Ultrasound-assisted extraction of pesticides from olive branches: a multifactorial approach to method development

Abstract

A rapid and simple method has been developed for the analysis in olive branches of two insecticides currently used in olive pest control, dimethoate and alpha-cypermethrin. The effects of analytical conditions on pesticide recovery and the optimal extraction conditions were evaluated by means of a factorial design. The use of this chemometric tool in analytical method development allows the identification of the principal and interaction effects of the extraction conditions on the recovery of pesticides. It also gives information about the location of pesticide maximum recovery with minimal experimental investment. Extraction was carried out with an ultrasonic bath and the experimental conditions studied included the volume of extractant, the time of extraction, the number of extraction steps and the sample weight. The sample was further cleaned up using a Florisil solid-phase extraction cartridge. For the overall extraction procedure, recoveries of 99 % for alpha-cypermethrin and 90 % for dimethoate from the spiked samples were found for 1 g of sample extracted three times with 35 mL hexane, sonicating for 2 min in each step. The complete process including ultrasonic extraction and filtration will not require more than 15-20 min, in contrast with several hours for conventional liquid-solid extraction techniques. The proposed method allows a high sample throughput, as commonly required in monitoring studies.