A Rapid and Sensitive Method for the Analysis of Pyrethroid Pesticides Using the Combination of Liquid–Liquid Extraction and Dispersive Liquid–Liquid Microextraction

For the first time, combination of liquid–liquid extraction and dispersive liquid–liquid microextraction (LLE‐DLLME) is reported in this study. The method is efficient and was applied to the analysis of pyrethroid pesticides (fenpropathrin, sumithrin, cyhalothrin, permethrin, and deltamethrin) in fruit juices and fresh grape using gas chromatographic techniques with flame ionization detection system and mass spectrometric detection system. Five milliliter n‐hexane was used for the traditional liquid–liquid extraction of target analytes from 50 mL aqueous samples. After manual shaking, the supernatant phase (n‐hexane) was transferred into a test tube to which 0.75 mL dimethylformamide (DMF) was added then and the tube was shaken manually. After centrifugation, 0.6 mL of DMF was removed and used in a following DLLME procedure in which the extraction solvent was 20 μL of 1,1,2‐trichloroethane. Extraction with the optimized conditions resulted in linear analytical signals within the range 0.5–1200 μg L−1 and the limits of detection and quantification were in the ranges of 0.1–15 and 0.4–50 μg L−1, respectively. The method also showed high enrichment factors (2570–6835) and relatively good extraction recoveries (26–68%). Finally, the method was successfully applied to determination of analytes in tap water, strawberry juice, apricot juice, and fresh grape.