Development and validation of a UHPLC-MS/MS method for quantifying glyphosate and AMPA residues in canola oilseeds using FMOC-Cl derivatization

Glyphosate and its primary metabolite aminomethylphosphonic acid (AMPA) are herbicide residues of significant concern in agricultural products like canola oilseeds. This study developed and validated a sensitive UHPLC-MS/MS method with FMOC-Cl derivatization to quantify glyphosate and AMPA in canola oilseeds. The method demonstrated high linearity, with R² values of 0.9997 for glyphosate and 0.9996 for AMPA. Recovery rates were 83.09% for glyphosate and 82.28% for AMPA, indicating good accuracy and precision. The limits of detection (LOD) were 0.0009 mg/kg for glyphosate and 0.0004 mg/kg for AMPA, and the limits of quantification (LOQ) were 0.0031 mg/kg and 0.0014 mg/kg, respectively. Application to real samples from Dezful and Kermanshah showed higher seed (canola) residues in Kermanshah for both glyphosate and AMPA, whereas chaff residues were higher in Dezful. The method complies with international regulatory standards, including those of Codex Alimentarius and the European Union, providing a reliable tool for food safety monitoring and regulatory compliance. • FMOC-Cl derivatization enabled sensitive LC–MS/MS detection of glyphosate and AMPA. • Matrix-matched calibration ensured accuracy in oilseed (canola) matrices. • Method validated according to SANTE/11312/2021 guidelines. • Oilseed-specific challenges (lipids, co-extractives) were successfully managed. • Approach supports reliable monitoring of glyphosate/AMPA in edible oils and seeds.