Akademik Veri Yönetim Sistemi
Microchemical Journal, cilt.215, 2025 (SCI-Expanded)
Pesticides are a long-standing food safety and ecological concern for human health. Therefore, accurate and sensitive determination of pesticide residues before consumption is an important issue. In this study, the d-SPE step of the QuEChERS method was modified using a novel nitrogen-doped graphene-coated FexOy (Fe-N-GN) synthesized by solvothermal method. Optimization of the d-SPE step and chromatographic method, linearity, detection and quantification limits, inter- and intra-day recovery studies were carried out with a total of 40 representing pesticides belonging to carbamate, organophosphorus and triazole groups in challenging arugula and black mulberry matrices by liquid chromatography-tandem mass spectrometry. Satisfactory interference removal and method performance results were obtained using Fe-N-GN and also compared with GCB results. The LOQ values of studied pesticides were calculated between 0.001 mg kg−1 to 0.010 mg kg−1 with a satisfying correlation coefficient (R2 > 0.99). The overall average recoveries ranged from 73.3 % to 113.4 % for arugula and 72.3 % to 112.1 % for black mulberry, with RSDs < 14 %, that means all results met the criteria of the SANTE document with low detection limits. Furthermore, the amount of Fe-N-GN used was reduced by 33 % for arugula and 60 % for black mulberry compared to the GCB used in QuEChERS EN 15662 and the Fe-N-GN is more economical regard to GCB. Total binding affinities of pesticides were also calculated and a relationship between affinity and recovery was also confirmed by pesticide-surface model studies. Fe-N-GN is expected to be an economical and effective alternative for pesticide analysis in complex matrices. The greenness of the method was evaluated by Green Analytical Procedure Index and Analytical Eco-Scale tools, and found as excellent according to the Analytical Eco-Scale.