A simple toxicological analysis of anabolic steroid preparations from the black market

Abstract

-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 (r 2 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.Key words: Anabolic steroids, ccounterfeits, black market, analysis Résumé -Objectifs : Une méthode d'identification de stéroïdes anabolisants obtenus sur les marchés parallèles par chromatographie en phase gazeuse simple et rapide avec détection par spectrométrie de masse a été développée. Matériel et Méthodes : Après une extraction liquide-liquide des principes actifs à pH acide, neutre et basique par le mélange chloroforme-isopropanol (9:1, v/v), les différents stéroïdes ont été séparés sur une colonne capillaire et détectés par spectrométrie de masse (impact électronique en mode d'ionisation positive). Le dosage a été validé sur la gamme 10-250 mg/g de préparations en poudre et sur la gamme 0,02-200 mg/mL de préparations liquides (r 2 0,99 pour les courbes d'étalonnage). Résultats et Conclusion : À trois concentrations comprises dans les gammes des courbes d'étalonnage, les recouvrements moyens étaient toujours supérieurs à 90 %, et les précisions intra-essai et inter-essai étaient toujours supérieures de 15 %. Cette méthode a été appliquée avec succès à l'analyse de 15 produits pharmaceutiques vendus par des sources illégales. Dans deux cas seulement, le contenu correspondait à ce qui était indiqué sur les étiquettes. Dans les autres cas, aucune autre substance n'a été trouvée, ou les stéroïdes détectés étaient différents de ceux inscrits sur les étiquettes ou comportaient des quantités différentes de celles indiquées.

The risk environment of anabolic–androgenic steroid users in the UK: Examining motivations, practices and accounts of use

“…Despite few doubting the reliability of the steroids accessed, the forensic analysis of the 10 samples sourced revealed that only three actually contained what was stated on the packaging and those that did had very low active ingredients compared with the strength indicated (see Coomber et al 2014 for further discussion on this). This is in line with international studies which highlight the variation in the forensic composition of steroids (Coopman and Cordonnier, 2012;Graham et al, 2009;Kohler et al, 2010;Pellegrini et al, 2012;Thevis et al, 2008). Coomber et al (2014, p. 138) point out, however, that caution is needed in extrapolating health risks from such data: 'inauthentic substances will present different risks and many of these will not be necessarily high risk nor the product of cynical acts'.…”

The supply of steroids and other performance and image enhancing drugs (PIEDs) in one English city: Fakes, counterfeits, supplier trust, common beliefs and access

“…More recently, Graham et al [38] A further study from Germany [40] yielded similar results with only four of 11 confiscated black market products containing the substance and amount declared on the label. Showing consistency across borders a recent Italian study [41] found that only two of 15 pharmaceutical preparations seized by authorities contained the content stated on the labels. In each of the other cases, either no PIED were present at all or steroids different from those listed on the labels or different amounts from those declared were found.…”

1H NMR determination of adulteration of anabolic steroids in seized drugs

“…The literature describes several methods for determination of the authenticity and quantification of anabolic steroids in different pharmaceutical formulations, highlighting chromatographic methods including gas chromatography [7,8,11,12] and liquid chromatography [9,[13][14][15]. However, although these techniques are well established for this type of analysis, with good detection limits, they have a number of disadvantages from the operational point of view, such as the need for specific chromatographic columns, laborious sample preparation steps, and sometimes the use of derivatization reactions and toxic solvents.…”