Determination of total acidic herbicide residues in Brazilian peanut products using QuEChERS with alkaline hydrolysis: occurrence, trade compliance, and dietary exposure assessment

Peanut, an important vegetal protein source, requires intensive weed control, usually with acidic herbicides. However, these pesticides undergo metabolic processes resulting in conjugated residues. Its analytical determination requires hydrolytic steps that increase analytical complexity, especially in high-lipid matrices. This study presents a QuEChERS method combined with alkaline hydrolysis for the determination of total acidic herbicides in peanut-derived products. Method tailoring via a fractional factorial design optimized the extraction conditions to 60 °C for 30 min without dispersive solid phase extraction as a cleanup, providing a streamlined workflow. The method validation revealed satisfactory performance: LOQ of 0.010 mg kg -1 , linear range of 0.010 to 0.200 mg kg -1 , recoveries between 66.1 to 117.4%, RSD < 20%, and expanded measurement uncertainty below 31.2%. In the occurrence analysis (n = 41, including peanut kernels, peanut butter, and paçoca), haloxyfop-P was the most prevalent analyte, with concentration of up to 0.040 mg kg -1 . Notably, 63% of positive results would have been underreported without hydrolysis. Dietary exposure assessments for Brazilian and Dutch populations revealed that the highest chronic and acute hazard quotients (up to 0.875% and 16.000%, respectively), meaning that well below the toxicological safety limit (100%), indicating no health risks. The proposed method serves as an efficient and practical tool for the fiscal routine monitoring of total acidic herbicides in peanut products, supporting both sanitary surveillance and trade compliance.