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Drostanolone is one of the most frequently detected anabolic androgenic steroids in doping control analysis. Here, we studied drostanolone urinary metabolic profiles using liquid chromatography quadruple time of flight mass spectrometry (LC-QTOF-MS) in full scan and targeted MS/MS modes with accurate mass measurement. The drug was administered to one healthy male volunteer and liquid-liquid extraction along with direct-injection were used to analyze urine samples. Chromatographic peaks for potential metabolites were identified with the theoretical [M-H](-) as a target ion in a full scan experiment and actual deprotonated ions were analyzed in targeted MS/MS mode. Eleven metabolites including five new sulfates, five glucuronide conjugates, and one free metabolite were confirmed for drostanolone. Due to the absence of useful fragment ions to illustrate the steroid ring structure of drostanolone phase II metabolites, gas chromatography mass spectrometry (GC-MS) was used to obtain structural details of the trimethylsilylated phase I metabolite released after enzymatic hydrolysis and a potential structure was proposed using a combined MS approach. Metabolite detection times were recorded and S4 (2-methyl-5-androstan-17-one-6-ol-3-sulfate) and G1 (2-methyl-5-androstan-17-one-3-glucuronide) were thought to be new potential biomarkers for drostanolone misuse which can be detected up to 24days by liquid-liquid extraction and 7days by direct-injection analysis after intramuscular injection. S4 and G1 were also detected in two drostanolone-positive routine urine samples.


PubMed | Edge Hill University, Shanghai Institute of Sport Science, Yun Nan Institute of Sport Science, Gui Zhou Institute of Sport Science and 15 more.
Type: Journal Article | Journal: The lancet. Diabetes & endocrinology | Year: 2016

Obesity, physical inactivity, and reduced physical fitness contribute to the rising burden of chronic diseases in China. We investigated these factors in Chinese adults over a 14-year period (2000-14) using data from randomised national surveys.We did four national surveys in 2000, 2005, 2010, and 2014 among Chinese adults aged 20-59 years. We used BMI to assess underweight (<185 kg/m(2)), overweight (230 to <275 kg/m(2)), and obesity (275 kg/m(2)). Central obesity was defined as a waist circumference greater than 90 cm in men and greater than 85 cm in women. We assessed leisure-time physical activity (LTPA) by whether or not participants had completed the recommended minimum 150 min of moderate or 75 min of vigorous exercise per week. Indices for assessment of physical fitness were forced vital capacity, resting heart rate, hand grip strength, sit and reach distance, and time standing on one leg.151656 (78%) of 193440 adults responded to the survey in 2000, 163386 (84%) in 2005, 154931 (80%) in 2010, and 146703 (76%) in 2014. The prevalence of obesity increased from 86% in 2000, to 103% in 2005, 122% in 2010, and 129% in 2014 (estimated increase 032% per year, 95% CI 030-033; p<00001). The equivalent estimates were 374%, 392%, 407%, and 412% for overweight (estimated increase 027% per year, 95% CI 025-030; p<00001) and 139%, 183%, 221%, and 249% for central obesity (estimated increase 078% per year, 076-080; p<00001). The prevalence of overweight, obesity, and central obesity increased with age (all p<00001) and was higher in men than in women (all p<00001). We noted a simultaneous decrease in the prevalence of underweight (estimated decrease of 006% per year, 95% CI 004-007; p<00001). The proportion of adults meeting the minimum LTPA recommendation increased over time (172% in 2000, 181% in 2005, and 228% in 2014), with the estimated prevalence change per year being 033% (95% CI 024-042; p<00001) for underweight people, 050% (047-053; p<00001) for normal-weight people, 037% (034-040; p<00001) for overweight people, and 006% (000-013; p=0044) for obese people. We noted deteriorations over time in all measures of physical fitness in normal-weight adults (all p<00001), apart from resting heart rate (p=069).Despite increased participation in LTPA, we noted increases in overweight or obesity and a decrease in physical fitness in Chinese adults. Continued nationwide interventions are needed to promote physical activity and other healthy lifestyle behaviours in China.National Physical Fitness Surveillance Center and Ministry of Science and Technology of the Peoples Republic of China.


