The confirmation by GC/C/IRMS of the exogenous origin of pseudo-endogenous steroids from human urine samples requires extracts of adequate purity. A strategy based on HPLC sample purification prior to the GC/C/IRMS analysis of human urinary endogenous androgens (i.e. testosterone, androsterone and/or androstenediols). is presented. A method without any additional derivatization step is proposed, allowing to simplify the urine pretreatment procedure, leading to extracts free of interferences permitting precise and accurate IRMS analysis, without the need of correcting the measured delta values for the contribution of the derivatizing agent. The HPLC extracts were adequately combined to both reduce the number of GC/C/IRMS runs and to have appropriate endogenous reference compounds (ERC; i.e. pregnanediol, 11-keto-etiocholanolone) on each GC-IRMS run. The purity of the extracts was assessed by their parallel analysis by gas chromatography coupled to mass spectrometry, with GC conditions identical to those of the GC/C/IRMS assay. The method has been validated according to ISO17025 requirements (within assay precision below 0.3 parts per thousand C-13 delta units and between assay precision below 0.6 parts per thousand C-13 delta units for most of the compounds investigated) fulfilling the World Anti-Doping Agency requirements. (C) 2012 Elsevier B.V. All rights reserved.

A comprehensive procedure based on gas chromatography-isotope ratio mass spectrometry following high performance liquid chromatography purification for the analysis of underivatized testosterone and its analogues in human urine / Xavier De La, Torre; Cristiana, Colamonici; Davide, Curcio; Francesco, Molaioni; Botre', Francesco. - In: ANALYTICA CHIMICA ACTA. - ISSN 0003-2670. - STAMPA. - 756:(2012), pp. 23-29. [10.1016/j.aca.2012.10.013]

A comprehensive procedure based on gas chromatography-isotope ratio mass spectrometry following high performance liquid chromatography purification for the analysis of underivatized testosterone and its analogues in human urine

BOTRE', Francesco
2012

Abstract

The confirmation by GC/C/IRMS of the exogenous origin of pseudo-endogenous steroids from human urine samples requires extracts of adequate purity. A strategy based on HPLC sample purification prior to the GC/C/IRMS analysis of human urinary endogenous androgens (i.e. testosterone, androsterone and/or androstenediols). is presented. A method without any additional derivatization step is proposed, allowing to simplify the urine pretreatment procedure, leading to extracts free of interferences permitting precise and accurate IRMS analysis, without the need of correcting the measured delta values for the contribution of the derivatizing agent. The HPLC extracts were adequately combined to both reduce the number of GC/C/IRMS runs and to have appropriate endogenous reference compounds (ERC; i.e. pregnanediol, 11-keto-etiocholanolone) on each GC-IRMS run. The purity of the extracts was assessed by their parallel analysis by gas chromatography coupled to mass spectrometry, with GC conditions identical to those of the GC/C/IRMS assay. The method has been validated according to ISO17025 requirements (within assay precision below 0.3 parts per thousand C-13 delta units and between assay precision below 0.6 parts per thousand C-13 delta units for most of the compounds investigated) fulfilling the World Anti-Doping Agency requirements. (C) 2012 Elsevier B.V. All rights reserved.
2012
sample preparation; hplc; doping in sports; isotope ratio mass spectrometry (irms); androgens
01 Pubblicazione su rivista::01a Articolo in rivista
A comprehensive procedure based on gas chromatography-isotope ratio mass spectrometry following high performance liquid chromatography purification for the analysis of underivatized testosterone and its analogues in human urine / Xavier De La, Torre; Cristiana, Colamonici; Davide, Curcio; Francesco, Molaioni; Botre', Francesco. - In: ANALYTICA CHIMICA ACTA. - ISSN 0003-2670. - STAMPA. - 756:(2012), pp. 23-29. [10.1016/j.aca.2012.10.013]
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Utilizza questo identificativo per citare o creare un link a questo documento: https://hdl.handle.net/11573/614647
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