高含量大豆皂苷的制备工艺研究  

Preparation of high content soyasaponins by column chromatography and crystallization

作　　者：苏宝根[1] 马杰[1] 吴彩娟[1] 杨亦文[1] 任其龙[1] 

机构地区：[1]浙江大学化学工程与生物工程学系二次资源化工国家专业实验室,杭州310027

出　　处：《农业工程学报》2007年第10期241-245,共5页Transactions of the Chinese Society of Agricultural Engineering

基　　金：国家十一五科技支撑计划项目(2006BAD27B03)资助

摘　　要：为了得到高含量大豆皂苷,该文对6种大孔吸附树脂即AB-8,XAD-2,HPD-100,ADS-7,HPD-300,HPD-600进行优选,以上样量、洗脱率和产品纯度为指标,用柱层析法对低含量的大豆皂苷提取液进行初步分离,得到大豆皂苷粗品。然后通过结晶进一步提高其纯度。考察并优化了结晶时的溶剂、大豆皂苷的初始浓度、降温速率等工艺条件。结果表明：ADS-7树脂为合适的吸附剂;优化的柱层析条件为：上样和洗脱温度60℃,上样原料浓度6mg/mL,上样和洗脱流量均为1.0BV/h;优化的结晶工艺条件为：结晶溶剂30%～40%乙醇,大豆皂苷初始浓度165mg/mL,降温速率3.2℃/h。在上述条件下,用柱层析法可使大豆皂苷的含量从原料中的3.0%提高至45%以上,大豆皂苷收率大于90%。再通过结晶可得含量大于96.0%的大豆皂苷,大豆皂苷收率大于50%。说明该文研究的制备工艺明显优于现有的萃取工艺,具有重要的工业应用价值。In order to obtain high content soyasaponins, Six macroporous adsorption resins including AB-8, XAD-2, HPD-100, ADS-7, HPD-300, and HPD-600 were used to separate soyasaponins by column chromatography. The loading amount, elution rate and purity of soyasaponins had been examined to get the best-suited resin and optimal processing conditions. Then, soyasaponins were further purified by crystallization in ethanol solution. The nature of solvent, initial concentration of soyasoponins and rate of temperature fall were investigated and optimized. The results showed that ADS-7 was the best resin for column chromatography, the optimal operation conditions were as follows： temperature of feed and elution 60℃, feed concentration 6 mg/mL and flowrate of feed and elution 1.0 BV/h. The suitable crystallization conditions were as follows： solvent 30%~40% ethanol, initial concentration 165 mg/mL and rate of temperature fall 3.2℃/h. Under these conditions, the content of soyasaponins could be increased from 3.0% to 45% by column chromatography. The recovery rate was more than 90%. The content could further be raised to more than 96% by crystallization, with a recovery rate of more than 50%. It was indicated that the technology for high content soyasaponins preparation developed in this article was more suitable for industrial production than traditional solvent extraction process.

关 键 词：大豆皂苷 大孔吸附树脂 柱层析 结晶 

分 类 号：TQ914.1[化学工程]