Ju_2026_Anal.Methods__

Carbamate pesticides are extensively employed in agricultural and public health, but their toxicity results from the inhibition of acetylcholinesterase, which can lead to poisoning in both humans and animals. In this study, a simple and rapid ultrasound-assisted dispersive liquid-liquid microextraction (UA-DLLME) method coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed and validated for the simultaneous determination of 22 carbamate pesticides and their metabolites in biological samples. The method exhibited excellent sensitivity, with limits of quantification (LOQ) determined to be 1.00 ng mL(-1), and showed good linearity (R(2) > 0.99) over the concentration range of 1.00-1000.00 ng mL(-1). Precision and accuracy met international bioanalytical guidelines, as indicated by intra- and inter-day relative standard deviation (RSD) below 15% and recoveries within acceptable limits. The method was successfully applied to authentic forensic cases involving human and animal poisonings, confirming its suitability for determining carbamate pesticides and their metabolites in complex matrices such as blood, liver, and urine. This robust and efficient analytical approach is well suited for applications in forensic investigations and clinical toxicology.