ART-中红外光谱在丁烯酸-β-环糊精酯合成中的应用  

Application of ART Mid-Infrared Spectroscopy in Synthesis ofβ-cyclodextrin Butenate

作　　者：李咏富[1,2] 田竹希 唐洪涛 罗其琪 何扬波 石彬 LI Yong-fu;TIAN Zhu-xi;TANG Hong-tao;LUO Qi-qi;HE Yang-bo;SHI Bin(Integrated Rural Development Center,Guizhou Academy of Agricultural Science,Guiyang 550006,China;Irradiation preservation and processing engineering technology research center of Guizhou agricultural products,Guiyang 550006,China;National Center for Child Nutriment Quality Supervision and Testing,Beijing 100035,China)

机构地区：[1]贵州省农业科学院现代农业发展研究所,贵阳550006 [2]贵州省特色农产品辐照保鲜与加工工程技术研究中心,贵阳550006 [3]中国儿童中心儿童营养与健康研究中心,北京100035

出　　处：《中国食物与营养》2022年第1期20-24,共5页Food and Nutrition in China

基　　金：贵州省基础研究计划项目“两亲性β-环糊精高分子聚合物制备及其应用研究”(项目编号:黔科合基础[2018]1420)。

摘　　要：目的:利用衰减全反射(ATR)中红外光谱技术实现丁烯酸-β-环糊精酯制备条件的快速优化。方法:制备丁烯酸-β-环糊精酯以二甲基甲酰胺为溶剂、N,N-羰基二咪唑为羧酸活化剂、二甲氨基吡啶为催化剂;通过分析不同条件下制备的丁烯酸-β-环糊精酯红外图谱中不饱和酯羰基C=O的伸缩振动吸收峰(1738 cm^(-1))评价β-环糊精的酯化率。结果:丁烯酸-β-环糊精酯的最佳合成条件为β-环糊精浓度50 mmol/L、二甲氨基吡啶的浓度12.5 mmol/L、丁烯酸浓度450 mmol/L、反应时间20 min、反应温度25℃。结论:ATR红外光谱技术的应用可极大地提升β-环糊精酯样品的分析速度,减少样品分析时间,适合用于丁烯酸-β-环糊精酯合成条件的快速优化。【Objective】 To use attenuated total reflection (ATR) mid-infrared spectroscopy to quickly optimize the preparation conditions of β-cyclodextrin butenate.【Method】β-cyclodextrin butenate was prepared by using dimethylformamide as solvent,N,N-carbonyl diimidazole as carboxylic acid activator and di-methyl-amino-pyridine as catalyst.The esterification rate of β-cyclodextrin was evaluated by analyzing the stretching vibration absorption peak (1738 cm^(-1)) of unsaturated ester carbonyl C=O in the infrared spectrum of β-cyclodextrin butenate prepared under different conditions.【Result】The optimum synthesis conditions of butenic acid-β-cyclodextrin were the concentration of β-cyclodextrin 50 mmol/L,the concentration of dimethyl-amino-pyridine 12.5 mmol/L,the concentration of butenic acid 450 mmol/L,the reaction time 20 min,and the reaction temperature 25℃.【Conclusion】The application of ATR infrared spectroscopy technology can improve the analysis speed of β-cyclodextrin butenate samples greatly and reduce the analysis time of sample,which is suitable for the rapid optimization of the synthesis conditions ofβ-cyclodextrin butenate.

关 键 词：中红外光谱 乙烯基β-环糊精衍生物 酯合成 衰减全反射(ATR) 

分 类 号：TQ2[化学工程—有机化工]