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...

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Main Authors: Fernando L. Vera-Baquero, Judith Gañán, Natalia Casado, Damián Pérez-Quintanilla, Sonia Morante-Zarcero, Isabel Sierra
Format: Article
Language:English
Published: MDPI AG 2025-03-01
Series:Foods
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Online Access:https://www.mdpi.com/2304-8158/14/7/1156
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Summary: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-SO<sub>3</sub>H-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, N<sub>2</sub> adsorption–desorption isotherms, nuclear magnetic resonance, and electron microscopy. These analyses confirmed an ordered mesoporous structure with a high specific surface area of 238 m<sup>2</sup>/g, pore volume of 0.45 cm<sup>3</sup>/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-SO<sub>3</sub>H-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.
ISSN:2304-8158