Rapid Screening of 25 Environmental Hormones in Aquatic Products Using QuEChERS‐Combined With Dispersive Liquid–Liquid Microextraction Based on Solidification of Floating Organic Droplet Coupled With UHPLC‐Q/Orbitrap HRMS

ABSTRACT An innovative analytical method integrating QuEChERS with dispersive liquid–liquid microextraction using solidified floating organic droplets (DLLME‐SFO) and ultra‐high‐performance liquid chromatography‐quadrupole/orbitrap high‐resolution mass spectrometry (UHPLC‐Q/Orbitrap HRMS) was developed for the rapid screening of 25 environmental hormones (EHs) in aquatic products. The method systematically optimized key parameters, including extraction solvent selection (1‐undecanol), water volume (5 mL), pH (native pH 6.5), adsorbent combination (C18/PSA, 20 mg each), and salt addition (0% NaCl), achieving high sensitivity with detection limits of 0.1–0.4 µg/kg and recoveries of 68.2%–112.8%. The method demonstrated excellent linearity ( R 2 > 0.995) across a concentration range of 0.4–40 µg/kg, with precision (intra‐ and inter‐day RSDs < 15%) and manageable matrix effects (−19.5% to 10.9%). The environmental impact assessment, conducted using the Analytical GREEnness Metric for Sample Preparation (AGREEprep score: 0.59) and Blue Applicability Grade Index (BAGI score: 80), confirmed that the proposed method satisfies both sustainability and practicality criteria for EHs analysis. Enhanced matrix purification and dual‐polarity HRMS detection enabled accurate identification and quantification of structurally diverse EHs, including pesticides and pharmaceuticals. Validated in 60 commercial samples, the method detected prometryn residues in 11.7% of cases, demonstrating its practicality for monitoring EH contamination in complex aquatic matrices. This approach represents a significant advancement in multi‐residue analysis, combining efficiency, sensitivity, and environmental compatibility.