Science of Polymeric Materials, Department of Biomaterial Sciences, Graduate School of Agricultural and Life Sciences, The University of Tokyo, 1-1-1 Yayoi, Tokyo 113-8657, Japan.
Carbohydr Polym. 2013 Feb 15;92(2):1827-34. doi: 10.1016/j.carbpol.2012.11.043. Epub 2012 Nov 23.
Fully substituted glucomannan triacetate (GMTAc) (degree of substitution (DS)=3.0) was prepared from konjac glucomannan (KGM) treated with acetic acid and trifluoroacetic anhydride (TFAA). The peaks in the (1)H- and (13)C NMR spectra of GMTAc were assigned in detail based on two-dimensional (DQF-COSY, HSQC and HMBC) NMR analysis. Glucomannan acetate samples (GMAc) with different degrees of substitution (DS=1.3, 1.7, 2.0 and 2.8) were prepared by partial deprotection of GMTAc. Thermal properties of GMAcs including GMTAc were analyzed by differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). Their decomposition temperatures were higher than that of KGM, and increased with increase in DS. DSC measurements revealed that GMAc had a high glass transition temperature in the range of 178-219 °C, which decreased with increase in DS. The samples did not exhibit melting peaks, indicating that the GMAcs were amorphous. All GMAcs formed transparent films upon solvent casting, and tensile tests revealed that GMAc had a higher tensile strength and elongation to break at lower DS (1.3 and 1.7) compared to higher DS (2.0, 2.8 and 3.0). This means that the mechanical properties of GMAc could be controlled by DS.
完全取代的葡甘露聚糖三醋酸酯(GMTAc)(取代度(DS)=3.0)是由经过乙酸和三氟乙酸酐(TFAA)处理的魔芋葡甘露聚糖(KGM)制备的。根据二维(DQF-COSY、HSQC 和 HMBC)NMR 分析,详细分配了 GMTAc 的(1)H 和(13)C NMR 谱中的峰。通过 GMTAc 的部分脱保护,制备了具有不同取代度(DS=1.3、1.7、2.0 和 2.8)的葡甘露聚糖醋酸酯(GMAc)样品。通过差示扫描量热法(DSC)和热重分析(TGA)分析了包括 GMTAc 在内的 GMAcs 的热性能。它们的分解温度高于 KGM,并随 DS 的增加而增加。DSC 测量表明,GMAc 在 178-219°C 的范围内具有较高的玻璃化转变温度,该温度随 DS 的增加而降低。这些样品没有表现出熔融峰,表明 GMAcs 是无定形的。所有 GMAcs 在溶剂浇铸后形成透明薄膜,拉伸测试表明,与较高 DS(2.0、2.8 和 3.0)相比,较低 DS(1.3 和 1.7)的 GMAc 具有更高的拉伸强度和断裂伸长率。这意味着 GMAc 的机械性能可以通过 DS 来控制。