This paper developed a new method with temperature controlled ionic liquid dispersive liquid-phase microextraction for the determination of pyrethroid insecticides such as fenpropathrin, fenvalerate and bifenthrin in water samples. The effect of alkyl chain length of ionic liquid 1-alkyl-3-methylimidazolium hexafluorophosphate and other parameters such as sample pH, temperature, salting-out effect and sample volume on the extraction efficiency were investigated in detail. Four different alkyl chain length ionic liquids ([CnMIM][PF6], n = 4, 6, 7, 8) were tested. The experimental results demonstrated that the alkyl chain length of ionic liquids (ILs) did have an important role on the extraction efficiency. The experimental results indicated that the longer alkyl chain length of ILs resulted in better extraction efficiency. Among the four ILs, 1-octyl-3-methylimidazolium hexafluorophosphate [C8MIM] [PF6] was the best one for extraction of the target analytes. Under the optimized conditions, three pyrethroid insecticides had limits of detection (LOD, S/N = 3) in the range of 0.34∼0.48 μg L−1. The precisions of the proposed method (RSDs, n = 6) with a spiked concentration of 20 μg L−1 were in the range of 2.0∼3.4%. The proposed method was evaluated with real water samples spiked at a concentration of 10 ng mL−1 and good spiked recoveries over the range of 89.2∼102.7% were obtained.
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