In-syringe low-density ionic liquid dispersive liquid–liquid microextraction for the fast determination of pyrethroid insecticides in environmental water samples by HPLC-DAD

Abstract

A new microextraction technique named in-syringe low-density ionic liquid dispersive liquid–liquid microextraction (LDIL-DLLME) followed by separation using high performance liquid chromatography has been developed to determine the levels of four pyrethroid insecticides (i.e., deltamethrin, fenvalerate, permethrin, and bifenthrin) in environmental water samples. In the developed method, an ionic liquid (IL) was used for the first time instead of an organic solvent, which is most often used in low-density solvent-based microextraction methods. The IL was placed in a long syringe needle using a microsyringe. It was then dispersed by drawing the sample solution into the syringe. The extraction was finished in the syringe, taking full advantage of the low-density property, and making this method easier and quicker. Several parameters affecting the experimental efficiency of LDIL-DLLME, such as the needle's inner diameter, salt addition, the volume of IL and sample, rotation speed and duration of centrifugation and ultrasound were thoroughly studied. Under optimized conditions, in the range of 1 to 500 μg L⁻¹, good linearity was obtained, with coefficients of determination greater than 0.9994. Three spiked water samples were studied, and recovery ranged from 88.0 to 102.8%, with relative standard deviations (RSDs) ranging from 0.3 to 6.7%. The limits of detection (LODs) for the four pyrethroid insecticides were in the range of 0.88–1.71 μg L⁻¹ and enrichment factors (EFs) were in the range of 242 to 257. The proposed method provides an inexpensive, rapid, simple and eco-friendly process for evaluating pyrethroid insecticides in environmental samples, making it a potential method for the pretreatment of experimental samples.