Rapid Determination of 13 Insecticides and Acaricides in Human Blood Using Dispersive Liquid–Liquid Microextraction Coupled With DART‐MS/MS

ABSTRACT A high‐throughput, solvent‐minimized analytical method was developed by coupling dispersive liquid–liquid microextraction (DLLME) with direct analysis in real‐time tandem mass spectrometry (DART‐MS/MS) for the simultaneous quantification of multiple insecticides and acaricides in human blood. This method obviates the need for chromatographic separation, substantially reducing total analysis time. Extraction conditions were systematically optimized to achieve efficient enrichment of target analytes from complex biological matrices. The method exhibited good linearity across compound‐specific calibration ranges ( R 2 = 0.9912–0.9993) with limits of quantification as low as 0.1 ng/mL. Recoveries ranged from 78.2% to 110.7%, while matrix effects remained within ±25%. Both intraday and interday precisions met commonly accepted validation criteria (RSD < 20%). Excellent agreement with HPLC‐MS/MS results confirmed the method's analytical reliability. Although tested on a limited number of samples, the method demonstrated robust performance in two real‐case blood samples and four spiked samples, highlighting its practical potential for the rapid screening and exposure assessment of insecticides and acaricides in time‐sensitive forensic casework.