Simultaneous determination of multi-pesticide residues in fish and shrimp using dispersive-solid phase extraction with liquid chromatography-tandem mass spectrometry

In this work, we developed and optimized an analytical method for the simultaneous determination of multi-pesticide residues in fishery products using dispersive-solid phase extraction and liquid chromatography-tandem mass spectrometry (LC-MS/MS). We selected 66 pesticides (insecticide, fungicides, and herbicides) and determined their residue concentrations in fish and shrimp. The samples were prepared according to the modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) procedure. Matrix-matched calibrations were carried out at three different spiking levels in flatfish, eel, and shrimp. The validation procedure was performed to determine the accuracy, precision, limits of detection, and limit of quantification (LOQ) according to the Codex guidelines (CAC/GL-71). Consequently, the proposed method is satisfactory in terms of accuracy (recoveries between 70 and 125%), precision (relative standard deviation below 20%). The matrix effects were between -98.1 and 48.6% in flatfish, eel, and shrimp. LOQs of this method was below 10 mu g kg(-1). The proposed method was applied to investigate the pesticide residue levels of fresh fish and shrimp samples (n = 78) obtained from domestic markets in Korea. As a result, 10 samples was positive (12.8%) for the 66 targeted pesticides. Based on our results, the developed method was successfully applied for the detection and quantification of pesticide residues in fish and shrimp.

Automated summary

In this study, an analytical method for the simultaneous determination of multi-pesticide residues in fishery products was developed and optimized using dispersive-solid phase extraction and liquid chromatography-tandem mass spectrometry (LC-MS/MS). The method was validated for accuracy, precision, and limits of detection according to Codex guidelines, showing satisfactory results. The proposed method successfully detected and quantified pesticide residues in fresh fish and shrimp samples obtained from domestic markets in Korea.