Analytical Method Development for Multiresidue Determination in Water Using Automated Parallel Dispersive Pipette Extraction and HPLC-DAD

Abstract

This work presents an automated parallel dispersive pipette extraction (Au-Pa-DPX) technique for analyzing nine organic compounds from different classes in river water. Separation and detection were performed using high performance liquid chromatography with diode array detector (HPLC-DAD). Sample preparation involved optimizing desorption and extraction parameters. The optimized methodology involves: acetonitrile (ACN) as the desorption solvent, with three desorption cycles.The optimized pH was 8, nine extraction cycles were employed, and no salt was added. To prevent carry-over effects, four cleaning cycles were performed on the DPX pipette tips. The Au-Pa-DPX method demonstrated a coefficient of determination (R 2 ) ranging from 0.9984 to 0.9998. Limits of detection (LODs) were between 0.33 and 1.67 μg L -1 , while limits of quantification (LOQs) varied from 1.00 to 5.00 μg L -1 . Interday precision ranged from 6.85% to 18.35%, whereas intraday precision fluctuated between 0.96% and 9.50%. The proposed method achieved relative recovery values between 89.88% and 125.56%. The enrichment factors ranged from 27.56 to 43.38. Compared to existing methods, Au-Pa-DPX is an environmentally friendly alternative, offering high throughput, reduced solvent and sample consumption, and lower waste production. This study highlights the importance of multiclass analyses for environmental monitoring.