Prevalence of caffeine use in elite athletes following its removal from the World Anti-Doping Agency list of banned substances

2011 ◽  
Vol 36 (4) ◽  
pp. 555-561 ◽  
Author(s):  
Juan Del Coso ◽  
Gloria Muñoz ◽  
Jesús Muñoz-Guerra
Keyword(s):  
Mass Spectrometry ◽  
Limit Of Detection ◽  
Elite Athletes ◽  
Urine Samples ◽  
Gas Chromatography Mass Spectrometry ◽  
Alkaline Extraction ◽  
Caffeine Concentration ◽  
The World ◽  
World Anti Doping Agency ◽  
Males And Females

The aim of this investigation was to determine the use of caffeine by athletes after its removal from the World Anti-Doping Agency list. For this purpose, we measured the caffeine concentration in 20 686 urine samples obtained for doping control from 2004 to 2008. We utilized only urine samples obtained after official national and international competitions. Urine caffeine concentration was determined using alkaline extraction followed by gas chromatography–mass spectrometry. The limit of detection (LOD) was set at 0.1 µg·mL–1. The percentage of urine samples below the LOD was 26.2%; the remaining 73.8% of the urine samples contained caffeine. Most urine samples (67.3%) had urinary caffeine concentrations below 5 µg·mL–1. Only 0.6% of urine samples exceeded the former threshold for caffeine doping (12 µg·mL–1). Triathlon (3.3 ± 2.2 µg·mL–1), cycling (2.6 ± 2.0 µg·mL–1), and rowing (1.9 ± 1.4 µg·mL–1) were the sports with the highest levels of urine caffeine concentration; gymnastics was the sport with the lowest urine caffeine concentration (0.5 ± 0.4 µg·mL–1). Older competitors (>30 y) had higher levels of caffeine in their urine than younger competitors (<20 y; p < 0.05); there were no differences between males and females. In conclusion, 3 out of 4 athletes had consumed caffeine before or during sports competition. Nevertheless, only a small proportion of these competitors (0.6%) had a urine caffeine concentration higher than 12 µg·mL–1. Endurance sports were the disciplines showing the highest urine caffeine excretion after competition.

scholarly journals Urine Caffeine Concentration in Doping Control Samples from 2004 to 2015

Nutrients ◽  
2019 ◽  
Vol 11 (2) ◽  
pp. 286 ◽  
Author(s):  
Millán Aguilar-Navarro ◽  
Gloria Muñoz ◽  
Juan Salinero ◽  
Jesús Muñoz-Guerra ◽  
María Fernández-Álvarez ◽  
...  
Keyword(s):  
Monitoring Program ◽  
Doping Control ◽  
Urine Samples ◽  
Ergogenic Effect ◽  
Caffeine Concentration ◽  
In Doping ◽  
The World ◽  
World Anti Doping Agency ◽  
Individual Sports ◽  
Control Samples

The ergogenic effect of caffeine is well-established, but the extent of its consumption in sport is unknown at the present. The use of caffeine was considered “prohibited” until 2004, but this stimulant was moved from the List of Prohibited Substances to the Monitoring Program of the World Anti-Doping Agency to control its use by monitoring urinary caffeine concentration after competition. However, there is no updated information about the change in the use of caffeine as the result of its inclusion in the Monitoring Program. The aim of this study was to describe the changes in urine caffeine concentration from 2004 to 2015. A total of 7488 urine samples obtained in official competitions held in Spain and corresponding to athletes competing in Olympic sports (2788 in 2004, 2543 in 2008, and 2157 in 2015) were analyzed for urine caffeine concentration. The percentage of samples with detectable caffeine (i.e., >0.1 μg/mL) increased from ~70.1%, in 2004–2008 to 75.7% in 2015. The median urine caffeine concentration in 2015 (0.85 μg/mL) was higher when compared to the median value obtained in 2004 (0.70 μg/mL; p < 0.05) and in 2008 (0.70 μg/mL; p < 0.05). The urine caffeine concentration significantly increased from 2004 to 2015 in aquatics, athletics, boxing, judo, football, weightlifting, and rowing (p < 0.05). However, the sports with the highest urine caffeine concentration in 2015 were cycling, athletics, and rowing. In summary, the concentration of caffeine in the urine samples obtained after competition in Olympic sports in Spain increased from 2004 to 2015, particularly in some disciplines. These data indicate that the use of caffeine has slightly increased since its removal from the list of banned substances, but urine caffeine concentrations suggest that the use of caffeine is moderate in most sport specialties. Athletes of individual sports or athletes of sports with an aerobic-like nature are more prone to using caffeine in competition.

