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中国精品科技期刊2020

辛烯基琥珀酸-脱乙酰魔芋葡甘露聚糖酯的制备工艺优化及结构表征

Preparation Optimization and Structural Characterization of Octenylsuccinated Deacetylated Konjac Glucomannan

  • 摘要: 以脱乙酰魔芋葡甘露聚糖凝胶颗粒(deacetylated konjac glucomannan gel,DK-G)为原料,辛烯基琥珀酸酐(octenyl succinic anhydride,OSA)为酯化剂,制备高吸油性辛烯基琥珀酸脱乙酰魔芋葡甘露聚糖酯材料(deacetylated konjac glucomannan octenyl succinate gel,DK-OS)。采用Box-Behnken试验设计研究反应温度、pH、DK-G浓度、OSA与DK-G质量比(mOSA/mDK-G)4个因素对DK-OS取代度和吸油率的影响,优化工艺条件,随后在最佳条件下制备高吸油率和取代度的DK-OS,并对该材料进行红外光谱、结晶结构、疏水性及微观形貌表征。结果表明,4个因素对DK-OS吸油率的影响大小顺序为mOSA/mDK-G>pH>反应温度>DK-G浓度,对取代度的影响大小顺序为mOSA/mDK-G>DK-G浓度>pH>反应温度,酯化最佳工艺为:反应温度39 ℃,pH8.5,DK-G浓度2%,mOSA/mDK-G=1.9,反应时间4 h,在此条件下获得的DK-OS取代度为0.0623±0.0002,吸油率为53.88±0.02 g/g。红外光谱结果表明DK-OS在1727 cm−1(酯基)处峰强度增强,同时在2926、2857、1566 cm−1处出现亚甲基拉伸振动峰和羧酸盐不对称伸缩振动峰;同时观察到DK-OS微观结构表面有孔洞形成且变粗糙,但酯化物晶型未受影响;酯化后其水接触角从61.5°增加至105.3°,表面疏水性明显增加。该研究可为高吸油性膳食纤维的制备提供技术参考。

     

    Abstract: In this study, highly oil-absorbing deacetylated konjac glucomannan octenyl succinate gel (DK-OS) was prepared using deacetylated konjac glucomannan gel (DK-G) as the raw material and octenyl succinic anhydride (OSA) as the esterifying agent. The Box-Behnken experimental design was employed to investigate the effects of four factors (reaction temperature, pH, DK-G concentration, and OSA and DK-G mass ratios mOSA/mDK-G) on the degree of substitution (DS) and oil absorption capacity (OAC) of DK-OS. To optimize the process conditions, DK-OS with high OAC and DS was prepared under optimal conditions. The DK-OS was further characterized via infrared spectroscopy, crystalline structure analysis, hydrophobicity assessment, and microscopic morphology. The influence of the four factors on the OAC of DK-OS followed the order of mOSA/mDK-G>pH>reaction temperature>DK-G concentration, whereas the order of influence on DS was mOSA/mDK-G>DK-G concentration>pH>reaction temperature. The optimal conditions for the esterification process were 39 °C, pH8.5, 2% DK-G concentration, mOSA/mDK-G=1.9, and 4 h reaction time. Under these conditions, the resulting DK-OS exhibited a DS of 0.0623±0.0002 and an OAC of 53.88±0.02 g/g. Infrared spectroscopy revealed that the peak intensity of DK-OS at 1727 cm−1 (associated with the ester group) was enhanced after esterification. Additionally, methylene stretching vibration peaks and carboxylate asymmetric stretching vibration peaks were observed at 2926, 2857, and 1566 cm−1, respectively. Notably, the pores that developed on the microstructural surface of DK-OS exhibited increased roughness, whereas the crystal form of the esterified product remained unchanged. The hydrophobic angle increased significantly from 61.5° to 105.3°, thereby reflecting a marked enhancement in surface hydrophobicity. This study provides a technical reference for the development of high-oil-absorption dietary fibers.

     

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