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Larina I.M.,Russian Academy of Sciences | Kochnova E.A.,Antidoping Center | Pastushkova L.K.,Russian Academy of Sciences | Rodchenkov G.M.,Antidoping Center | And 2 more authors.
Human Physiology | Year: 2011

In order to study the time course of the parameters of urine sex steroid profile and its potential boundary changes, the quantitative determination of a number of endogenous steroids and their metabolites in healthy human urine has been carried out by the gas chromatography method using mass-selective detection. The samples were obtained from six volunteers under the conditions of total monitoring of vital activity factors affecting urine steroid profile (diet, water consumption, physical activity, temperature and air composition, day-night rhythm, and the psychoemotional state) in an experimental study using a pressurized compartment. The healthy human profile parameters of urine steroids were found, which were affected by conditions of controlled vital activity in a pressurized compartment. Parameters of the individual and group variability of the parameters of steroid profile and their dependence on experimental factors, salt consumption mode, and autonomous vital activity, were found. © 2011 Pleiades Publishing, Ltd. Source


Sobolevskii T.G.,Antidoping Center | Prasolov I.S.,Antidoping Center | Rodchenkov G.M.,Antidoping Center
Journal of Analytical Chemistry | Year: 2011

Smoking mixtures containing cannabimimetic indoles may still be illegally sold in Russia. Although a method for their analysis is required for forensic toxicology authorities, the detection of synthetic cannabinoids is a complicated analytical task because of low anticipated concentrations in urine and the lack of in vivo data on their metabolism. Here, the urinary metabolites of 1-pentyl-3-(1-naphthoyl)indole (JWH-018) and a procedure for determining them in urine are reported. Using gas and high-performance liquid chromatography combined with tandem mass spectrometry, two main monohydroxylated metabolites were identified in urine. Based on differences in their electron ionization MS/MS spectra, it is supposed that one of them is formed by the hydroxylation of an indole ring and the other, by the hydroxylation of a pentyl side chain. The main metabolites are almost completely excreted as conjugates with glucuronic acid. The structure of minor metabolites was proposed. The parent compound was not detected in urine at a level of 50 pg/mL 12 h after administration. © 2011 Pleiades Publishing, Ltd. Source


Sobolevskii T.G.,Antidoping Center | Prasolov I.S.,Antidoping Center | Rodchenkov G.M.,Antidoping Center
Journal of Analytical Chemistry | Year: 2010

A procedure that makes it possible to establish the origin of endogenous steroids present in human urine by the determination of the 13C/ 12C carbon isotope ratio is described. A combination of solid-phase and liquid-liquid extraction, as well as semipreparative liquid chromatography, was used to separate fractions containing testosterone, 5α- and 5β-androstane-3α, 17β-diols, androsterone, ethiocholanolone, 5β-preg-nane-3α, 20S-diol, and 16(5α)-androstene-3α-ol. More than 100 samples were analyzed by gas chromatography coupled with isotope mass spectrometry. The resulting values of 13C/12C were statistically processed, and the ranges required for the interpretation of the results were found. The procedure was certified and accredited in accordance with ISO 17025 requirements. © Pleiades Publishing, Ltd., 2010. Source


Dikunets M.A.,Antidoping Center | Savel'Eva N.B.,Antidoping Center | Bolotov S.L.,Antidoping Center | Virus E.D.,Antidoping Center | Rodchenkov G.M.,Antidoping Center
Journal of Analytical Chemistry | Year: 2010

Factors affecting the sensitivity and selectivity of the determination of diuretics, anabolic steroids, central nervous system stimulants, and narcotics in the analysis of human urine extracts by high-performance liquid chromatography-tandem mass spectrometry with atmospheric pressure electrospray ionization and recording of positive ions were investigated. Mass spectra were obtained for all of the test compounds; the characteristic ions, retention times, detection limits, degree of ionization suppression by the matrix, the extraction of the analytes from human biological fluids were determined for all analytes; the selectivity and specificity of determination were evaluated. © 2010 Pleiades Publishing, Ltd. Source


Dikunets M.A.,Antidoping Center | Virus E.D.,Antidoping Center | Semenistaya E.N.,Antidoping Center | Sobolevsky T.G.,Antidoping Center | Rodchenkov G.M.,Antidoping Center
Journal of Analytical Chemistry | Year: 2010

The mass spectral properties of the peroxisome proliferator-activated receptor agonists (PPARδ) have been studied by high-performance liquid chromatography/tandem mass spectrometry (HPLC-MS/MS) and high-performance liquid chromatography/high resolution mass spectrometry (HPLC/HRMS). Dissociation pathways of the investigated compounds under the conditions of collision activation have been proposed on the basis of the consolidated analysis of the data provided by these methods. © 2010 Pleiades Publishing, Ltd. Source

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