Analysis of sediment-associated insecticides using ultrasound assisted microwave extraction and gas chromatography–mass spectrometry

An ultrasound assisted microwave extraction (UAME) method was developed to simultaneously extract five organophosphate (OP) and eight pyrethroid insecticides from sediment. The optimized UAME conditions were to use 100 ml of a mixture of hexane and acetone (1:1, v/v) solution as the extraction solvents, and extraction time, microwave and ultrasonic power settings of 6 min, 100 W and 50 W, respectively. Extracts were cleaned using solid phase extraction and analyzed by gas chromatography–mass spectrometry in negative chemical ionization mode and quantification was based on matrix-matched standard solutions along with internal standard calibration. At the spiked concentrations of 1, 5 and 20 ng/g dry weight (dw), recoveries of OPs were 77.6–122%, 65.2–128% and 75.6–141% with relative standard deviations (RSDs) of 10.6–18.1%, 3.1–12.5% and 8.0–35.3%, respectively, while recoveries of pyrethroids were 78.0–101%, 76.4–104% and 71.0–99.5% with RSDs of 10.3–23.5%, 4.7–17.6% and 8.8–18.7%, respectively. Method detection limits ranged from 0.31 to 0.45 ng/g dw for the OP insecticides and from 0.27 to 0.70 ng/g dw for the pyrethroid insecticides. The newly developed UAME method was validated by comparing it to Soxhlet and sonication extraction methods. Better recoveries were achieved for most OPs by the novel UAME method, whereas there was no significant difference in recoveries for most of the pyrethroids. Finally, the UAME method was used to quantify the target insecticides in field-contaminated sediment samples which were collected in Guangzhou, China.