Optimization of a QuEChERS-LC-MS/MS method for 51 pesticide residues followed by determination of the residue levels and dietary intake risk assessment in foodstuffs

Abstract

A modified QuEChERS purification-liquid chromatography-tandem mass spectrometry method has been developed to determine 51 pesticide residues with newly established maximum residue limits (MRLs) in foodstuffs. Samples were extracted with acetonitrile under citrate-buffered conditions and purified using a modified QuEChERS method employing hydroxylated MWCNTs, SAX, and C₁₈. The limits of quantification ranged from 0.2 to 9.8 µg/kg. Recoveries in ten different foodstuffs ranged from 70.2% to 117.9%, with relative standard deviations between 2.3% and 19.9% at three spiking levels. This method was applied to analyze 352 market samples, detecting 14 pesticides in 97 samples. Notably, Afidopyropen, cyantraniliprole, and fluxapyroxad residues in vegetables exhibited a consistent pattern of higher levels in the spring and winter and lower levels in the summer and autumn. Moreover, the risk assessments for acute and chronic dietary exposure to the 14 detected pesticides indicated that the %ADI and %ARfD were well below 100%.

Keywords: Dietary intake risk assessment; Hydroxylated MWCNTs; LC-MS/MS; Pesticide residues; QuEChERS; Residue level analysis.