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Authenticity assessment of anabolic androgenic steroids in counterfeit drugs by 1H NMR


Anabolic steroids are synthetic hormone derivatives of testosterone, a masculine sex hormone. Their main effects include greater muscle size, physical strength, and resistance. The need for safe and reliable quality control of products and/or raw materials in the pharmaceutical industry makes analyses of active ingredients and other constituents of drug formulations extremely important for the manufacturers as well as users of these products. In this work, we propose the use of 1H NMR spectroscopy to analyze formulations containing anabolic steroids. Six types of anabolic steroids were studied (testosterone propionate, methyltestosterone, acetate methenolone, oxandrolone, nandrolone decanoate, and stanozolol), with analysis of 16 samples of anabolic drugs that are used in injectable, tablet, and capsule forms. The 1H NMR spectroscopic measurements were performed using a 600 MHz spectrometer, with deuterated chloroform (CDCl3) containing 0.03% TMS as solvent. Of the 16 samples analyzed, four did not show the presence of the active principle stated on the label. For quantitative analysis, dimethyl sulfone (DMSO2) was used as an internal reference standard. All the analytical curves were obtained for concentration ranges of 1.0-16.0 mg mL-1. The limits of detection and quantification varied in the ranges 0.18-0.61 and 1.30-2.19 mg mL-1, respectively. The intra-day and inter-day precision RSD values were in the ranges 1.86-4.22% and 2.17-4.75%, respectively. The recovery values ranged from 95.2 to 104.0%. The spectroscopic results statistically agreed with those obtained by reference methods (HPLC).

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Publication details

The article was received on 22 Jan 2018, accepted on 10 Feb 2018 and first published on 12 Feb 2018

Article type: Paper
DOI: 10.1039/C8AY00158H
Citation: Anal. Methods, 2018, Accepted Manuscript
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    Authenticity assessment of anabolic androgenic steroids in counterfeit drugs by 1H NMR

    M. V. D. M. Ribeiro, N. Boralle, H. R. Pezza and L. PEZZA, Anal. Methods, 2018, Accepted Manuscript , DOI: 10.1039/C8AY00158H

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