Determination of Tuaminoheptane in Doping Control Urine Samples

2007 ◽  
Vol 13 (3) ◽  
pp. 213-221 ◽  
Author(s):  
Mario Thevis ◽  
Gerd Sigmund ◽  
Anja Koch ◽  
Wilhelm Schänzer
Keyword(s):  
Drug Testing ◽  
Limit Of Detection ◽  
Urine Samples ◽  
Fragment Ions ◽  
Liquid Liquid Extraction ◽  
In Doping ◽  
Aldehydes And Ketones ◽  
Characteristic Fragment ◽  
World Anti Doping Agency

Since January 2007, the list of prohibited substances established by the World Anti-Doping Agency includes the sympathomimetic compound tuaminoheptane (1-methyl-hexylamine, 2-heptylamine). Primarily used as a nasal decongestant drug it has been considered relevant for sports drug testing due to its stimulating properties. A confirmatory gas chromatographic-mass spectrometric procedure was developed including liquid–liquid extraction and imine formation of tuaminoheptane employing various aldehydes and ketones such as formaldehyde, acetaldehyde, benzaldehyde and acetone. Extraction and derivatisation conditions were optimised for utmost efficiency and characteristic fragment ions obtained after electron ionisation allowed for a sensitive and selective analytical assay, which was validated with regard to recovery (50%), lower limit of detection (20 ng mL−1) as well as interday- and intraday precision (< 15%). The applicability to authentic urine samples was demonstrated using administration study specimens obtained from two male persons using Rhinofluimucil (tuaminoheptane hemisulfate) for intranasal application. The administered drug was detected up to 46h after repeated topical instillation of a total of approximately 3 mg.

Recyclable amitraz-ethylene vinyl acetate strips used for beehives treatment against Varroa destructor

2017 ◽  
Vol 50 (5) ◽  
pp. 391-402 ◽  
Author(s):  
Federico Karp ◽  
Julio A Luna ◽  
Luciano N Mengatto
Keyword(s):  
Mass Spectrometry ◽  
Differential Scanning Calorimetry ◽  
Vinyl Acetate ◽  
Varroa Destructor ◽  
Ethylene Vinyl Acetate ◽  
Gas Chromatography Mass Spectrometry ◽  
Recycling Process ◽  
Scanning Calorimetry ◽  
The World ◽  
Natural Pollination

In this work, a new recyclable ethylene-vinyl acetate (EVA)-based strip impregnated with amitraz (AMZ) was prepared, characterized, and evaluated for the treatment of Apis mellifera against Varroa destructor. Bees are important for natural pollination, honey, and related goods production. Varroa destructor is currently considered one of the major pests and important efforts around the world are focused on methods for varroasis treatment. The procedure of strips preparation presented in this work consisted of two steps: impregnation and molding of impregnated pellets. Differential scanning calorimetry and gas chromatography–mass spectrometry analyses confirmed that AMZ molecule resisted the impregnation and molding conditions. The strips were sufficiently strong to resist destruction by the bees. The final infestation was lower in the hives treated with AMZ/EVA strips than in those treated with commercial strips. In order to check the possibility of recycling, strips were cut into little pieces and were subjected to total AMZ extraction. Finally, the fragments were exposed to re-impregnation and molding. The strips prepared after the recycling process presented the same shape and AMZ load than fresh strips.

Simultaneous Determination of Alachlor, Metolachlor, Atrazine, and Simazine in Water and Soil by Isotope Dilution Gas Chromatography/Mass Spectrometry

1989 ◽  
Vol 72 (2) ◽  
pp. 349-354 ◽  
Author(s):  
Lee Q Huang
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Simultaneous Determination ◽  
Isotope Dilution ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Gas Chromatography Mass Spectrometry ◽  
Selected Ion Monitoring ◽  
Chromatography Mass Spectrometry

Abstract A multiresidue method was developed for the simultaneous determination of low parts per billion (ppb) concentrations of the herbicides alachlor, metolachlor, atrazine, and simazine in water and soil using isotope dilution gas chromatography/mass spectrometry (GC/MS). Known amounts of 15N,13C-alachlor and 2H5-atrazine were added to each sample as internal standards. The samples were then prepared by a solid phase extraction with no further cleanup. A high resolution GC/low resolution MS system with data acquisition in selected ion monitoring mode was used to quantitate herbicides in the extract. The limit of detection was 0.05 ppb for water and 0.5 ppb for soil. Accuracy greater than 80% and precision better than 4% was demonstrated with spiked samples.

Determination of Phytosterols in Butter Samples by Using Capillary Column Gas Chromatography

1987 ◽  
Vol 70 (5) ◽  
pp. 912-915 ◽  
Author(s):  
Randall L Smith ◽  
Darryl M Sullivan ◽  
Earl F Richter
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Retention Time ◽  
Capillary Column ◽  
Limit Of Detection ◽  
Packed Column ◽  
Gas Chromatography Mass Spectrometry ◽  
Positive Bias ◽  
Capillary Column Gas Chromatography

