Optimization and validation of an extraction method for endosulfan lactone on a solid substrate

Abstract

Endosulfan lactone is a metabolite obtained from the biological oxidation of the insecticide endosulfan by action of the microorganisms present in the soil. This metabolite is more toxic and persistent than the parent compound. Therefore, it is extremely important to be able to determine the presence of this metabolite in the soil. However, accessible methods for extraction of endosulfan lactone in soil were not found in published literature. For this reason, the aim of this study was to evaluate two conventional methods of liquid–solid extraction for the determination of endosulfan lactone in solid substrate using two solvents (ethyl acetate and acetonitrile) and HPLC UV-VIS. The acetonitrile and rotary agitation extraction method was the one with the highest efficiency (97%), optimized using a factorial 32 response surface design, and validated in terms of linearity and pre-cision. The linearity shown was r > 0.999 in a wide spike level (0.15–100 mg kg−1), with the detection limit (DL) of 0.045 mg kg−1 and quantification limit (QL) of 0.15 mg kg−1. The extraction of endosul-fan lactone in solid substrate using acetonitrile was more efficient than that used with ethyl acetate, so this method could be used to extract and quantify endosulfan lactone in agricultural soil.