为合成高比表面积阿魏酸多孔淀粉酯(ferulic acid porous starch ester,FA-PS),探索其结构特性及体外消化性能,丰富食品级活性物质吸附剂及功能性递送载体材料的种类,该研究以溶剂交换法制备的多孔淀粉(porous starch,PS)为主体,阿魏酸(ferulic acid,FA)为酯化剂,在非水相体系中制备了取代度为0.150~0.885的FA-PS。扫描电子显微镜和N2-吸附/脱附结果表明,PS的比表面积为67.74 m2/g,平均孔径为20.23 nm,酯化改性后孔变得小而密集,FA-PS的比表面积可达到83.50 m2/g,平均孔径低至8.59 nm,可归属于介孔材料范畴。傅立叶变换红外光谱和13C固体核磁共振光谱证明FA和PS之间形成了酯键。X射线衍射显示PS处于非晶无序状态,而FA-PS发生晶型回生形成了新的结晶结构。FA-PS具备较强的抗氧化活性,酯化后水溶性得到改善,体外抗消化能力显著提升(P<0.05)。结果表明,FA-PS具备有效的纳米级多孔结构、高比表面积和较强的抗氧化活性,水溶性和体外消化抗性优于PS,可进一步运用于活性物质吸附及药物递送研究。
In this study, porous starch (PS), which was prepared by solvent exchange method, and ferulic acid (FA) were used to synthesis ferulic acid porous starch ester (FA-PS). FA-PS with high specific surface area, its structural characteristics and in vitro digestibility were explored, and the types of food-grade active material adsorbents and functional delivery carrier materials were studied. FA-PS with a degree of substitution of 0.150-0.885 were prepared in a non-aqueous system. Scanning electron microscope and N2-adsorption/desorption results showed that the specific surface area of PS was 67.74 m2/g and the average pore diameter was 20.23 nm. After esterification, the pores become smaller and densely distribute, the specific surface area of FA-PS could reach 83.50 m2/g and the average pore diameter was only 8.59 nm which indicating that PS and FA-PS could be classified as mesoporous materials. Fourier transform infrared spectroscopy and 13C solid state nuclear magnetic resonance confirmed the formation of ester linkage between FA and PS. X-ray diffraction showed that PS was in an amorphous and disordered state, while FA-PS undergone crystalline retrogradation to form a new crystalline structure. FA-PS had strong antioxidant activity, after esterification, the water solubility was improved and the in vitro digestion resistance was significantly enhanced (P<0.05). The results showed that FA-PS possessed an effective nano-scale porous structure, high specific surface area, strong antioxidant activity, and its water solubility and anti-digestion ability in vitro were better than PS. FA-PS can be further applied to active substance adsorption and drug delivery research.
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