Ultrasound-Assisted Dispersive Solid-Phase Filter Extraction Coupled with Green Supercritical Fluid Chromatography...

The migration of hindered phenolic antioxidants from food contact materials (FCMs) into foodstuffs poses health risks due to endocrine disruption and organ toxicity. Hence, the development of a high-efficiency analytical method for hindered phenolic antioxidants is of great importance for food safety. This study developed a novel ultrasound-assisted dispersive solid-phase filter extraction (d-SPFE) coupled with green supercritical fluid chromatography (SFC) method for the simultaneous determination of six representative hindered phenolic antioxidants. Under optimized conditions, the method achieved high extraction efficiency, with the complete separation of all analytes within 10 min. A wide linearity range (0.02-2.0 μg/mL) was achieved, with coefficients of determination all greater than 0.9996. The limits of detection (LOD, S/N = 3) and limits of quantification (LOQ, S/N = 10) were 2.4-3.6 ng/mL and 8-12 ng/mL, respectively. Validation tests demonstrated precise spiked recoveries (89.4-101.6%), with intra-day and inter-day relative standard deviations (RSDs) all less than 10%. The d-SPFE-SFC synergy significantly outperforms conventional techniques in terms of analysis speed and eco-efficiency. Successful application to food simulants confirms its reliability in monitoring hindered phenolic antioxidant migration from FCMs. This green and rapid methodology will enable the direct assessment of migration risks.