LC–MS/MS and GC–MS/MS Cross-Checking Analysis Method for 426 Pesticide Residues in Agricultural Products: A Method Validation and Measurement of Uncertainty

A method was developed to analyze residual pesticides in various vegetables using liquid chromatography-tandem mass spectrometry (LC-MS/MS) and gas chromatography-tandem mass spectrometry (GC-MS/MS). A method can analyze over 200 individual compounds, selectively separate peaks within 30 min, and meet various criteria such as those by the Codex Alimentarius Commission (CODEX). Most compounds showed recovery rates between 70 and 120%, and a relative standard deviation was within 20%. Measurement uncertainty, considering various influencing factors such as instrument precision, method sensitivity, experimental conditions, sample handling, and analytical procedures, was meticulously calculated. The expanded uncertainties of cross-checking 33 available pesticides ranged from 10.1 to 26.2 μg/kg at a confidence level of approximately 95%. Risk assessment of detected pesticides in agricultural products indicated a safety range of 0.00003-2.87240%. The developed method effectively analyzes diverse compounds simultaneously, contributing to agricultural product safety.