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

Abstract

Counterfeiting and adulteration of pharmaceuticals is a prevalent problem worldwide and represents a major health risk to the population, with anabolic steroids being one of the main classes of drugs consumed and obtained from dubious sources. In this work, we propose the use of the 1H NMR technique to evaluate formulations containing anabolic steroids, with analysis of 40 samples of anabolic drugs that are used in injectable and capsule forms. The samples analyzed presented the following active ingredients: testosterone propionate, testosterone phenylpropionate, testosterone isocaproate, testosterone decanoate, testosterone cypionate, testosterone undecanoate, stanozolol, drostanolone propionate, trenbolone acetate, oxymetholone, and methandrostenolone. The 1H NMR spectroscopic measurements were performed using a 600 MHz Bruker Avance III spectrometer, with deuterated chloroform (CDCl3) containing 0.1% TMS as solvent. Of the 40 samples analyzed, eight did not show the presence of the active principle stated on the label. Three types of adulteration were found in the analyzed samples: absence of the active ingredient, adulteration with other substances, and concentration values below those indicated on the label. Sildenafil citrate was found in four samples. The GC-MS technique was used to confirm the adulteration results found using 1H NMR. Quantitative determination by NMR was performed using internal standard and ERETIC 2 methods, and the results obtained were statistically the same.

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  • Authors+Show Affiliations

    ,

    Institute of Chemistry, São Paulo State University "Júlio de Mesquita Filho", 14800-060 Araraquara, SP, Brazil.

    ,

    Institute of Chemistry, São Paulo State University "Júlio de Mesquita Filho", 14800-060 Araraquara, SP, Brazil.

    ,

    Institute of Chemistry, São Paulo State University "Júlio de Mesquita Filho", 14800-060 Araraquara, SP, Brazil.

    ,

    Institute of Chemistry, São Paulo State University "Júlio de Mesquita Filho", 14800-060 Araraquara, SP, Brazil.

    Institute of Chemistry, São Paulo State University "Júlio de Mesquita Filho", 14800-060 Araraquara, SP, Brazil. Electronic address: pezza@iq.unesp.br.

    Source

    Steroids 138: 2018 10 pg 47-56

    MeSH

    Gas Chromatography-Mass Spectrometry
    Proton Magnetic Resonance Spectroscopy
    Sildenafil Citrate
    Steroids
    Testosterone Congeners

    Pub Type(s)

    Journal Article
    Research Support, Non-U.S. Gov't

    Language

    eng

    PubMed ID

    30003910

    Citation

    Ribeiro, Marcos Vinícius de Moura, et al. "1H NMR Determination of Adulteration of Anabolic Steroids in Seized Drugs." Steroids, vol. 138, 2018, pp. 47-56.
    Ribeiro MVM, Boralle N, Felippe LG, et al. 1H NMR determination of adulteration of anabolic steroids in seized drugs. Steroids. 2018;138:47-56.
    Ribeiro, M. V. M., Boralle, N., Felippe, L. G., Pezza, H. R., & Pezza, L. (2018). 1H NMR determination of adulteration of anabolic steroids in seized drugs. Steroids, 138, pp. 47-56. doi:10.1016/j.steroids.2018.07.002.
    Ribeiro MVM, et al. 1H NMR Determination of Adulteration of Anabolic Steroids in Seized Drugs. Steroids. 2018;138:47-56. PubMed PMID: 30003910.
    * Article titles in AMA citation format should be in sentence-case
    TY - JOUR T1 - 1H NMR determination of adulteration of anabolic steroids in seized drugs. AU - Ribeiro,Marcos Vinícius de Moura, AU - Boralle,Nivaldo, AU - Felippe,Lidiane Gaspareto, AU - Pezza,Helena Redigolo, AU - Pezza,Leonardo, Y1 - 2018/07/10/ PY - 2018/03/26/received PY - 2018/06/11/revised PY - 2018/07/05/accepted PY - 2018/7/14/pubmed PY - 2019/3/21/medline PY - 2018/7/14/entrez KW - (1)H NMR KW - Adulteration KW - Anabolic steroids KW - Authenticity KW - Quantification SP - 47 EP - 56 JF - Steroids JO - Steroids VL - 138 N2 - Counterfeiting and adulteration of pharmaceuticals is a prevalent problem worldwide and represents a major health risk to the population, with anabolic steroids being one of the main classes of drugs consumed and obtained from dubious sources. In this work, we propose the use of the 1H NMR technique to evaluate formulations containing anabolic steroids, with analysis of 40 samples of anabolic drugs that are used in injectable and capsule forms. The samples analyzed presented the following active ingredients: testosterone propionate, testosterone phenylpropionate, testosterone isocaproate, testosterone decanoate, testosterone cypionate, testosterone undecanoate, stanozolol, drostanolone propionate, trenbolone acetate, oxymetholone, and methandrostenolone. The 1H NMR spectroscopic measurements were performed using a 600 MHz Bruker Avance III spectrometer, with deuterated chloroform (CDCl3) containing 0.1% TMS as solvent. Of the 40 samples analyzed, eight did not show the presence of the active principle stated on the label. Three types of adulteration were found in the analyzed samples: absence of the active ingredient, adulteration with other substances, and concentration values below those indicated on the label. Sildenafil citrate was found in four samples. The GC-MS technique was used to confirm the adulteration results found using 1H NMR. Quantitative determination by NMR was performed using internal standard and ERETIC 2 methods, and the results obtained were statistically the same. SN - 1878-5867 UR - https://www.unboundmedicine.com/medline/citation/30003910/1H_NMR_determination_of_adulteration_of_anabolic_steroids_in_seized_drugs L2 - https://linkinghub.elsevier.com/retrieve/pii/S0039-128X(18)30118-1 DB - PRIME DP - Unbound Medicine ER -