A rapid, environmentally friendly, and reliable method for pesticide analysis in high-fat samples

This report describes the development and validation of a simple, rapid, and efficient method in which solid-phase extraction followed by analysis in a gas chromatograph equipped with an electron capture detector (SPE-GC-ECD) is used for the simultaneous determination of dicofol, dieldrin, endosulfan, and permethrin in rat adipose tissue. This study targeted pesticides for which controversies exist regarding the harm that they may cause to humans, such as endocrine disruption or cancer, and that have also been found in recent years in vegetables consumed by the Brazilian population. The analytical procedure was optimised for SPE extraction and for GC-ECD conditions. The optimised method includes the extraction of the samples with n-hexane followed by an SPE procedure in which deactivated neutral alumina cartridges are used as the sorbent and a mixture of n-hexane:dichloromethane is used for elution. Recovery studies with spiked samples were used to evaluate the method's efficiency. Mean recoveries ranged from 75% to 119% with relative standard deviations (RSD)90%). ► This method is fast and reliable, adequate to application to a large set of samples. ► The matrix effect was achieved for all studied pesticides in rat adipose tissue. ► Pesticides were detected in 54% of the samples (n=125), even at low exposure doses. ► The bioaccumulation of cis-permethrin has not been described for similar studies.