Microwave-assisted extraction and differential scanning calorimetry in the chemical identification of sliming agents apprehended in the south region of Brazil.
Autor: | de Freitas SC; Center of Chemical, Pharmaceutical and Food Sciences, Lipidomic and Bio-Organic Laboratory, Bioforensic Research Group, Federal University of Pelotas, Eliseu Maciel St., s/n, 96900-010 Pelotas, RS, Brazil., Dos Santos MAZ; Center of Chemical, Pharmaceutical and Food Sciences, Lipidomic and Bio-Organic Laboratory, Bioforensic Research Group, Federal University of Pelotas, Eliseu Maciel St., s/n, 96900-010 Pelotas, RS, Brazil. Electronic address: marcziemann@gmail.com., Berneira LM; Center of Chemical, Pharmaceutical and Food Sciences, Lipidomic and Bio-Organic Laboratory, Bioforensic Research Group, Federal University of Pelotas, Eliseu Maciel St., s/n, 96900-010 Pelotas, RS, Brazil., Ortiz RS; Rio Grande do Sul Technical and Scientific Division, Bioforensic Research Group, Brazilian Federal Police, Ipiranga Av., 1365, 90160-093 Porto Alegre, RS, Brazil., de Pereira CMP; Center of Chemical, Pharmaceutical and Food Sciences, Lipidomic and Bio-Organic Laboratory, Bioforensic Research Group, Federal University of Pelotas, Eliseu Maciel St., s/n, 96900-010 Pelotas, RS, Brazil. |
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Jazyk: | angličtina |
Zdroj: | Science & justice : journal of the Forensic Science Society [Sci Justice] 2019 Mar; Vol. 59 (2), pp. 190-198. Date of Electronic Publication: 2018 Nov 06. |
DOI: | 10.1016/j.scijus.2018.11.001 |
Abstrakt: | Over the past decades, consume of slimming agents considerably increased in several countries, including Brazil, due to weight-loss and stimulant properties. Since these drugs are controlled to prevent illicit and indiscriminate use, there is a parallel illegal market that uses the Internet and irregular pharmacies in order to distribute these formulations. Slimming agents produced by these illegal sources are known for being manufactured with little or none quality control resulting in uncertain and unknown formulations. For forensic purposes, apprehended pharmaceuticals have to undergo a process of chemical identification that can be difficult due to its complex matrix. In this sense, application of assisted energies in the extraction step such as microwave irradiation can be a promising method to increase the recuperation of the target molecules of the sample. Therefore, the aim of this research was to identify four slimming agents apprehended in Brazil by means of visual inspection, Fourier Transform Infrared Spectroscopy, Differential Scanning Calorimetry and Gas Chromatography - Mass Spectrometry. Moreover, the efficiency of solid-liquid extraction and microwave-assisted extraction was compared. It should be noted that our work was one of the few to use Differential Scanning Calorimetry and the application of microwave irradiation in the analysis of apprehended materials. Results showed that the majority of the samples was counterfeit being composed of one or several adulterants or contaminants. Initially, visual inspection resourcefully screened the slimming agents for possible signs of falsification, however it failed to detect fraudulent products that were very similar to veridical medicines. Sequentially, Fourier Transform Infrared Spectroscopy detected functional groups present in the samples while the presence or absence of the alleged active ingredients were successfully measured with Differential Scanning Calorimetry and, thus, providing a full chemical screening of the apprehended materials. Gas Chromatography- Mass Spectrometry confirmed the presence of adulterants such as caffeine, fluoxetine and phenolphthalein as well as contaminants such as sulfurol in the falsified samples. Finally, comparison of extraction procedures indicated that microwave-assisted extraction increased the recovery of compounds detected in chromatographic analysis to a greater extent than solid-liquid extraction. (Copyright © 2018 The Chartered Society of Forensic Sciences. Published by Elsevier B.V. All rights reserved.) |
Databáze: | MEDLINE |
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