Application of Rice Husk-Derived SBA-15 Bifunctionalized with C18 and Sulfonic Groups for Solid-Phase Extraction of Tropane, Pyrrolizidine, and Opium Alkaloids in Gluten-Free Bread

Rice husk (RH), a globally abundant agri-food waste, presents a promising renewable silicon source for producing SBA-15 mesoporous silica-based materials. This study aimed to synthesize and bifunctionalize SBA-15 using RH as a silica precursor, incorporating sulfonic and octadecyl groups to create a mixed-mode sorbent, RH-SBA-15-SO₃H-C18, with reversed-phase and cation exchange properties. The material's structure and properties were characterized using advanced techniques, including X-ray diffraction, infrared spectroscopy, N₂ adsorption-desorption isotherms, nuclear magnetic resonance, and electron microscopy. These analyses confirmed an ordered mesoporous structure with a high specific surface area of 238 m²/g, pore volume of 0.45 cm³/g, pore diameter of 32 Å, and uniform pore distribution, highlighting its exceptional textural qualities. This sorbent was effectively utilized in solid-phase extraction to purify 29 alkaloids from three families-tropane, pyrrolizidine, and opium-followed by an analysis using ultra-high performance liquid chromatography coupled to ion-trap tandem mass spectrometry. The developed analytical method was validated and applied to gluten-free bread samples, revealing tropane and opium alkaloids, some at concentrations exceeding regulatory limits. These findings demonstrate that RH-derived RH-SBA-15-SO₃H-C18 is a viable, efficient alternative to commercial sorbents for monitoring natural toxins in food, offering a sustainable solution for repurposing agri-food waste while addressing food safety challenges.