Automated Dispersive Liquid–Liquid Microextraction (DLLME) for Rapid PFAS Analysis Across Environmental and Aquatic Matrices

Per- and Polyfluoroalkyl Substances (PFAS) in the Environment
Oral Presentation

Prepared by E. George1, B. Gauriat2, A. Ganci3, J. Garnier3
1 - Thermo Fisher Scientific, 355 River Oaks Parway, San Jose, California, 95134, United States
2 - Thermo Fisher Scientific, , , Courtaboeuf, France
3 - Thermo Fisher Scientific, , Courtaboeuf, , France


Contact Information: [email protected]; 408-300-4267

ABSTRACT

Per- and polyfluoroalkyl substances (PFAS) are widely distributed across environmental media, including water, soils, sediments, and aquatic organisms. Regulatory drinking water methods rely on solid-phase extraction (SPE), which is labor-intensive and not optimized for rapid, large-scale monitoring efforts. The objective of this work is to evaluate automated dispersive liquid–liquid microextraction (DLLME) as a high-throughput, non-regulatory sample preparation approach for PFAS analysis in environmental surveys requiring fast turnaround and large numbers of samples.

An automated DLLME workflow was applied to a range of environmentally relevant matrices, including drinking water, groundwater, surface water, wastewater, soils, sediments, industrial effluents with high dissolved solids, and fish tissue. DLLME integrates extraction, concentration, and cleanup into a single automated process using small sample volumes and less than 2 mL of organic solvent per sample, without cartridges or filtration. Sample preparation is performed under full robotic control, enabling unattended operation and consistent processing of mixed-matrix batches. Following extraction, PFAS are analyzed using EFOX-enabled LC-MS systems. Targeted quantitation is performed using either the TSQ Altis™ Plus EFOX Edition triple quadrupole mass spectrometer or the Orbitrap Exploris™ EFOX mass detector operating in full-scan high-resolution mode with accurate-mass extracted ion quantitation. The high-resolution workflow also enables confirmatory analysis and retrospective data review.

Across the matrices evaluated, DLLME-generated data demonstrated strong analytical performance using an extracted calibration approach, in which all calibration standards undergo the same extraction process. This strategy avoids the need for explicit recovery calculations while ensuring matrix-consistent quantitation. Matrix effects are therefore assessed relative to a clean water reference extracted under identical conditions. The workflow supports quantitation at environmentally relevant levels, including low part-per-trillion concentrations (sub-ng/L to tens of ng/L) in water matrices and low ng/kg to low µg/kg levels in solids and fish tissue. While DLLME is not included in current EPA drinking water regulatory methods, these results demonstrate its value as a rapid and scalable approach for PFAS surveillance in site investigations and environmental monitoring programs.