响应面法优化顺丁烯二酸-β-环糊精单乙酯的制备工艺

Optimization of β-cyclodextrin-maleate preparation using Response Surface Methdology

摘要:

β-环糊精是一种具有疏水性内腔的环状低聚糖，能将一定大小和形状的疏水性客体包合而形成包合物，对疏水性药物具有增溶作用和对天然药物具有保护和缓释作用等，而β-环糊精水溶性有限，与某些疏水性物质包合后形成的包合物水溶性得不到改善，容易从水溶液中析出。为增加β-环糊精的水溶性，拓展其在食品、药物领域中的应用，本文采用响应面试验对其衍生物顺丁烯二酸-β-环糊精单乙酯合成参数进行优化，得到最佳条件为顺丁烯二酸用量4.327 mmol，固液比0.408，反应温度109.462 ℃，乙醇浓度48.213%，在最佳工艺参数下，CDM实际酯化率达到40.977±2.032%，与预测值（40.71%）接近（相对误差0.656%），结果表明方法准确可靠；并且采用傅里叶红外光谱和质谱对顺丁烯二酸-β-环糊精单乙酯进行表征，验证了产物的合成。

Abstract:

Cyclodextrins are cyclic oligosaccharides possessing hydrophobic cavity, the cavity size and the inner hydrophobicity are suitable for encapsulating a variety of guests, which could improve the solubility of hydrophobic drug and protect the natural medicine. Some binding compounds could decrease β-cyclodextrin solubility in water, which limits its applications. In this study, the β-cyclodextrin-maleate (CDM) was prepared to improve solubility of β-cyclodextrin for application to food and drug industries. A response surface methodology was used to obtain a mathematical model that described the process and the optimal parameters were determined: the maleic acid 4.327 mmol, solid-to-liquid ratio 0.408, reaction temperature 109.462 ℃ and ethanol concentration 48.213%. Under these optimum conditions, the esteri?cation rate could be up to 40.977±2.032%, which was closed to the predicted value (40.71%). Moreover, the obtained product was characterized and identified by IR and MS.