A novel amphiphilic porous adsorbent material was prepared via micelle–emulsion polymerization for use as a solid-phase extraction (SPE) sorbent. In parallel, a fully automated SPE sampling device (LVED) was developed for on-site large-volume enrichment of trace contaminants in water. Using this newly developed device, an LVED–HPLC–MS/MS method was established for the rapid determination of 40 trace emerging contaminants in environmental water samples. The large-volume SPE conditions were systematically optimized, and method validation demonstrated good linearity (r² ≥ 0.992) and low limits of detection ranging from 0.002 to 0.10 ng/L. The method was applied to on-site enrichment and detection of emerging contaminants in real environmental water samples, with spiked recoveries for various contaminants ranging from 78.0% to 107%, and actual detected concentrations of some contaminants between 0.05 and 90.5 ng/L. This method represents a simple, rapid, and efficient approach for on-site large-volume extraction of trace emerging contaminants in environmental waters, showing broad application and promotion potential.

Emerging Contaminants, Trace Enrichment, In-situ Solid-phase Extraction