Validation of multi-residue method for determination of pesticides in meat products using official guideline of analytical methods in Japan

A multi-residue analytical method for 185 pesticides (including metabolites) in meat products was validated by the guideline of the Japanese Ministry of Health, Labour and Welfare. This method involved extraction with ethyl acetate–cyclohexane (1 : 1) and cleanup by gel permeation chromatography (GPC), and primary secondary amine (PSA) and silica-gel mini-column solid-phase extraction (SPE). The target compounds were determined by gas chromatography/mass spectrometry (GC-MS) and liquid chromatography/mass spectrometry (LC-MS). Validation tests were performed on beef, chicken and pork muscles fortified at 0.01 and 0.10 μg/g. Among 185 pesticides tested, 175 in beef, 175 in chicken and 172 in pork were found to conform to the guideline when the solvent standard was used, and 181 in beef, 176 in chicken and 177 in pork when the matrix-matched standard was used. Although significant matrix effects were not observed for most pesticides, use of the matrix-matched standard was preferable for accurate quantitation to the solvent standard. Limits of quantitation (S/N ≥10) were set at 0.01 μg/g for all pesticides. The method was applied to the regulatory monitoring of meat products.