PubMed | China Anti Doping Agency and Peking Union Medical College
Type: Journal Article | Journal: International journal of molecular sciences | Year: 2016

In this study, methasterone urinary metabolic profiles were investigated by liquid chromatography quadrupole time of flight mass spectrometry (LC-QTOF-MS) in full scan and targeted MS/MS modes with accurate mass measurement. A healthy male volunteer was asked to take the drug and liquid-liquid extraction was employed to process urine samples. Chromatographic peaks for potential metabolites were hunted out with the theoretical [M - H](-) as a target ion in a full scan experiment and actual deprotonated ions were studied in targeted MS/MS experiment. Fifteen metabolites including two new sulfates (S1 and S2), three glucuronide conjugates (G2, G6 and G7), and three free metabolites (M2, M4 and M6) were detected for methasterone. Three metabolites involving G4, G5 and M5 were obtained for the first time in human urine samples. Owing to the absence of helpful fragments to elucidate the steroid ring structure of methasterone phase II metabolites, gas chromatography mass spectrometry (GC-MS) was employed to obtain structural information of the trimethylsilylated phase I metabolite released after enzymatic hydrolysis and the potential structure was inferred using a combined MS method. Metabolite detection times were also analyzed and G2 (18-nor-17-hydroxymethyl-2, 17-dimethyl-androst-13-en-3-ol--O-glucuronide) was thought to be new potential biomarker for methasterone misuse which can be detected up to 10 days.


Botre F.,University of Rome La Sapienza | Botre F.,Sportiva | Wu M.,China Anti Doping Agency | Boghosian T.,World Anti Doping Agency
Bioanalysis | Year: 2012

This article outlines the process of preparation of an anti-doping laboratory in view of the activities to be performed on the occasion of the Olympic Games, focusing in particular on the accreditation requirements of the World Anti-Doping Agency (WADA) and ISO/IEC 17025, as well as on the additional obligations required by the International Olympic Committee, which is the testing authority responsible for the anti-doping activities at the Olympics. Due to the elevated workload expected on the occasion of the Olympic Games, the designated anti-doping laboratory needs to increase its analytical capacity (samples processed/time) and capability by increasing the laboratorys resources in terms of space, instrumentation and personnel. Two representative cases, one related to the Winter Olympic Games (Torino 2006) and one related to the Summer Olympic Games (Beijing 2008), are presented in detail, in order to discuss the main aspects of compliance with both the WADA and ISO/IEC 17025 accreditation requirements. © 2012 Future Science Ltd.


Wang J.,China Anti Doping Agency | Wu M.,China Anti Doping Agency | Liu X.,China Anti Doping Agency | Xu Y.,China Anti Doping Agency
Steroids | Year: 2011

Androstenedione (4-androstene-3,17-dione) is banned by the World Anti-Doping Agency (WADA) as an endogenous steroid. The official method to confirm androstenedione abuse is isotope ratio mass spectrometry (IRMS). According to the guidance published by WADA, atypical steroid profiles are required to trigger IRMS analysis. However, in some situations, steroid profile parameters are not effective enough to suspect the misuse of endogenous steroids. The aim of this study was to investigate the atypical steroid profile induced by androstenedione administration and the detection of androstenedione doping using IRMS. Ingestion of androstenedione resulted in changes in urinary steroid profile, including increased concentrations of androsterone (An), etiocholanolone (Etio), 5α-androstane-3α,17β-diol (5α-diol), and 5β-androstane-3α,17β-diol (5β-diol) in all of the subjects. Nevertheless, the testosterone/epitestosterone (T/E) ratio was elevated only in some of the subjects. The rapid increases in the concentrations of An and Etio, as well as in T/E ratio for some subjects could provide indicators for initiating IRMS analysis only for a short time period, 2-22 h post-administration. However, IRMS could provide positive determinations for up to 55 h post-administration. This study demonstrated that, 5β-diol concentration or Etio/An ratio could be utilized as useful indicators for initiating IRMS analysis during 2-36 h post-administration. Lastly, Etio, with slower clearance, could be more effectively used than An for the confirmation of androstenedione doping using IRMS. © 2011 Elsevier Inc. All rights reserved.


