Optimizing the QuEChERS method for efficient monitoring of fipronil, thiobencarb, and cartap residues in paddy soils with varying properties.

Abstract

This study aims to optimize the QuEChERS methodology for extracting three pesticides (fipronil, thiobencarb, and cartap) from two paddy soils with distinct characteristics. Various modifications were explored to enhance extraction efficiency, employing acetonitrile (MeCN) or ethyl acetate (EtOAc) for extraction and primary-secondary amine (PSA) and graphitized carbon black (GCB) for the clean-up. Assessment criteria included accuracy, precision, linearity, detection limits, uncertainty, and matrix effects. Results revealed that the clayey soil with lower organic carbon (OC) content (1.26%) and 100% moisture yielded the highest pesticide recoveries (113.72%, 115.73%, and 116.41% for FIP, THIO, and CART, respectively). In contrast, the silty clayey soil with higher OC content (2.91%) and 20% water content exhibited poor recoveries (< 60%). FIP and CART demonstrated better recoveries with MeCN, while THIO performed better with EtOAc under specific moisture conditions. Clean-up sorbents significantly reduced FIP and CART recoveries, with THIO recoveries less affected. Acidifying with HCl substantially improved CART recovery. EtOAc introduced a moderate to strong matrix effect for FIP and THIO, while MeCN in soils with 100% moisture resulted in a strong matrix effect for CART. The study highlighted the substantial impact of extraction conditions, pesticide properties, and soil conditions on the outcomes of the QuEChERS method. A comprehensive understanding of these interplays was deemed crucial for accurately quantifying pesticide residues in agricultural soils.