吸附法制备高纯度磷脂酰胆碱的研究
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摘要
本文以醇溶性大豆磷脂为原料,研究了吸附法制备高纯度磷脂酰胆碱(PC)的方法,研究内容主要包括:
1、以醇溶性大豆磷脂为原料,以乙醇为溶剂,用固体吸附剂搅拌纯化磷脂,对此制备方法的各因素进行了实验,得知影响产品纯度和PC得率的主要因素为:乙醇体积分数、液料比、吸附剂用量、吸附温度、吸附时间、吸附次数。用均匀设计法来设计实验,并用BP神经网络模型对实验结果进行建模分析,得出最优试验条件为:乙醇体积分数94.0%,乙醇:磷脂原料比为18 mL/g,吸附剂:磷脂原料比为0.5g/g,吸附温度为38.0℃,每次吸附时间为10min,吸附次数为6次,在此条件下进行了验证实验,可以使产品纯度达到93.055%,PC得率达到76.797%。
2、对吸附剂对磷脂的吸附特性进行了研究,发现吸附剂对PE具有较强的选择吸附能力,但是它对PC也并不是绝对不吸附;吸附温度对PC的吸附有一定的影响,随着温度升高,PC的吸附率逐渐增加;吸附时间对吸附选择性有一定影响,在最佳吸附剂用量下,PC吸附达到平衡的时间比PE完全去除所需时间稍长;溶液中的PC浓度在一定范围内不影响吸附剂对PE的高选择性吸附;溶液中乙醇体积分数对PE吸附有一定影响,在乙醇体积分数较低如为76.0%和85.3%时,吸附剂并不能将PE完全吸附,但是同时随着乙醇体积分数的增加,吸附剂对PC的吸附也加强。
3、对吸附剂对PE的吸附平衡及吸附动力学进行了研究,得知:PE在吸附剂上的吸附平衡能够用Langmuir模型很好地描述,即PE在吸附剂上的吸附平衡可表示为Qe=QmKCe/(1+ KCe);吸附剂吸附PE的吸附热△HA,m﹤20 kJ/mol,所以此吸附属于物理吸附的范畴;吸附剂吸附PE的吸附速率曲线表现为一级动力学特征,可采用Lagergren一级速率方程:lg(1-F)= -K`t/2.303计算吸附速率;用孔扩散方程对吸附剂吸附PE的吸附速率曲线进行拟合,各相关系数都大于0.99,表明孔扩散是该吸附过程的主要控制步骤,但由于其拟合直线都不经过原点,表明它不是唯一的控制因素,所以认为膜表面扩散与孔扩散共同影响吸附剂对PE的吸附过程。
4、同时对吸附剂吸附法和吸附剂层析法所制得的磷脂酰胆碱产品进行了比较分析,得到:两者均含有肉豆蔻酸(C14:0)、棕榈酸(C16:0)、棕榈油酸(C16:1)、硬脂酸(C18:0)、油酸(C18:1)、亚油酸(C18:2)和亚麻酸(C18:3),而亚油酸含量最高,达65%左右; HPLC/MS分析结果为:两种PC产品中均含有16:1/18:1-PC、16:0/18:2-PC、16:0/18:1-PC、18:3/18:3-PC、18:2/18:3-PC、18:2/18:2-PC、18:1/18:2-PC、18:0/18:2-PC、18:0/18:1-PC等九种PC分子种,两种PC产品中二亚油酰磷脂酰胆碱(18:2/18:2-PC)的含量均最高。
Highly purified phosphatidylcholine was obtained using adsorption process,and alcohol-soluble phospholipids as raw materials. The main content in this thesis are:
1.The phospholipids was purified using ethanol as solvent,adsorbing technique ,and alcohol-soluble soybean phospholipids as raw materials.The processing parameters was studied.The experiment was designed by the uniform design table,and The BP neural network was used to optimize the results of uniform experiment.Under the conditions : volume percent of ethanol is 94.0%, use level of ethanol is 18mL/g, use level of sorbent is 0.5g/g, processing temperature is 38.0℃, processing time is 10min,and 6 times,which content of phosphatidylcholine reach 93.055%, yield of phosphatidylcholine reach 76.797%.