Wang J.,China Anti Doping Agency | Yang R.,Beijing Sport University | Yang W.,Beijing University of Chinese Medicine | Liu X.,China Anti Doping Agency | Xing Y.,China Anti Doping Agency
Analytical and Bioanalytical Chemistry | Year: 2014

Progesterone (PROG) is a naturally occurring progestagen, which has been used to prevent preterm birth, control persistent anovulatory bleeding, and treat premenstrual syndrome in clinical practices. Studies on the metabolism of PROG have demonstrated that PROG is the precursor of other steroids such as 5β-pregnane-3α,20α-diol (PD), testosterone (T), and 17-hydroxyprogesterone. PD is the most commonly used endogenous reference compound (ERC) in the isotope ratio mass spectrometry (IRMS) analysis for doping control. It is expected that the PROG administration could affect the carbon isotope ratios (13C/12C, expressed as δ 13C-value) of PD and T metabolites, and lead to the false-negative or false-positive results in doping test. The influences of oral and intramuscular administration of PROG on the urinary steroid profile and carbon isotope ratios of steroids were investigated in this study. It was demonstrated that the urine concentrations and the δ 13C-values of PD were affected obviously. The depleted δ 13C-values of PD could be used to suggest PROG administration. Using PD as ERC may result in the distorted evaluation for suspicious urine sample in IRMS analysis when PROG is ingested. The 5α-androst-16-en-3α-ol and 11β-hydroxyandrosterone could be used as the alternative ERCs in case of PROG administration. The carbon isotope ratios of androsterone (An) and etiocholanolone (Etio), two T metabolites, remained unchanged throughout the excretion study, which suggested that the δ values of An and Etio could still be used as the urinary markers of T administration even when PROG was administrated. © 2014 Springer-Verlag Berlin Heidelberg.


He Y.,National Institutes for Food and Drug Control | Wang J.,China Anti Doping Agency | Liu X.,China Anti Doping Agency | Xu Y.,China Anti Doping Agency | He Z.,China Anti Doping Agency
Steroids | Year: 2013

Musk is widely used as a traditional drug in Asia for the treatment of stroke, tumour, and cardiopathy with an oral dosage of 0.03-0.1 g per day. Because of the potential anabolic effect, musk preparations have been included in the list of medical products containing prohibited substances employed for doping. The application of musk pod formulation was regarded as the reason of some adverse analytical findings in the 2011 FIFA Women's World Cup. In order to investigate the influence of musk administration on the doping test, we executed a chemical analysis and excretion study. The gas chromatography/mass spectrometry (GC-MS) analysis demonstrated the diversity of steroid concentrations in musk samples. Furthermore, the δ13C-values of steroids from wild deer musk showed more depleted than those of domestic deer musk by gas chromatography/combustion/isotope ratio mass spectrometry (GC/C/IRMS) analysis. Because the steroids from some musk had δ13C-values in the range of naturally produced steroids in human body, the possible abuse of this kind of musk is very hard to be detected by isotope ratio mass spectrometry (IRMS) in doping control. Musk grains from wild and domestic deer were administrated for the excretion study respectively. Spot urine samples were collected from two male volunteers before and after 100 mg musk grains administration. The profiles and carbon isotope ratios of urinary steroids were determined by GC-MS and GC/C/IRMS. The ingestion of either wild or domestic deer musk did not lead to the adverse analytical finding of doping control in the single dosage of 100 mg. © 2013 Elsevier Inc. All rights reserved.


Lu J.,China Anti Doping Agency | Wang X.,China Anti Doping Agency | Xu Y.,China Anti Doping Agency | Dong Y.,China Anti Doping Agency | And 4 more authors.
Analyst | Year: 2011

