period. The results show that there was no fall in drug abuse over this period and steroids were taken even by body builders associated with an organisation against the use of anabolic steroids. In 1988 and 1989 popular anabolic steroids were nandrolone and testosterone. From 1990 on, a wide range of mostly injectable steroids including nandrolone, metenolone, drostanolone and testosterone were administered. Polydrug abuse including several anabolics in combination with stimulants and diuretics was also widespread. The beta agonist clenbuterol was detected in several urine samples taken in 1991, one year before its appearance in other sports.

A method is described for the GC-NPD determination of urinary codeine and morphine after derivatization with trifluoroacetic anhydride. The lower limit for accurate quantitative determination was 0.05 microgram ml-1. After the oral administration of Bisolvon Griblettes corresponding to 30 mg codeine phosphate to seven subjects maximum codeine concentrations were obtained after 1-2 h and codeine remained detectable generally 24 h post dosing. The mean maximum level was 5.1 +/- 2.8 micrograms ml-1 found after enzymatic hydrolysis with Suc Helix pomatia juice (SHP). Based on these and previous results (mean 6.3 +/- 3.4 micrograms ml-1) a threshold level for codeine of 16 micrograms ml-1 is proposed. Significant differences were noticed between urinary codeine concentrations found after enzymatic hydrolysis with SHP, beta-glucuronidase from Patella vulgata and acid hydrolysis, respectively. Generally, highest values were obtained after SHP, while beta-glucuronidase and especially acid hydrolysis resulted in much lower levels. No morphine could be detected after acid hydrolysis. Concerning doping analysis, in particular the uniformity of methods and interpretation of the results, it is recommended that the hydrolysis method should be specified in the rules of those sporting federations allowing codeine and/or morphine.

A high-performance liquid chromatographic method to measure urinary indomethacin levels is described. In 0.5 ml urine, 1 micrograms/ml of indomethacin could be detected. Alkaline hydrolysis of urine resulted in the decomposition of indomethacin. When two suppositories of Indocid corresponding to 200 mg indomethacin were administered rectally to four horses the drug was rapidly absorbed and remained detectable in urine from 1 to 12 h. The excretion rate peaked after 2-3 h while the maximal concentration ranged from 18.5 to 80.6 micrograms/ml. Only 8 to 16% of the indomethacin dose was eliminated in urine after 12 h. A fraction of the dose was excreted as the glucuronide conjugate.

A high pressure liquid chromatographic (HPLC) method for measuring the theobromine content in cocoa husks, pelleted food and horse urine is described. Starting with 2 ml of urine, concentrations of 500 ng/ml could easily be detected. When feed containing 38.4 mg of theobromine was given twice daily to horses for 2 1/2 days, two days were needed after the last intake before the theobromine concentrations fell below the threshold value of 2 micrograms/ml. The time at which the peak excretion rate occurred varied from 2 to 12 h after the last administration, while the excretion rate seemed to be dependent on the urinary flow. Theobromine could not be detected in plasma after administration in this way.

A capillary GC method with nitrogen-specific detection is described for the analysis of codeine and morphine in urine. Both drugs were determined after enzymatic hydrolysis of the urine. Morphine was derivatized with trifluoroacetic anhydride. For 5-ml samples of urine, the lower detection limits for accurate quantitation were 50 ng ml-1 and 100 ng ml-1 for morphine and codeine, respectively. Both codeine and morphine were already detectable in urine 1 h after the intake of the analgesic preparation Perdolan. Codeine excretion and concentration peaked 2 h after administration of a dose. The percentage of the dose excreted as codeine was 3.0-6.2%. Administration of the antitussive preparation Bisolvon Griblettes resulted in detectable codeine and morphine levels for at least one day; 5.6-9% was excreted as total codeine over 24 h, the conjugated metabolite morphine accounting for 1.7-7.4% of the dose. Nearly the same amounts of codeine and morphine were excreted after administration of the antitussive syrup Bronchodine. The maximum excretion rate of codeine occurred after 1 h. Generally codeine and morphine remained detectable for 12 h. The results of these administration studies are discussed in relation to the codeine and morphine threshold levels recently introduced by the International Cyclist Union.

A sensitive method for the quantitative determination of the respiratory stimulant dimefline in 5 ml urine using capillary gas chromatography with nitrogen specific detection is presented. After the oral administration of a therapeutical amount of 16 mg dimefline to five subjects only 0.26 +/- 0.16% of the dose is excreted as the conjugated drug in 24 h. The maximum excretion rate occurred 3 h after dosing, the peak concentration being 154 +/- 60 ng ml-1. The influence of diuretics taken 2 h after the administration of dimefline was studied in three subjects. From these results it appeared that the use of acetazolamide and hydrochlorthiazide in order to circumvent a positive dimefline doping case is questionable. Due to the potent diuretic effect of furosemide, the intake of this diuretic could result in a suppression of the dimefline concentration below the detection limit of 10 ng ml-1.

The urinary caffeine content was compared between a control group and 775 cyclists checked for doping during the 1982 season. The data for sportsmen demonstrate that the (mis)use of caffeine is more pronounced in both professional and amateur classes than in the younger categories (debutant and junior). Caffeine was also monitored during a 60-h period in the urine of several coffee drinkers. Based on all results, a "maximum level of caffeine" of 15 micrograms X ml-1 in urine for sporting competitions is proposed.

The urinary excretion of caffeine in humans was followed over a period of 36 h after the oral administration of ANIMINE, a formulation containing caffeine-alpha-naphthylacetate. The excretion of caffeine was not as markedly affected by the urinary pH as was found with stimulant amines. Excretion peaks were obtained 1-2 h after the ingestion and the total amount of unchanged caffeine excreted during 12 h varied from 0.57 to 1.51 per cent. The ingestion of the diuretics acetazolamide or furosemide 2 h after caffeine resulted in a urine-flow dependent and consequently increased caffeine excretion during 2-4 h post-diuretic. This increase paralleled the increase in urine volume resulting in no meaningful differences in caffeine concentration compared to normal conditions.

The urinary excretion of phentermine in humans was followed over a period of several days after the oral administration of two formulations. The intake of phentermine in a capsule generally resulted in an excretion peak 4 h after the administration followed by a second peak 12 or 24 h post dosing. The total amount excreted during 72 h varied from 62.7 to 84.8%. Concerning the administration of Ionamine 15, a sustained release formulation, the maximal excretion rate was spread over 3-9 h, while more than 85% of phentermine were excreted after 72 h. The excretion was affected by urinary pH. The intake of acetazolamide shortly after phentermine resulted in a decrease of the phentermine excretion during one day and in one subject in a suppression below the detection limit 4 h post dosing. The administration of furosemide or bumetanide produced only a diluting effect during 2 h.