2. After researching adsorption process between adsorbent and phospholipids ,we find the adsorbent is the first to adsorb phosphatidylethanolamine,and when the adsorbent is excessive,the phosphatidylcholine is adsorbed,too.The temperature,time,concentration of phosphatidylcholine in solution and volume percent of ethanol of processing changed the adsorption phosphatidylethanolamine by adsorbent.
3.Adsorption dynamics research of PE indicated that adsorption isotherm of PE could be described with the equation of Langmuir,namely, Qe=QmKCe/(1+ KCe).Because the adsorption heat of PE on sorbent△HA,m﹤20 kJ/mol, the adsorption process is physical adsorption; The adsorption rate of PE could be calculated with Lagergren level rate equation,it can be expressed as lg(1-F)= -K`t/2.303.The intra-particle diffusion equation was used to fit the adsorption rate curves of PE on sorbent,the relative coefficients were greater than 0.99,it showed that intra-particle diffusion is the main control step of the adsorption of PE on sorbent.Whereas,The fitting of straight lines don’t pass by origin,we thought the adsorption rate of PE was governed by surface diffusion and intra-particle diffusion.
4.The result of comparing the two PC prouducts as follows:the two both had tetradecanoic acid, palmitic acid, zoomaric acid, stearic acid, oleic acid, linoleic acid, linolenic acid,and the content of linoleic acid was the most;The outcome pf HPLC-MS analysis was the product had different molecule species,such as: 16:1/18:1-PC、16:0/18:2-PC、16:0/18:1-PC、18:3/18:3-PC、18:2/18:3-PC、18:2/18:2-PC、18:1/18:2-PC、18:0/18:2-PC and 18:0/18:1-PC,the maximum was 18:2/18:2-PC.
1、以醇溶性大豆磷脂为原料,以乙醇为溶剂,用固体吸附剂搅拌纯化磷脂,对此制备方法的各因素进行了实验,得知影响产品纯度和PC得率的主要因素为:乙醇体积分数、液料比、吸附剂用量、吸附温度、吸附时间、吸附次数。用均匀设计法来设计实验,并用BP神经网络模型对实验结果进行建模分析,得出最优试验条件为:乙醇体积分数94.0%,乙醇:磷脂原料比为18 mL/g,吸附剂:磷脂原料比为0.5g/g,吸附温度为38.0℃,每次吸附时间为10min,吸附次数为6次,在此条件下进行了验证实验,可以使产品纯度达到93.055%,PC得率达到76.797%。
2、对吸附剂对磷脂的吸附特性进行了研究,发现吸附剂对PE具有较强的选择吸附能力,但是它对PC也并不是绝对不吸附;吸附温度对PC的吸附有一定的影响,随着温度升高,PC的吸附率逐渐增加;吸附时间对吸附选择性有一定影响,在最佳吸附剂用量下,PC吸附达到平衡的时间比PE完全去除所需时间稍长;溶液中的PC浓度在一定范围内不影响吸附剂对PE的高选择性吸附;溶液中乙醇体积分数对PE吸附有一定影响,在乙醇体积分数较低如为76.0%和85.3%时,吸附剂并不能将PE完全吸附,但是同时随着乙醇体积分数的增加,吸附剂对PC的吸附也加强。
3、对吸附剂对PE的吸附平衡及吸附动力学进行了研究,得知:PE在吸附剂上的吸附平衡能够用Langmuir模型很好地描述,即PE在吸附剂上的吸附平衡可表示为Qe=QmKCe/(1+ KCe);吸附剂吸附PE的吸附热△HA,m﹤20 kJ/mol,所以此吸附属于物理吸附的范畴;吸附剂吸附PE的吸附速率曲线表现为一级动力学特征,可采用Lagergren一级速率方程:lg(1-F)= -K`t/2.303计算吸附速率;用孔扩散方程对吸附剂吸附PE的吸附速率曲线进行拟合,各相关系数都大于0.99,表明孔扩散是该吸附过程的主要控制步骤,但由于其拟合直线都不经过原点,表明它不是唯一的控制因素,所以认为膜表面扩散与孔扩散共同影响吸附剂对PE的吸附过程。
