Yanli Wang, Wenyuan Gao, Xia Li
School of Pharmaceutical Science and Technology, Tianjin University, Tianjin 300072, China.
Carbohydr Res. 2009 Sep 8;344(13):1764-9. doi: 10.1016/j.carres.2009.06.014. Epub 2009 Jun 21.
Carboxymethyl starch (CMS) was obtained as a product of the reaction of starch and monochloroacetic acid (MCA) in the presence of sodium hydroxide. The influence of the molar ratio of NaOH/AGU, the molar ratio of MCA/AGU, the reaction time, reaction temperature, and the water content on the degree of substitution (DS) was studied. The optimal molar ratio of NaOH/AGU and MCA/AGU is 2.4 and 1.0, respectively. Increase of the ratio of NaOH/AGU or MCA/AGU leads to an increase in DS, but only to certain extent. The highest values of the DS were obtained when the carboxymethylation was performed at 60 degrees C for 2.5 h. The water content in the reaction media ethanol was optimal at 20% (v/v). The scanning electron micrographs (SEMs) revealed that the carboxymethylation affected the structural arrangement of the starch and caused granular disintegration. The particle size distribution (PSD) also displayed that the average particle diameter increased greatly after modification from 37.37 microm to 72.88 microm. Wide angle X-ray diffractometry (XRD) revealed that starch crystallinity was obviously reduced after carboxymethylation. The new bands at 1600 cm(-1) and 1426 cm(-1) in FT-IR indicated that the starch granules were substituted.
羧甲基淀粉(CMS)是淀粉与一氯乙酸(MCA)在氢氧化钠存在下反应的产物。研究了氢氧化钠/脱水葡萄糖单元(AGU)的摩尔比、MCA/AGU的摩尔比、反应时间、反应温度和含水量对取代度(DS)的影响。氢氧化钠/AGU和MCA/AGU的最佳摩尔比分别为2.4和1.0。氢氧化钠/AGU或MCA/AGU比例的增加会导致DS增加,但仅在一定程度上。当羧甲基化在60℃下进行2.5小时时,获得了最高的DS值。反应介质乙醇中的含水量最佳为20%(v/v)。扫描电子显微镜(SEM)照片显示,羧甲基化影响了淀粉的结构排列并导致颗粒解体。粒度分布(PSD)也表明,改性后平均粒径从37.37微米大幅增加到72.88微米。广角X射线衍射(XRD)表明,羧甲基化后淀粉结晶度明显降低。傅里叶变换红外光谱(FT-IR)中1600 cm-1和1426 cm-1处的新谱带表明淀粉颗粒被取代。