Otimização do método extração sólido-líquido com partição em baixa temperatura para determinação de carbaril em abacaxi pérola (ananas comosus) por cromatografia líquida de alta eficiência

Abstract

The use of agrochemicals in Brazil has driven several researches in food analysis, since, Brazil has been placed in a prominent position in the ranking of the largest consumers of these compounds. The indiscriminate use of these compounds causes great losses and damages to human health and the environment. The National Agency of Sanitary Surveillance (ANVISA), together with the Food Agrochemical Waste Analysis Program (PARA), monitors the food to detect if the producers are indiscriminately using these compounds. Therefore, the objective of this research was to optimize the analytical process of the solid-liquid extraction method with low temperature partition for extraction of carbaryl in pearl pineapple (ananas comosus) matrices. The pineapple was chosen due to its great commercialization in the region of Itumbiara-GO and because it was one of the fruits that presented pesticide residues above that allowed in the last report of the PARA, published in 2016. For optimization of the solid liquid extraction method with partition (ESL-PBT), a complete factorial design 2³ was used to evaluate the simultaneous behavior of three factors in two levels, in triplicate. For separation, identification and quantification of carbaryl, high performance liquid chromatography with ultraviolet detector (HPLC-UV) was used. The ESL / PBT method applied in the determination of carbaryl in pineapple matrices was simple and efficient, consuming small amounts of solvents and samples, with good average recovery percentage. The best factorial design test was the factorial design test 5, in which the optimized methodology consumed only 2 mL of extractive solution (acetonitrile with ethyl acetate) and it was not necessary to add salt to increase the ionic strength. The percentage of recovery of carbaryl in pineapples was 103.10%. The experiments with real samples of pineapple marketed in the municipality of Itumbiara-GO using the ESL-PBT method optimized in this work and analysis by HPLC UV did not present the presence of carbaryl or those were below the detection limit of the method and the apparatus.