Etminanrezaeiye Sara, Rezazadeh Khadije, Jalilnejad Elham, Rafiee Reza
Faculty of Chemical Engineering, Urmia University of Technology, Urmia, Iran.
Sci Rep. 2025 Jul 8;15(1):24450. doi: 10.1038/s41598-025-07588-0.
This study focuses on the synthesis and structural analysis of biocomposites comprising chitosan (Cs), hydroxyapatite (HA), and pectin (Pe). Cs was extracted from shrimp skin, HA from bovine teeth and bones, and Pe from orange peel and apple. The biocomposites were prepared via a freeze-drying method using glutaraldehyde (GA) as a cross-linking agent. FTIR, XRD, FE-SEM, EDS-EDAX and BET were employed to characterize the chemical structure, crystallinity, morphology, surface area, and elemental composition. The extracted Cs had a molecular weight of 4.1 × 10⁵ Da, a 70% degree of deacetylation, and an extraction yield of 31.2%. The results confirmed biocomposite formation with a near-stoichiometric Ca/P ratio (1.67) in HA. Biocomposites containing HA calcined at 1000 °C and Pe from orange peel with 72% galacturonic acid, exhibited enhanced crystallinity (up to 70.61%), uniform dispersion, and high porosity. While an increased HA content improved morphology and surface area (up to 12.5 m/g), it also reduced crystallinity after reaching the maximum point, possibly due to weakened intermolecular interactions between Cs and Pe.
本研究聚焦于壳聚糖(Cs)、羟基磷灰石(HA)和果胶(Pe)组成的生物复合材料的合成与结构分析。Cs从虾壳中提取,HA从牛牙和骨头中提取,Pe从橙皮和苹果中提取。生物复合材料通过冷冻干燥法制备,使用戊二醛(GA)作为交联剂。采用傅里叶变换红外光谱(FTIR)、X射线衍射(XRD)、场发射扫描电子显微镜(FE-SEM)、能谱仪-能量色散X射线分析(EDS-EDAX)和比表面积分析仪(BET)来表征化学结构、结晶度、形态、表面积和元素组成。提取的Cs分子量为4.1×10⁵ Da,脱乙酰度为70%,提取产率为31.2%。结果证实了在HA中形成了钙磷比接近化学计量比(1.67)的生物复合材料。含有在1000℃煅烧的HA和来自橙皮且半乳糖醛酸含量为72%的Pe的生物复合材料表现出增强的结晶度(高达70.61%)、均匀分散和高孔隙率。虽然增加HA含量改善了形态和表面积(高达12.5 m/g),但在达到最大值后也降低了结晶度,这可能是由于Cs和Pe之间的分子间相互作用减弱所致。