A salting-out assisted liquid–liquid extraction (SALLE) combined with gas chromatography-mass spectrometry (GC–MS) method was developed for the determination of four pyrethroid insecticides (PYRs) in high salinity and biological samples. Several parameters including sample pH, salting-out solution volume and salting-out solution pH influencing the extraction efficiency were systematically investigated with the aid of orthogonal design. The optimal extraction conditions of SALLE were: 4 mL of salting-out solution with pH = 4 and the sample pH = 3. Under the optimum extraction and determination conditions, good responses for four PYRs were obtained in a range of 5–5000 ng/mL, with linear coefficients greater than 0.998. The recoveries of the four PYRs ranged from 74% to 110%, with standard deviations ranging from 1.8% to 9.8%. The limits of detection based on a signal-to-noise ratio of 3 were between 1.5–60.6 ng/mL. The method was applied to the determination of PYRs in urine, seawater and wastewater samples with a satisfactory result. The results demonstrated that this SALLE-GC–MS method was successfully applied to determine PYRs in high salinity and biological samples. SALLE avoided the need for the elimination of salinity and protein in the sample matrix, as well as clean-up of the extractant. Most of all, no centrifugation or any special apparatus are required, make this a promising method for rapid sample preparation procedure.Graphical abstract
A salting-out assisted liquid–liquid extraction (SALLE) combined with gas chromatography-mass spectrometry (GC–MS) method was successfully developed for simultaneous determination of four pyrethroid insecticides (PYRs) including bifenthrin, permethrin, β-cyfluthrin and fenvalerate in high salinity and biological samples.