羊毛脂中胆甾醇的分离提取工艺
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摘要
胆甾醇作为一种广泛存在的天然甾体资源,可以用于甾体药物合成、化妆品和液晶材料领域。羊毛脂来源于洗毛工业废水,其水解后的产物羊毛脂醇中富含胆甾醇和羊毛甾醇。
本文以羊毛脂醇为原料,研究了提取胆甾醇的相关问题,提出了以分子蒸馏法结合溶剂选择性结晶分离提取胆甾醇的工艺路线。此工艺对环境友好,同时可回收羊毛甾醇。
建立了羊毛脂醇中胆甾醇的反相高效液相色谱分析方法。保留时间定性,外标法定量。胆甾醇的加标回收率为97.56~101.60%,相对标准偏差0.86~1.31%。此法简便、准确、重现性好。
对皂化后的羊毛脂醇进行分子蒸馏精制,轻相馏分的羊毛脂醇色泽得到明显改善。应用响应面法对分子蒸馏实验条件进行优化,建立了优化模型,通过对拟合模型进行优化计算得到了含量和收率兼顾的优化工艺条件,三次平行实验值与预测值吻合较好,验证了模型的可靠性。胆甾醇的平均含量达到17.47%,回收率大于90%。
采用溶剂选择性结晶分步得到羊毛甾醇、高级脂肪醇和胆甾醇。考察了降温速率、溶剂用量、养晶终止温度和养晶时间等主要因素对结晶过程的影响。在优化的操作条件下,胆甾醇粗品纯度为76.24%,回收率79.81%。
应用静态法测定了胆甾醇在六种有机溶剂中的溶解度,为实验提供基本的溶解度数据参考,并采用λh模型和Apelblat方程关联了溶解度随温度的变化关系,相关系数R2在0.95以上,表明两种模型合适有效。
以乙酸或甲醇-异丙醇的混合溶剂对胆甾醇粗品进行重结晶,胆甾醇纯度达到92%以上。
As a widespread natural steroid resource, cholesterol can be used for synthesis of steroid drugs, cosmetics and liquid crystal materials. Lanolin is a by-product extracted from wool lotion. As one hydrolysis product of lanolin, lanolin alcohol is rich in cholesterol and lanostreol.
This thesis supposed a process route to extract cholesterol from lanolin alcohol, which included molecular distillation and selective crystallization. The process is more environmentally friendly while lanosterol could also be recycled. A RP-HPLC method was established to analyze cholesterol in lanolin alcohol. Retention time and peak area using external standard method was used for the qualitative and quantitative analysis respectively. The average recoveries are 97.56~101.60%, the relative standard deviations are 0.86~1.31%. This method is simple, accurate and reproducible.
The sopanification product of lanolin alcohol was trated by molecular distillation. The distillate was composed of cholesterol, lanosterol and fatty alcohols, which was called refined lanolin alcohol. The color of refined lanolin alcohol was improved. Using response surface methodology, the experimental conditions of molecular distillation were optimized, and the optimal model was established. The optimum balance between the content and recovery of cholesterol is obtained. The reliability of the model was validated by three parallel experiments. The average content and recovery of cholesterol reached 17.47% and 90% respectively. Using selective crystallization method, lanosterol, high-level fatty alcohols, and cholesterol were isolated step by step. The main influential factors in selective crystallization process were investigated, including solvent volume, cooling rate, cooling temperature, and crystallization time. Under the optimum operating conditions, the purity of crude cholesterol was 76.24%, and the recovery of cholesterol was 79.81%.
Solubility of cholesterol in six solvents was determined by steady method. The variation of solubility with temperature was correlated byλh model and Apelblat equation, and correlation coefficient R2 0.95, which indicated two models were appropriate and effective.
The purity of cholesterol achieved more than 92% after recrystallization with acetic acid or methanol-isopropanol as solvent.
本文以羊毛脂醇为原料,研究了提取胆甾醇的相关问题,提出了以分子蒸馏法结合溶剂选择性结晶分离提取胆甾醇的工艺路线。此工艺对环境友好,同时可回收羊毛甾醇。
建立了羊毛脂醇中胆甾醇的反相高效液相色谱分析方法。保留时间定性,外标法定量。胆甾醇的加标回收率为97.56~101.60%,相对标准偏差0.86~1.31%。此法简便、准确、重现性好。
对皂化后的羊毛脂醇进行分子蒸馏精制,轻相馏分的羊毛脂醇色泽得到明显改善。应用响应面法对分子蒸馏实验条件进行优化,建立了优化模型,通过对拟合模型进行优化计算得到了含量和收率兼顾的优化工艺条件,三次平行实验值与预测值吻合较好,验证了模型的可靠性。胆甾醇的平均含量达到17.47%,回收率大于90%。
采用溶剂选择性结晶分步得到羊毛甾醇、高级脂肪醇和胆甾醇。考察了降温速率、溶剂用量、养晶终止温度和养晶时间等主要因素对结晶过程的影响。在优化的操作条件下,胆甾醇粗品纯度为76.24%,回收率79.81%。
应用静态法测定了胆甾醇在六种有机溶剂中的溶解度,为实验提供基本的溶解度数据参考,并采用λh模型和Apelblat方程关联了溶解度随温度的变化关系,相关系数R2在0.95以上,表明两种模型合适有效。
以乙酸或甲醇-异丙醇的混合溶剂对胆甾醇粗品进行重结晶,胆甾醇纯度达到92%以上。
As a widespread natural steroid resource, cholesterol can be used for synthesis of steroid drugs, cosmetics and liquid crystal materials. Lanolin is a by-product extracted from wool lotion. As one hydrolysis product of lanolin, lanolin alcohol is rich in cholesterol and lanostreol.
This thesis supposed a process route to extract cholesterol from lanolin alcohol, which included molecular distillation and selective crystallization. The process is more environmentally friendly while lanosterol could also be recycled. A RP-HPLC method was established to analyze cholesterol in lanolin alcohol. Retention time and peak area using external standard method was used for the qualitative and quantitative analysis respectively. The average recoveries are 97.56~101.60%, the relative standard deviations are 0.86~1.31%. This method is simple, accurate and reproducible.
The sopanification product of lanolin alcohol was trated by molecular distillation. The distillate was composed of cholesterol, lanosterol and fatty alcohols, which was called refined lanolin alcohol. The color of refined lanolin alcohol was improved. Using response surface methodology, the experimental conditions of molecular distillation were optimized, and the optimal model was established. The optimum balance between the content and recovery of cholesterol is obtained. The reliability of the model was validated by three parallel experiments. The average content and recovery of cholesterol reached 17.47% and 90% respectively. Using selective crystallization method, lanosterol, high-level fatty alcohols, and cholesterol were isolated step by step. The main influential factors in selective crystallization process were investigated, including solvent volume, cooling rate, cooling temperature, and crystallization time. Under the optimum operating conditions, the purity of crude cholesterol was 76.24%, and the recovery of cholesterol was 79.81%.
Solubility of cholesterol in six solvents was determined by steady method. The variation of solubility with temperature was correlated byλh model and Apelblat equation, and correlation coefficient R2 0.95, which indicated two models were appropriate and effective.
The purity of cholesterol achieved more than 92% after recrystallization with acetic acid or methanol-isopropanol as solvent.
引文
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