ESTiG - Dissertações de Mestrado Alunos
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Browsing ESTiG - Dissertações de Mestrado Alunos by Subject "2,4-dinitrofenol"
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- Development of a GC-MS methodology for determining the adulterant 2,4-dinitrophenol in weight loss food supplementsPublication . Gomes, Bernardo Luiz Mendes; Amaral, Joana; Ribeiro, António; Patrício, PattersonCurrently, the pursuit of a body that meets beauty standards has become a major goal for a large part of the population, greatly intensified by pictures of perfect bodies shared on social networks. This has impelled the growth of the “fitness” market, which offers a wide range of products for weight loss, including plant food supplements (PFS). Since overweight currently affects millions of individuals worldwide, weight-loss products are undoubtedly one of the most popular types of PFS. However, different reports, including from the Food and Drug Administration (FDA) and the EU Rapid Alert System of Food and Feed (RASFF), have raised concerns about fraudulent practices in this sector, particularly the addition of pharmaceutical drugs to boost the PFS effect. Different adulterants have been reported in PFS supplements, including 2,4-dinitrophenol (2,4-DNP), a compound used in the 1st World War to produce ammunition that showed weight loss as a side effect. Although 2,4-DNP is able to cause weight loss, it is associated with a high rate of dangerous effects since the drug causes the uncoupling of mitochondrial oxidative phosphorylation, leading to hyperthermia and diaphoresis, which, together with tachycardia and decreased blood pressure, can lead to death. Nevertheless, due to its thermogenic capacity, 2,4-DNP is a potential adulterant of weight loss PFS. Therefore, this work aimed at developing a methodology using gas chromatography coupled with mass spectrometry (GC-MS) to identify and quantify this compound if present in commercial samples of PFS. After optimization of the GC-MS operational parameters and derivatization procedure, the methodology was validated following the general guidance “ICH Q2 Validation of analytical procedures” of the European Medicines Agency (EMA) for method validation. All the parameters followed the EMA guideline including specificity, linearity, range of the curve, precision, accuracy, detection and quantification limit, and matrix effect. The calibration curve was shown to be linear within the range of 5 ppm to 0.05 ppm, with a limit of quantification of 0.05 mg/L and a limit of detection of 0.015 mg/L. Subsequently, the methodology was applied to a small set of commercial supplements, with the compound not being detected in any of the analyzed products.