An Integrated Strategy for Purification by Combining Solid-Phase Extraction with Dispersive-Solid-Phase Extraction for Detecting 22 Pesticides and Metabolite Residues in Fish.

A robust isotope-labeled internal standard method was established for the detection of 22 pesticides and metabolite residues in four kinds of fish; two were from freshwater fish, and two were from marine fish. Pesticides with wide application possibilities in rice in China, strong leaching to water, or high bioconcentration factors (BCF) in fish were selected. The samples were extracted with 1% acetic acid-99% acetonitrile. The extracts were first purified by solid-phase extraction (PEP-plus), cleaned with dispersive-solid-phase extraction (PSA and C18), and finally analyzed by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The results showed that good linearities for the target compounds were observed in the range of 0.1-100 ng/mL, and the correlation coefficient (R2) of each compound was greater than 0.99. The recoveries of the method were within 70-120% with RSDs <20% at three different spiked concentration levels (0.5, 5, and 100 ng/g). The quantitative limit of the method was 0.5-5 ng/g. The method is shown to be sensitive and accurate and can meet the demands for the quantitative analysis of pesticides in fish.