%0 Journal Article
%T A simple toxicological analysis of anabolic steroid preparations from the black market Analyse toxicologique simple de st¨¦ro diens anabolisants provenant de march¨¦s parall¨¨les
%A Pellegrini Manuela
%A Rotolo Maria Concetta
%A Di Giovannadrea Rita
%A Pacifici Roberta
%J Annales de Toxicologie Analytique
%D 2012
%I 
%R 10.1051/ata/2012011
%X Objectives: A simple and rapid gas chromatography (GC) method with mass spectrometry (MS) detection was developed for the identification and quantification of anabolic steroids in pharmaceutical preparations from the black market. Material and Methods: After a liquid-liquid extraction of pharmaceutical products at acidic, neutral and basic pH with chloroform-isopropanol (9:1, v/v), the different steroids were separated by fused silica capillary column and detected by electron impact (EI)-MS in positive ionization mode. Results and Conclusion: The assay was validated in the range from 10 mg to 250 mg/g powder preparations and 0.02 mg to 200 mg/mL liquid preparations with good determination coefficients (hbox{$r^{2} geqslant 0.99$}r2   0.99) for the calibration curves. At three concentrations spanning the linear dynamic ranges of the calibration curves, mean recoveries were always higher than 90% and intra-assay and inter-assay precision and accuracy were always better than 15%. This method was successfully applied to the analysis of 15 pharmaceutical preparations sold by illegal sources. In only two cases the content was the one reported on the labels. In the other cases, no substances at all, or steroids different from those reported on the labels or different amounts from those declared were found. Objectifs : Une m¨¦thode d¡¯identification de st¨¦ro des anabolisants obtenus sur les march¨¦s parall¨¨les par chromatographie en phase gazeuse simple et rapide avec d¨¦tection par spectrom¨¦trie de masse a ¨¦t¨¦ d¨¦velopp¨¦e. Mat¨¦riel et M¨¦thodes : Apr¨¨s une extraction liquide-liquide des principes actifs ¨¤ pH acide, neutre et basique par le m¨¦lange chloroforme-isopropanol (9:1, v/v), les diff¨¦rents st¨¦ro des ont ¨¦t¨¦ s¨¦par¨¦s sur une colonne capillaire et d¨¦tect¨¦s par spectrom¨¦trie de masse (impact ¨¦lectronique en mode d¡¯ionisation positive). Le dosage a ¨¦t¨¦ valid¨¦ sur la gamme 10¨C250 mg/g de pr¨¦parations en poudre et sur la gamme 0,02¨C200 mg/mL de pr¨¦parations liquides (hbox{$r^{mathrm{2}} geqslant $}r2    0,99 pour les courbes d¡¯¨¦talonnage). R¨¦sultats et Conclusion : ¨¤ trois concentrations comprises dans les gammes des courbes d¡¯¨¦talonnage, les recouvrements moyens ¨¦taient toujours sup¨¦rieurs ¨¤ 90 %, et les pr¨¦cisions intra-essai et inter-essai ¨¦taient toujours sup¨¦rieures de 15 %. Cette m¨¦thode a ¨¦t¨¦ appliqu¨¦e avec succ¨¨s ¨¤ l¡¯analyse de 15 produits pharmaceutiques vendus par des sources ill¨¦gales. Dans deux cas seulement, le contenu correspondait ¨¤ ce qui ¨¦tait indiqu¨¦ sur les ¨¦tiquettes. Dans les autres cas, aucune autre substance n¡¯a ¨¦t¨¦ trouv¨¦e, ou les st¨¦ro des
%K Anabolic steroids
%K ccounterfeits
%K black market
%K analysis
%K St¨¦ro des anabolisants
%K contrefa ons
%K march¨¦ parall¨¨le
%K analyse
%U http://dx.doi.org/10.1051/ata/2012011