维生素C磷酸酯的工艺优化研究-毕业论文.docVIP

维生素C磷酸酯的工艺优化研究 摘 要 维生素C磷酸酯克服了维生素C易被氧化的缺点，所以在食品、医药及化妆品方面应用广泛。 用VC和丙酮（摩尔比为1∶12.4）作为原料三氯氧磷为催化剂，用量为VC用量的0.46倍（摩尔比），20℃下反应4 h，合成中间产物56-O-异丙叉-L-抗坏血酸（IPAA），产率90.88%。以IPAA为原料，三氯氧磷为磷酰化剂磷酰化反应时三氯氧磷的用量为IPAA的1.8倍（摩尔比），反应含有高浓度吡啶水溶液，保持pH=12~13，温度0~10℃下反应1.5 h。反应液L-抗坏血酸-2-磷酸酯(AP-Mg)，产率86%，纯度93.3%。通过化学显色法、紫外分光光度法、红外光谱法、高效液相色谱等对产物进行确定。分析结果表明，该方法合成的产品与标准品相符。 关键词： L-抗坏血酸-2-磷酸酯镁 5，6-O-异丙叉-L-抗坏血酸 工艺优化 Title: Study on the Optimal Preparation Process of L-Ascorbic acid-2-Phosphate Abstract: L-ascorbic acid-2-phosphate overcomes the shortcoming of L-ascorbic acid which is vulnerable to be oxidized, and has been broadly applied in food, medicine and cosmetic industry. This paper studied the properties, background and preparation technology of L-ascorbic acid and L-ascorbic acid-2-phosphate. Radical protection method for the preparation of magnesium L-ascorbic acid 2-phosphate was summarized. L-ascorbic acid reacted with acetone to prepare 5,6-O-isopropylidene-L-ascorbic acid ( IPAA), then phosphorylation with phosphoryl chloride and removing protective group to synthesize magnesium L-ascorbate-2-phosphate. Purify was followed by the hydrogen-type strong acid cation exchange resin, desalination, magnesium oxide neutralization and recrystallization. L - ascorbic acid -2 - magnesium phosphate obtained was .white or light yellow. Orthogonal and monothetic test indicated that the high yield and purity of the product was 86% and 93.3% respectively, which obtained under molar ratio of IPAA and phosphorus oxychloride (1:1.8), the concentrations of pyridine (2.6mol/L) and pH (12.5). the product was characterized by UV, IR, HPLC and it was in line of standard. Keywords: magnesium L-ascorbic acid 2-phosphate, 5,6-O-isopropy-lidene-L-ascorbic acid, process optimization 目 次 1 绪 论 8 1.1 维生素C 8 1．2. 近年来国内外VC衍生物的研究概况 8 1.2.1 VC钠 8 1.2.2 VC钙 2 1.2.3 VC多磷酸酯 2 1.2.4 维生素C棕榈酸酯 2 1.2.5 维生素C磷酸酯 3 1.3 维生素C磷酸酯的合成方法 4 2 维生素C磷酸酯镁的合成实验 5 2.1 实验部分 5 2.2 主要仪器与设备 5 2.3 试剂的配制 6 2.4 L-抗坏血酸-2-磷酸酯镁的合成