【作者】 安红；

【导师】 程侣柏； 邓启刚； 王墨林；

【作者基本信息】 大连理工大学 ， 应用化学， 2002， 博士

【摘要】 本文以膏状磷脂为原料，用丙酮为溶剂，采用溶剂法，以粉状大豆磷脂为原料，利用乳化萃取技术进行了分离提纯制备高卵磷脂含量大豆磷脂的研究，优化了工艺条件，并建立了影响因素的二次回归方程。同时对多相溶剂萃取进行了研究。研究内容主要包括： 1、以膏状大豆磷脂为原料，用丙酮为溶剂制备了粉状磷脂。对萃取参数进行了优化，研究了洗涤次数，溶剂与膏状磷脂的比，丙酮中水的含量及萃取时的温度对粉状磷脂的纯度的影响。用正交设计优化了的萃取条件。在12℃，洗涤5次，膏状磷脂(g)：溶剂(ml)=30：250，萃取2min可得纯度为98.5％的粉状磷脂。 2、以乙醇为溶剂，以粉状大豆磷脂为原料进行分离提纯，(a)研究了抽提温度、乙醇浓度、磷脂与溶剂的比例、抽提时间对抽提结果的影响；(b)通过正交设计实验确定了最优条件为：抽提温度：-10℃；磷脂/溶剂：25g/300ml；乙醇体积分数为：95％；抽提时间：10min，使PC含量从原料中的25.6％提高到了69.65％；(c)通过二次回归正交设计试验进一步分析了各因素对抽提结果的综合影响，用数学优化方法建立了各因素影响的二次回归方程。 3、以乙醇为溶剂，以PC含量为54.48％的大豆磷脂为原料，进行二次萃取，实际操作为降温提取，实验结果证明了此方法的可行性；在所设计的实验中，提取物中PC含量从原料中的54.48％提高到了76.68％。以己烷—乙腈为溶剂对粉状磷脂的乙醇提取物进行双溶剂萃取，从原料中的63％提高到90％左右。优化的萃取条件为：在30℃，磷脂/正己烷为0.01g/ml，正己烷/乙腈(v/v)为1：2.5时，乙腈相提取物中PC含量、PC含量与PE的分离度可分别达到90％和52。 4、对大豆磷脂的表面物性进行了研究，测定了不同PC含量的磷脂的水溶液的电导率。测定了磷脂的润湿力和乳化力。建立了测定HLB值的实用方法。研究了磷脂作为乳化剂对豆油—水的乳化液的乳化稳定性，并观察了电解质(NaCl)对其乳化液稳定性的影响，发现加入电解质时形成稳定的乳状液需要更多的乳化剂。 5、建立了利用HPLC方法测定磷脂中各组分的定性及定量的分析方法。方法的准确度、精密度和可靠性均达到要求。更多还原

【Abstract】 The Phospholipids with high content Phosphatidylcholine was obtained using Acetone and Ethanol as solvents, emulsifying extraction technique, and wet gum Phospholipids as raw materials. The extraction conditions were optimized. A full factorial experiment method and a second-order orthogonal design were used in the study. The regression equations were calculated for maximum value of the response functions optimized. The main content in this thesis are:1. The granule Soya lecithin was purified by deoiling with acetone from Soya wet gum. The extraction parameters were studied. Through orthogonal design the optimum conditions were determined. Under the condition of using anhydrous acetone, Soya wet gum (g) : solvent Soya (ml) is 30 = 250, temperature is 12C and extraction time is 2 min, lecithin can be made into granule Soya lecithin, which acetone insoluble can reach 98.5%.2. Soybean phospholipids with high content of phosphatidylcholine was fractionated with ethanol, and optimum conditions have been determined to improve phosphatidylcholine(PC) enrichment. The effects of extraction time, solvent volume, ethanol concentration and temperature on the yield and PC enrichment have been described. A full factorial experiment method and a second-order orthogonal design were used in the study. The use of calculated optimal parameters in the fractionation process led to 69.65% PC enrichment and the yield of 25.6% , respectively.3. Based on the first-step extracting with ethanol as solvent, a second extracting with the same solvent was experimented. The availability of this method was proved. And PC content of the extracts was increased from 54.48% to 76.68%. The PC content about 90% of Phospholipids could be obtained using extracts of ethanol as raw material.4. Surfacial properties of Soybean lecithin with different PC content were studied in this paper. The conductivity of water solution (or emulsion) of phospholipids was measured and the changing was observed when ethanol added to the solution (or emulsion). Wetting power and emulsifying ability of lecithin were also measured. Stability of emulsions of soybean oil-lecithin-water was studied in which phospholipids were used as emulsifier, and it was found that stable emulsion required more of emulsifier when electrolyte(NaCl) was added to the emulsion.5. Soybean phospholipids were analyzed by positive-phase high performance liquid chromatography using gradient eluted program and evaporative light-scattering detector. The quantitative analysis of the four important components PC,PE,PI,PA of soybean phospholipids has been achieved with external standard method. The relative standard deviations is 0.82% ~ 1.34%, The recovery of the method is 96.7% ~ 100.8%. This method has been applied to the analysis of soybean phospholipids.更多还原