Analysis of seized stanozolol formulations in South Brazil by liquid chromatography coupled to quadrupole time-of-flight-mass spectrometry

Everton Rafael Campos; Sarah Eller; Leticia Birk; Masurquede Azevedo Coimbra; Sandra Manoela Dias Macedo; Mauricio Yonamine; Josias Oliveira Merib; Tiago Franco de Oliveira

doi:10.22456/2527-2616.108853

Authors

Everton Rafael Campos Pharmacosciences Department - Federal University of Health Sciences of Porto Alegre
Sarah Eller Pharmacosciences Department - Federal University of Health Sciences of Porto Alegre
Leticia Birk Pharmacosciences Department - Federal University of Health Sciences of Porto Alegre
Masurquede Azevedo Coimbra Pharmacosciences Department - Federal University of Health Sciences of Porto Alegre
Sandra Manoela Dias Macedo Pharmacosciences Department - Federal University of Health Sciences of Porto Alegre; Instituto Nacional de Ciência e Tecnologia Forense (INCT Forense)
Mauricio Yonamine School of Pharmaceutical Sciences - University of São Paulo
Josias Oliveira Merib Pharmacosciences Department - Federal University of Health Sciences of Porto Alegre
Tiago Franco de Oliveira Pharmacosciences Department - Federal University of Health Sciences of Porto Alegre

DOI:

https://doi.org/10.22456/2527-2616.108853

Keywords:

Anabolic-androgenic steroids, stanozolol, liquid chromatography, mass spectrometry

Abstract

Anabolic-androgenic steroids (AAS) are synthetic derivatives of testosterone which are used medically for several diseases. However, misuse is commonly observed by athletes to promote enhancement of strength and performance. AAS are frequently obtained through online black markets from clandestine drug manufacturing laboratories, without any quality standards, being potentially dangerous for users. The purpose of this work was the development and application of a fast and simple procedure for the quantitation of stanozolol by liquid chromatography coupled to quadrupole time-of-flight-mass spectrometry (LC-QTOF-MS) in tablets packs seized in Rio Grande do Sul state, Brazil. The samples of stanozolol were separated considering its dosage form. The internal standard (methyltestosterone) was added to the aliquots of the samples, dissolved in methanol and 5μL were injected into the analytical system. The newly developed method has been validated for lower limit of quantitation (LLOQ), linearity, accuracy, precision and selectivity. The LLOQ was 0.1 µg/mL. The developed method was successfully applied to 31 samples seized by the Secretaria da Receita Federal do Brasil (a Brazilian federal revenue service agency). According to the results, 90.3% of the suspected medicines (n=31) were adulterated, and 65% exhibited higher concentrations of stanozolol than those indicated in the label. This work successfully established a new method for quantification of stanozolol using LC-QTOF-MS. This method aims at contributing to the identification and quantification of this anabolic androgenic steroid frequently seized by federal inspection agencies.

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