Abstract A positive bias in the gas chromatographic (GC) analysis of butter for β-sitosterol was discovered when attempting to confirm values by gas chromatography/mass spectrometry (GC/MS). The source of the problem was traced to an interfering material that was not effectively separated by packed column GC. Because capillary columns are known to provide superior separation, they were substituted for packed columns in the assay, and instrument parameters were modified accordingly. A compound with a similar retention time, identified by GC/MS as lanosterol, was separated from β-sitosterol by the capillary column. The capillary column technique was applied to over 300 butter samples. The results indicate that the method can accurately quantitate β-sitosterol in butter with no known interferences. The limit of detection for this method is 1 mg/100 g. Recoveries at a level of 3 mg/100 g averaged 98% with a coefficient of variation of 3.45%

scholarly journals Optimization and Comparison of Information-Dependent Acquisition (IDA) to Sequential Window Acquisition of All Theoretical Fragment Ion Spectra (SWATH) for High-Resolution Mass Spectrometry in Clinical Toxicology

2019 ◽  
Vol 65 (7) ◽  
pp. 862-870 ◽  
Author(s):  
Jeffrey D Whitman ◽  
Kara L Lynch
Keyword(s):  
Mass Spectrometry ◽  
High Resolution ◽  
Data Acquisition ◽  
High Resolution Mass Spectrometry ◽  
Limit Of Detection ◽  
Clinical Toxicology ◽  
Urine Samples ◽  
Analytical Sensitivity ◽  
High Resolution Mass ◽  
Resolution Mass

Abstract BACKGROUND Untargeted data acquisition on high-resolution mass spectrometers (HRMSs) has been used in clinical toxicology for screening and identifying unknown compounds in patient samples. A common modality for untargeted HRMS data acquisition is information-dependent acquisition (IDA), which analyzes the most abundant small molecules within an acquisition cycle. This process can potentially lead to false negatives of clinically relevant compounds at low concentrations. Sequential window acquisition of all theoretical fragment ion spectra (SWATH) has emerged as a method of unbiased, untargeted HRMS data acquisition in which no spectral data are lost. SWATH has yet to be optimized and assessed for use in clinical toxicology. METHOD We developed a variable-window SWATH method (vSWATH) and compared it to IDA by limit of detection studies in drug-supplemented urine (81 compounds) and against a retrospective cohort of 50 clinical urine samples characterized by LC-MS/MS. RESULTS vSWATH had a lower limit of detection than IDA for 33 (41%) drugs and metabolites added into urine samples. Both IDA and vSWATH were equivalent in discovering compounds from clinical urine samples and confirmed 26 additional compounds not previously discovered by targeted LC-MS/MS. Lastly, the unbiased acquisition of spectra in vSWATH allowed for identification of 5 low-abundance compounds missed by IDA. CONCLUSIONS This vSWATH method for clinical toxicology demonstrated equivalent analytical sensitivity and specificity for untargeted drug screening and identification in urine samples. vSWATH provided the additional benefit of collecting all tandem mass spectrometry spectra in a sample, which could be useful in discovering low-abundance compounds not discovered by IDA.

THC and CBD concentrations in blood, oral fluid and urine following a single and repeated administration of “light cannabis”

2020 ◽  
Vol 58 (5) ◽  
pp. 682-689 ◽  
Author(s):  
Roberta Pacifici ◽  
Simona Pichini ◽  
Manuela Pellegrini ◽  
Maria Concetta Rotolo ◽  
Raffaele Giorgetti ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Oral Fluid ◽  
Repeated Administration ◽  
Urine Samples ◽  
Gas Chromatography Mass Spectrometry ◽  
Sample Collection ◽  
Valuable Alternative ◽  
The Mean ◽  
Single And Repeated Administration

AbstractBackground“Light cannabis” is a product legally sold in Europe with Δ9-tetrahydrocannabinol (THC) concentration lower than 0.2% and variable cannabidiol (CBD) content. We studied THC and CBD excretion profiles in blood, oral fluid (OF) and urine after smoking one or four light cannabis cigarettes.MethodsBlood, OF and urine samples were obtained from six healthy light cannabis consumers after smoking one 1 g cigarette containing 0.16% THC and 5.8% CBD and from six others after smoking four 1 g cigarettes within 4 h. Sample collection began 0.5 and 4.5 h after smoking one or four cigarettes, respectively. Cannabinoid concentrations were quantified by gas chromatography-mass spectrometry (GC-MS).ResultsAt the first collection, the highest THC and CBD concentrations occurred in blood (THC 7.0–10.8 ng/mL; CBD 30.2–56.1 ng/mL) and OF (THC 5.1–15.5 ng/mL; CBD 14.2–28.1 ng/mL); similar results occurred 0.5 h after the last of four cigarettes in blood (THC 14.1–18.2 ng/mL, and CBD 25.6–45.4 ng/mL) and OF (THC 11.2–24.3 ng/mL; CBD 14.4–37.0 ng/mL). The mean OF to blood ratio ranged from 0.6 to 1.2 after one and 0.6 to 1.9 after four light cannabis cigarettes. THC/CBD ratios in blood and OF were never greater than 2. Urinary 11-nor-9-carboxy-THC concentrations peaked 8 h after one and four cigarettes.ConclusionsOF was a valuable alternative to blood in monitoring consumption of light cannabis. Blood and OF THC/CBD concentration ratios, never exceeded 2, possibly providing a useful biomarker to identify light cannabis vs illegal higher THC cannabis use, where THC/CBD ratios are generally greater than 10.

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