Application of differential scanning calorimetry in the analysis of apprehended formulations of anabolic androgenic steroids

Berneira, Lucas M.; Freitas, S. C. de; Silva, Caroline Carapina da; Machado, Alexandre de Mattos; Pereira, Cláudio M. P.; Santos, Marco Aurélio Ziemann dos

doi:10.1016/j.forsciint.2018.12.022

Cited by 11 publications

(18 citation statements)

References 19 publications

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“…The evaluation of extraction methods is recurrent in the literature for several classes of substances. Nonetheless, few works compare the analytical procedures developed in the literature for the analysis of formulation of AASs, which is important in forensic science, given that the results are used as criminal evidence 10 . Among research studies, da Justa Neves and Caldas reported that there was a 5% increase in the recovery of testosterone, nandrolone, or trenbolone esters from oily formulations using ultrasonic bath compared with liquid–liquid or solid–liquid extraction.…”

Section: Discussionmentioning

confidence: 99%

“…According to the World Health Organization, falsified pharmaceutical products comprise formulations that have misspelled, absent, or incorrect label, as well as unknown or differently marketed chemical compositions/concentrations. Given that differences in the stated concentration of the active ingredients and the amounts detected in formulations also characterize signs of falsification, the extraction methods applied should retrieve the analytes quantitatively in the preparation 5,10 . Evaluation of the extractive protocols showed that generally the use of conventional methods (liquid–liquid, solid–liquid, or ultrasonic bath) had lower retrievals of the active ingredient compared with microwave assisted and ultrasonic probe.…”

Section: Discussionmentioning

confidence: 99%

“…For the identification and quantitation of the components of the matrix of the oily‐based formulations, a mix of 37 fatty acid methyl esters as a standard was purchased from Supelco (Bellefonte, USA) and used as a solution of 2 mg/mL in n ‐hexane. Quantitation of AASs was performed according to Berneira et al 10 using a stock solution (2 mg/mL) of cholesterol (≤99%, Sigma‐Aldrich, St Louis, USA) in methanol that was used to obtain the working solution (1 mg/mL) and the calibration curve (0.15, 0.25, 0.50, 0.75, and 1 mg/mL) 10 …”

Section: Methodsmentioning

confidence: 99%

“…These analytical tools provide separation and identification of the constituents of the sample, resulting in significant information about the questioned material. Besides colorimetric tests, other feasible techniques used to detect AASs include infrared (IR) spectroscopy, 9 nuclear magnetic resonance (NMR), 9 and differential scanning calorimetry (DSC) 10 …”

Section: Introductionmentioning

confidence: 99%

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Analytical approaches applied to the analysis of apprehended formulations of anabolic androgenic steroids

Berneira

Silva

Passos

et al. 2020

Drug Testing and Analysis

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Anabolic androgenic steroids (AASs) comprise a class of synthetic androgens resulting from chemical modifications of testosterone, known for their illicit consumption, which can result inextensive side effects. Extraction procedures applied to the analysis of their formulations are still limited to a few methodologies, despite the increasing numbers of confiscations of AASs. In this sense, the aims of this work were to evaluate the extraction of active ingredients from formulations of anabolic agents using solid‐liquid or liquid‐iquid, ultrasonic bath, ultrasonicprobe, and microwave‐assisted extraction. The results indicated that the extraction procedures influenced the detected concentration of AASs, as the use of ultrasonic probe and microwave irradiation increased the overall extraction of anabolic agents compared with solid‐liquid, liquid‐liquid, and ultrasonic bath. Regarding oxymetholone, for instance, the microwave‐assisted extraction and ultrasonic probe extracted, respectively, 37.46 ± 1.36 and 35.69 ± 0.98 mg/tablet, while solid‐liquid extracted 29.63 ± 0.40 mg/tablet of the activeingredient. Therefore, alternative methods such as microwave‐assisted extraction or theultrasonic probe could be used for the analysis of formulations of AASs assisting with the identification of illicit and toxic components.

