Otimização da separação de hidrocarbonetos policíclicos aromáticos por cromatografia líquida de alta eficiência utilizando metodologia da superfície de resposta para análise de amostras de mexilhão e salmão defumado

Abstract

PAHs can be absorbed by humans over animal and vegetable food consumption. The contaminated soil, air, water, or the adoption of thermal techniques for food processing such as drying, curing, roasting and grilling may contribute to this type of contamination. Thus, PAHs are described in literature as contaminants in various foods such as barbecue meats, smoked meats, oils, fats, vegetables, nuts, cereals and also in seafood like shrimp, oysters, mollusks and mussels. These organisms are filter feeding and may accumulate PAHs due to the metabolism characteristics. Thus, the aim of this study carried out at the Laboratories of Liquid Chromatography of Embrapa and Federal Institute of Rio de Janeiro - Campus Nilópolis was develop and optimize the chromatographic separation methodology of 16 USEPA priority PAHs isomers and investigate the PAHs contamination of mussels and smoked salman imported from Chile. Samples were acquired in market places in the city of Rio de Janeiro and lyophilized for conservation until analytical work. Analyses were performed using high performance liquid chromatography with diode array coupled to a variable wavelength fluorescence detector. The identification of the contaminants was performed by comparing their UV spectra with NIST spectral library. The method validation was performed by determining the limit of detection, limit of quantitation, linearity and dynamic range. The total analysis time for the 16 polycyclic aromatic hydrocarbons separation was optimized for 21 minutes with quantitative resolution values (Rs > 1,5). The limits of detection and quantification of the method ranged from 0,0035 a 0,3523μg/Kg e 0,0107 a 0,9576μg/Kg, respectively, and are in accordance with the current legislation of the European Community (CE 835/2011). The presence of benzo(a)antraceno, criseno, benzo(b)fluoranteno, benzo(k)fluoranteno, benzo(a)pireno, dibenzo(a,h)antraceno, benzo(g,h,i)perileno e indeno(cd-1,2,3)pireno PAHs were identified in the mussel samples in a concentration range of 0,3548-2,1895μg/Kg. Benzo(b)fluoranteno, benzo(k)fluoranteno, benzo(a)pireno, dibenzo(a,h)antraceno e benzo(g,h,i)perileno PAHs were identified in samples of smoked salman in a concentration range of 0,0420-2,5052μg/Kg. In both samples the concentrations of these contaminants are below the maximum contamination level (MCL) allowed by CE Resolution 835/2011. These results demonstrate that the processing used in the preparation of these foods did not eliminate the presence of contaminants, showing the fundamental importance for the development or improvement of analytical methodologies for monitoring PAHs in seafood samples.