RESUMO
Liquid smoke is a food additive and cresols are among its chemical constituents, potentially toxic to human health. Thus, the objective of this study was to develop a method to quantify cresols in liquid smoke. First, the liquid-liquid extraction with low temperature purification (LLE-LTP) was validated for cresols in water, as there are no cresol-free liquid smoke samples. Analyzes were performed by gas chromatography coupled to mass spectrometry in full scan mode. LLE-LTP was subsequently applied in five commercial samples of liquid smoke. Validation results showed that the proposed extraction method was selective for cresols, linear in the range of 0.5 to 35 mg L-1, limit of quantification of 0.5 mg L-1, recovery rate between 90% and 104% and relative standard deviation lower than 10%. The quantification of cresols in liquid smoke samples ranged from 3.0 to 38.3 mg L-1 and the concentration of these chemical contaminants in liquid smoke remained constant for at least 21 days at 25 °C.
Assuntos
Cromatografia Gasosa-Espectrometria de Massas , Extração Líquido-Líquido , Fumaça , Extração Líquido-Líquido/métodos , Cromatografia Gasosa-Espectrometria de Massas/métodos , Fumaça/análise , Temperatura BaixaRESUMO
Honey is widely consumed worldwide, however, this food can be contaminated by chemical contaminants, such as the insecticide dichlorodiphenyltrichloroethane (DDT). Despite legal restrictions on DDT use, this organochlorine pesticide has been detected in honey collected in several developed and developing countries, representing risks to human health, animals, and the environment due to its high environmental persistence, potential carcinogenicity, and ecotoxicological effects. Thus, the development of an analytical method for DDT monitoring in this matrix is important to ensure food security. Therefore, this study aimed to optimize and validate a simple, low-cost, and efficient method using the liquid-liquid extraction with low-temperature purification (LLE-LTP) to determine DDT in honey samples by high-performance liquid chromatography with diode array detector (HPLC-DAD). The proposed method was validated according to SANTE guidelines, being considered selective, precise, accurate, and linear in the range of 8.0-160 µg kg-1. The limits of detection (LOD) and quantification (LOQ) achieved were 4.0 and 8.0 µg kg-1, respectively. This LOQ value is lower than the maximum residue limit established by the Brazilian and European Union legislation. Therefore, the LLE-LTP combined to HPLC-DAD allows the routine analysis of DDT in honey samples and can be widely applied in studies to monitor this pesticide, especially in developing countries, where DDT use is still allowed.