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Section: Discussionmentioning

confidence: 99%

Section: Discussionmentioning

confidence: 99%

Section: Methodsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Analytical approaches applied to the analysis of apprehended formulations of anabolic androgenic steroids

Berneira

Silva

Passos

et al. 2020

Drug Testing and Analysis

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“…Besides, AASs can exist as polymorphs, which can alter the aspect and position of bands in the spectra and hamper the detection of the AAS (Chiong et al, 1992). In this sense, IR spectroscopy is generally used as a complementary and screening technique to further analytical tools (Berneira et al, 2019). Recently, IR spectroscopy has been combined with chemometry tools including principal component analysis (PCA) and partial least squares-discriminant analysis (PLS-DA) in order to detect possible falsifications or adulterations in a questioned sample based on previous results of supposed similar samples (Neves et al, 2016;Rebiere et al, 2016).…”

Section: Ir Spectroscopymentioning

confidence: 99%

Extraction and analytical approaches in the forensic evaluation of anabolic androgenic steroid formulations

Berneira

Poletti

Freitas

et al. 2021

WIREs Forensic Science

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Anabolic androgenic steroids are controlled or prohibited substances worldwide since their abusive usage can lead to extensive side effects. For forensic purposes, apprehended formulations of anabolic agents have to be analyzed to determine their components as well as possible adulterants and contaminants. Nevertheless, there are no comprehensive reviews in the field in order to compile the methods and analytical techniques that have been described so far.Therefore, the aim of this work was to review the analytical techniques and methods of extraction available for the analysis of formulations of anabolic agents. In this sense, 76 research works that analyzed formulations of anabolic agents from 1979 to 2021 were reviewed and distributed under the extraction methods and the analytical techniques employed by the authors. Generally, ultrasonic-assisted extraction associated with methanol as extractor solvent is the procedure of choice with little contribution of solid or liquid-liquid extraction. According to the literature, there are several analytical tools available for the analysis of these substances, although gas and liquid chromatography coupled to mass spectrometry as well as spectroscopic techniques are frequently employed. Nonetheless, novel techniques have been developed in order to decrease analysis time, cost, and sample preparation, which are important features in the expressive numbers of anabolic agents apprehended yearly. Therefore, the application of adequate methods of extraction coupled to suitable analytical techniques can be efficient forensic tools in order to contest the illicit supply of anabolic androgenic steroids providing consistent evidence to legal courts.

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Screening method for the characterization of anabolic steroids seized in Brazil using paper spray mass spectrometry and chemometric tools

et al. 2022

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This paper reports the use of paper spray mass spectrometry (PS‐MS) combined with chemometric models to analyze seized samples of anabolic steroids. Because many forensic laboratories typically demand high‐throughput analysis for this type of sample, we developed a quicker and simpler alternative analytical method for routine analysis with minimal sample preparation. Oily samples (n = 39) resulting from seizures carried out by Brazilian Federal and State Police units were selected for this study. These samples were analyzed by PS‐MS in the positive ion mode and full scan (50–1000 m/z), providing spectra containing patterns of the respective active ingredients present in each product. A principal component analysis (PCA) model was built, which discriminated samples mainly according to their active ingredients and allowed to detect and characterize some cases of product counterfeiting. The variable selection method ordered predictors selection was employed jointly with PCA to improve sample cluster separation and to provide model simplification. The final PCA model was built with three principal components and using only 28 spectral variables. This model accounted for 69.82% of the variance and discriminated samples according to their specific active ingredients.

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Application of differential scanning calorimetry in the analysis of apprehended formulations of anabolic androgenic steroids

Cited by 11 publications

References 19 publications

Analytical approaches applied to the analysis of apprehended formulations of anabolic androgenic steroids

Analytical approaches applied to the analysis of apprehended formulations of anabolic androgenic steroids

Extraction and analytical approaches in the forensic evaluation of anabolic androgenic steroid formulations

Screening method for the characterization of anabolic steroids seized in Brazil using paper spray mass spectrometry and chemometric tools

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