Preparation and evaluation of Fe3O4@C@NiCo-LDH@CDs composites for magnetic solid-phase extraction of trace endocrine disruptors†

Abstract

The widespread use of endocrine disruptors (EDPs) has certain potential hazards to organisms and environments, and it is particularly important to develop effective pretreatment methods before detection of EDPs in complex samples. In this work, a novel magnetic nanocomposite decorated with layered double hydroxides (LDHs) and carbon dots (CDs) was designed and prepared for magnetic solid-phase extraction (MSPE) of EDPs (bisphenol S, bisphenol F, bisphenol A, bisphenol AF, diethylstilbestrol and 4-cumylphenol) combined with high-performance liquid chromatography-ultraviolet (HPLC-UV) detection. The prepared composites were characterized by field emission scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR) and X-ray photoelectron spectroscopy (XPS), and the adsorption mechanism towards these EDPs might be mainly based on hydrogen bonds and π–π conjugation. Under the optimized conditions, the proposed method showed limits of detection within 0.05–0.50 μg L⁻¹ and limits of quantitation within 0.2–2.0 μg L⁻¹, and good linearity (R² ≥ 0.9975) was presented in the range of 0.2–200 μg L⁻¹. Finally, the Fe₃O₄@C@NiCo-LDH@CDs composite-based MSPE-HPLC-UV method was applied for enrichment and determination of EDPs in water, milk, and tea beverage samples with recoveries in the range of 81.2–119.8% and relative standard deviations below 9.7%.