Customized dispersive micro-solid-phase extraction device combined with micro-desorption for the simultaneous determination of 39 multiclass pesticides in environmental water samples

Abstract

A dispersive micro-solid phase extraction (d-µ-SPE) procedure was developed for the simultaneous extraction of 39 multiclass pesticides, containing a variety of chemical groups (organophosphate, organochlorine, pyrethroid, strobilurin, thiocarbamate, triazole, imidazole, and triazine), from water samples. A customized d-µ-SPE glass device was combined with a multi-tube platform vortex and a micro-desorption unit (Whatman Mini-UniPrep G2 syringeless filter), which allowed the unique simultaneous desorption, extract filtration, and injection. A simplex-centroid mixture design and Doehlert design were employed to optimize the extraction conditions. The optimized extraction conditions consisted of an extraction time of 30 min, an addition of 6.74 % of NaCl into 100 mL of water sample, and a desorption time of 24 min with 500 µL of EtAc. The procedure provided a low limit of detection (LOD), ranging from 0.51 ng L−1 (4,4-DDE) to 22.4 ng L−1 (dimethoate), and an enrichment factor ranging from 72.5 (dimethoate) to 200 (tebuconazole). The relative recoveries of the pesticides from spiked freshwater and seawater ranged from 74.2 % (endrin) to 123 % (molinate). The proposed procedure was applied to detect the presence of multiclass pesticides in environmental water samples. Three pesticides commonly applied in Brazil, namely, malathion, dimethoate, and lambda-cyhalothrin, were detected in concentrations ranging from <LOD to 120 ng L−1 (dimethoate).