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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.

Lu J.,China Anti Doping Agency | He G.,China Anti Doping Agency | Wang X.,China Anti Doping Agency | Xu Y.,China Anti Doping Agency | And 6 more authors.
Journal of Chromatography A | Year: 2012

Clomiphene, a selective estrogen receptor modulator, is prohibited by World Anti Doping Agency (WADA) out-of-competition and in-competition. As it is extensively metabolized, further investigation of clomiphene metabolic profile will be essential to routine anti-doping analysis. The metabolic pathway and the different metabolites of clomiphene in human urine collected from three healthy volunteers during 1. week were studied by liquid chromatography-quadrupole time-of-flight mass spectrometry (LC-QTOFMS) based on accurate mass measurement. Seven unreported metabolites were identified and characterized, and all of the newly found urinary metabolites belonged to a new metabolic pathway (hydrogenation). An approach for the metabolism study of clomiphene and its analogs by LC-QTOFMS was presented. Two metabolites, 3,4-dihydroxy-dihydro-clomiphene (m/. z 440.1991) and 3,4-dihydroxy-dihydro-deethyl-clomiphne (m/. z 412.1674), are the potential biomarkers for monitoring oral administration of clomiphene in doping control. © 2012 Elsevier B.V.

Lu J.,China Anti Doping Agency | He C.,China Anti Doping Agency | He G.,China Anti Doping Agency | Wang X.,China Anti Doping Agency | And 4 more authors.
Journal of Mass Spectrometry | Year: 2014

In this study, tamoxifen metabolic profiles were investigated carefully. Tamoxifen was administered to two healthy male volunteers and one female patient suffering from breast cancer. Urinary extracts were analyzed by liquid chromatography quadruple time-of-flight mass spectrometry using full scan and targeted MS/MS techniques with accurate mass measurement. Chromatographic peaks for potential metabolites were selected by using the theoretical [M + H] + as precursor ion in full-scan experiment and m/z 72, 58 or 44 as characteristic product ions for N,N-dimethyl, N-desmethyl and N,N-didesmethyl metabolites in targeted MS/MS experiment, respectively. Tamoxifen and 37 metabolites were detected in extraction study samples. Chemical structures of seven unreported metabolites were elucidated particularly on the basis of fragmentation patterns observed for these metabolites. Several metabolic pathways containing mono- and di-hydroxylation, methoxylation, N-desmethylation, N,N-didesmethylation, oxidation and combinations were suggested. All the metabolites were detected in the urine samples up to 1 week. Copyright © 2014 John Wiley & Sons, Ltd. Copyright © 2014 John Wiley & Sons, Ltd.

Lu J.,China Anti Doping Agency | Wang S.,China Anti Doping Agency | Dong Y.,China Anti Doping Agency | Wang X.,China Anti Doping Agency | And 7 more authors.
Analytica Chimica Acta | Year: 2010

A method for the simultaneous screening and confirmation of the presence of fourteen tertiary amine stimulants in human urine by gas chromatography-mass spectrometry (GC-MS) in combination with liquid chromatography-tandem mass spectrometry (LC-MS/MS) has been developed and validated. Solid phase extraction (SPE) and liquid-liquid extraction (LLE) approaches were utilized for the pre-treatment of the urine samples. The study indicated that the capillary temperature played a significant role in the signal abundances of the protonated molecules of cropropamide and crotethamide under positive ion electrospray ionization (ESI) conditions. In addition, comparison studies of two different pre-treatment approaches as well as the two ionization modes were conducted. The LODs of the developed method for all the analytes were lower than the minimum required performance limit (MRPL) as set forth in the World Anti-Doping Agency (WADA) technical document for laboratories. The human urine sample obtained after oral administration of prolintane·HCl was successfully analyzed by the developed method, which demonstrated the applicability and reliability of the method for routine doping control analysis. © 2009 Elsevier B.V. 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.

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