The metabolism and excretion of toremifene were investigated in one healthy male volunteer after a single oral administration of 120 mg toremifene citrate. Different liquid chromatographic/tandem mass spectrometric (LC/MS/MS) scanning techniques were carried out for the characterization of the metabolites in human urine for doping control purposes. The potential characteristic fragmentation pathways of toremifene and its major metabolites were presented. An approach for the metabolism study of toremifene and its analogs by liquid chromatography-tandem mass spectrometry was established. Five different LC/MS/MS scanning methods based on precursor ion scan (precursor ion scan of m/z 72.2, 58.2, 44.2, 45.2, 88.2 relative to five metabolic pathways) in positive ion mode were assessed to recognize the metabolites. Based on product ion scan and precursor ion scan techniques, the metabolites were proposed to be identified as 4-hydroxy-toremifene (m/z 422.4), 4′-hydroxy-toremifene (m/z 422.4), α-hydroxy-toremifene (m/z 422.4), 3,4-dihydroxy-toremifene (m/z 404.2), toremifene acid (m/z 402.2), 3-hydroxy-4-methoxy-toremifene (m/z 456.2), dihydroxy-dehydro-toremifene (m/z 440.2), 3,4-dihydroxy-toremifene (m/z 438.2), N-demethyl-4-hydroxy-toremifene (m/z 408.3), N-demethyl-3-hydroxy-4-methoxy- toremifene (m/z 438.3). In addition, a new metabolite with a protonated molecule at m/z 390.3 was detected in all urine samples. The compound was identified by LC/MS/MS as N-demethyl-4,4′-dihydroxy-tamoxifene. The results indicated that 3,4-dihydroxy-toremifene (m/z 404.2), toremifene acid (m/z 402.2) and N-demethyl-4,4′-dihydroxy-tamoxifene (m/z 390.3) were major metabolites in human urine. © 2011 The Royal Society of Chemistry.


PubMed | Beijing Sport University and China Anti Doping Agency
Type: | Journal: Steroids | Year: 2016

In this study, metenolone metabolic profiles were investigated. Metenolone was administered to one healthy male volunteer. Liquid-liquid extraction and direct-injection were applied to processing urine samples. Urinary extracts were analyzed by liquid chromatography quadrupole time-of-flight mass spectrometry (LC-QTOFMS) using full scan and product ion scan with accurate mass measurement for the first time. Due to the lack of useful fragment ion for structural elucidation, GC-MS instrumentation was employed to obtain structural details of the trimethylsilylated phase I metabolite released after hydrolysis, and the EI mass spectrum was always informative in steroidal structure studies owing to more useful fragment ions than the ESI mass spectrum. 16 metabolites including 6 glucuronide and 9 unreported sulfate conjugates were characterized and tentatively identified. All the metabolites were evaluated in terms of how long they could be detected. The sulfate conjugate S6 (1-methylen-5-androst-3,17-dione-2-sulfate) was considered to be a new long term metabolite for metenolone misuse that could be detected 40 days by liquid-liquid extraction and up to 30 days by direct-injection analysis after oral administration.


PubMed | China Anti Doping Agency
Type: Journal Article | Journal: Drug testing and analysis | Year: 2016

Oxymesterone (17-methyl-4, 17-dihydroxy-androst-4-ene-3-one) is one of the anabolic androgenic steroids (AAS) banned by the World Anti-Doping Agency (WADA). The biotransformation of oxymesterone is performed in vitro by human heptocytes and human urinary metabolic profiles are investigated after single dose of 20 mg to two adult males as well. Cell cultures and urine samples were hydrolyzed by -glucuronidase, extracted, and reacted with N-Methyl-N-trimethylsilyltrifluoroacetamide (MSTFA), ammonium iodide (NH4 I), and dithioerythritol. After derivatization, a gas chromatography triple quadruple tandem mass spectrometry (GC-MS/MS) using full scan and MS/MS modes was applied. The total ion chromatographs of the blank and the positive samples are compared, and 7 new metabolites were found. In addition to the well-known 17-epioxymesterone, oxymesterone is metabolized by 4-ene-reduction, 3-keto-reduction, 11-hydroxylation, and 16-hydroxylation. Based on the behavior of the MS/MS results of product ion and precursor ion modes, a GC-MS/MS method has been developed monitoring these metabolites. The structures of metabolite 2 and 4 are tentatively identified as 17-methyl-3, 17-dihydroxy-5-androstane-4-one and 17-methyl-3, 4, 17-trihydroxy-5-androstane, respectively. Detection of oxymesterone using new metabolites M2 and M4 can extend the detection window up to 4 days since the parent steroid was not detectable. Copyright 2015 John Wiley & Sons, Ltd.

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