4、同时对吸附剂吸附法和吸附剂层析法所制得的磷脂酰胆碱产品进行了比较分析,得到:两者均含有肉豆蔻酸(C14:0)、棕榈酸(C16:0)、棕榈油酸(C16:1)、硬脂酸(C18:0)、油酸(C18:1)、亚油酸(C18:2)和亚麻酸(C18:3),而亚油酸含量最高,达65%左右; HPLC/MS分析结果为:两种PC产品中均含有16:1/18:1-PC、16:0/18:2-PC、16:0/18:1-PC、18:3/18:3-PC、18:2/18:3-PC、18:2/18:2-PC、18:1/18:2-PC、18:0/18:2-PC、18:0/18:1-PC等九种PC分子种,两种PC产品中二亚油酰磷脂酰胆碱(18:2/18:2-PC)的含量均最高。
Highly purified phosphatidylcholine was obtained using adsorption process,and alcohol-soluble phospholipids as raw materials. The main content in this thesis are:
1.The phospholipids was purified using ethanol as solvent,adsorbing technique ,and alcohol-soluble soybean phospholipids as raw materials.The processing parameters was studied.The experiment was designed by the uniform design table,and The BP neural network was used to optimize the results of uniform experiment.Under the conditions : volume percent of ethanol is 94.0%, use level of ethanol is 18mL/g, use level of sorbent is 0.5g/g, processing temperature is 38.0℃, processing time is 10min,and 6 times,which content of phosphatidylcholine reach 93.055%, yield of phosphatidylcholine reach 76.797%.
2. After researching adsorption process between adsorbent and phospholipids ,we find the adsorbent is the first to adsorb phosphatidylethanolamine,and when the adsorbent is excessive,the phosphatidylcholine is adsorbed,too.The temperature,time,concentration of phosphatidylcholine in solution and volume percent of ethanol of processing changed the adsorption phosphatidylethanolamine by adsorbent.
3.Adsorption dynamics research of PE indicated that adsorption isotherm of PE could be described with the equation of Langmuir,namely, Qe=QmKCe/(1+ KCe).Because the adsorption heat of PE on sorbent△HA,m﹤20 kJ/mol, the adsorption process is physical adsorption; The adsorption rate of PE could be calculated with Lagergren level rate equation,it can be expressed as lg(1-F)= -K`t/2.303.The intra-particle diffusion equation was used to fit the adsorption rate curves of PE on sorbent,the relative coefficients were greater than 0.99,it showed that intra-particle diffusion is the main control step of the adsorption of PE on sorbent.Whereas,The fitting of straight lines don’t pass by origin,we thought the adsorption rate of PE was governed by surface diffusion and intra-particle diffusion.
4.The result of comparing the two PC prouducts as follows:the two both had tetradecanoic acid, palmitic acid, zoomaric acid, stearic acid, oleic acid, linoleic acid, linolenic acid,and the content of linoleic acid was the most;The outcome pf HPLC-MS analysis was the product had different molecule species,such as: 16:1/18:1-PC、16:0/18:2-PC、16:0/18:1-PC、18:3/18:3-PC、18:2/18:3-PC、18:2/18:2-PC、18:1/18:2-PC、18:0/18:2-PC and 18:0/18:1-PC,the maximum was 18:2/18:2-PC.
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