Desenvolvimento de métodos cromatográficos para análise de plastificantes, alquilfenóis e seus metabólitos em alimentos e urina

Abstract

Development of Chromatographic Methods for Analysis of Plasticizers, Alkylphenols and its Metabolites in Food and Urine Endocrine disrupting chemicals (EDC) are present in many foods, they are substancesthat produce endocrine dysfunction in men and animals. These compounds are found in very low concentrations, high sensitivity analytical techniques are required for their quantification. This work presents the development of chromatographic methods foranalysis of alkylphenols and plasticizers in food and bisphenol A e plasticizers metabolites in urine samples. Samples of chicken, vegetables and food simulants were analyzed in migration studies of plasticizers from plastic containers to food. It was developed and validated methods to analyze plasticizers using gas chromatography andsolid phase microextraction. The study of plasticizers migration of was initially made to evaluate if the process of heating plastic containers in microwave ovens cause the migration of plasticizers for food. A new method using solid-phase microextraction with cooled fiber by liquid nitrogen (CF-SPME) with determination by gas chromatography coupled to mass spectrometry was developed and validated. To evaluate the migration of plasticizers, new plastic containers and long-term usedcontainers were filled with ultrapure water (used as food simulant) and heated in domestic microwave at different periods of time and different power levels. The plasticizer dibutyl phthalate was found in the samples. In general, an increase in migration was observed in containers with long-term use in larger heating times. The CF-SPME was also used to evaluate the migration of plasticizers to roast chicken in plastic bags using a conventional oven. The samples of spices, which were sold together with plastic bags was also evaluated. The plasticizers diisobutylphatalae and dibutylphthalate were found in samples of spice and meat spiced chicken. The alkylphenols and plasticizers migration was also evaluated in marketed frozen vegetables. For such, a method using solid phase microextraction and comprehensive two-dimensional gas chromatography with flame ionization detector (GC × GC-FID)was developed and validated. The compounds were analyzed on samples of carrot, potato and corn. The compounds tert-octylphenol, dibutylphthalate and benzylbutylphthalate were found in samples of carrot. The dibutylphthalate was found in one corn sample. The evaluation of plasticizers in food showed the possible sourcesof human contamination by these compounds, but not their exposure. Thus, for evaluation of plasticizers exposure biological samples were analyzed. Bisphenol A and plasticizers metabolites were determined in women urine samples. It was developed and validated a method for the analysis of bisphenol A and plasticizers metabolites usingliquid phase microextraction and gas chromatography coupled to mass spectrometry. The metabolites were found at different concentrations in the urine samples. An evaluation study of the relationship between endometriosis and bisphenol A and plasticizers was also realized. The study showed that there is not a relationship between the concentration of bisphenol A and plasticizers metabolites in urine and the presenceof endometriosis in women when the metabolites were compared.