Determination of Trace Phthalates in Foods by C18-SiO2@C-Tip Solid-Phase Microextraction Coupled with Gas Chromatography-Mass Spectrometry
A novel core-shell composite adsorbent, C18-SiO2@C, was synthesized for the determination of five phthalates in food samples. The adsorbent was prepared by assembling hexamethylcyclotrisiloxane (D3) into γ-cyclodextrin (γ-CD) cavities via saturated solution method, followed by hydrothermal oxidation to form SiO2@C, and subsequent C18 modification on the inner SiO2 core. The outer hydrophilic amorphous carbon shell enables effective extraction, while the inner C18 layer provides hydrophobic interactions. Using tip-based solid-phase microextraction (SPME), the adsorbent (10 mg) efficiently enriched phthalates from water, milk, and cola. Under optimized conditions (pH, eluent type/volume, sample volume, salt concentration), the method coupled with GC/MS exhibited linearity in the range of 0.5–10 ng·mL−1 (R² > 0.99), limits of detection (S/N ≥ 3) of 0.04–0.15 μg·L−1, and spiked recoveries of 74%–100% (RSD 1.32%–3.49%). For real samples, recoveries were 84.6%–102.3% for tap water, 80.7%–104.6% for cola, and 80.2%–101.4% for milk. The method offers simplicity, rapidity, low sample consumption, high enrichment efficiency, and strong matrix interference resistance, demonstrating significant potential for trace phthalate monitoring in foods.