Copper clean-up procedure for ultrasonic extraction and analysis of pyrethroid and phenylpyrazole pesticides in sediments by gas chromatography-electron capture detection

A rapid ultrasonic extraction method coupled with a heated-copper clean-up procedure for removing interfering constituents was developed for analyzing pyrethroid and phenylpyrazole pesticides in sediments. Incubation of the 60 mL extract with 12 g copper granules at 60 oC for 2 h was determined to be the optimal conditions for removing the interfering constituents. Eleven pyrethroid and phenylpyrazole pesticides were spiked into sediment samples to determine the effectiveness of the ultrasonic extraction method. The average recoveries of pyrethroids and phenylpyrazoles in sediment at 4 oC storage on day 0, 1, 7, 14, and 21 ranged from 98.6 to 120.0%, 79.2 to 116.0%, 85.0 to 119.7%, 93.6 to 118.7%, and 92.1 to 118.2%, respectively, with all percent relative standard deviations less than 10% (most < 6%). This illustrated the stability of pyrethroids and phenylpyrazoles in sediment during sediment aging at 4 oC. Recoveries of the pesticides ranged from 98.6% to 120.0% for lowest fortification level (2-16 μg kg-1), from 97.8% to 117.9% for middle fortification level (10-80 μg kg-1), and from 94.3% to 118.1% for highest fortification level (20-160 μg kg-1). Relative standard deviations of pesticide recoveries were usually less than 7%. Method detection limits of target pesticides ranged from 0.22 μg kg-1 to 3.72 μg kg-1. Furthermore, field sediment samples collected from four residential lakes during a three-month monitoring period were analyzed to evaluate the effectiveness of this method. Bifenthrin was detected in all of sediment samples (highest concentration 260.33 ± 41.71 μg kg-1, lowest concentration 5.68 ± 0.38 μg kg-1), and fipronil sulfone was detected at least once in sediment samples collected from three sites with concentrations ranging from 1.73 ± 0.53 to 7.53 ± 0.01 μg kg-1. - Highlights: → A rapid extraction and copper-based clean-up method was developed. → Recoveries after storage at 4 oC for 21 d ranged from 79.2 to 120.0%. → Percent relative standard deviations less than 10% (most < 6%). → Recoveries ranged from 94.3% to 120.0% at three fortification levels. → Method detection limits ranged from 0.22 μg kg-1 to 3.72 μg kg-1.