CN104610417A - 一种从山楂中提取熊果酸和齐墩果酸的方法 - Google Patents
一种从山楂中提取熊果酸和齐墩果酸的方法 Download PDFInfo
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Abstract
本发明旨在提供一种能够有效地提取分离山楂中熊果酸和齐墩果酸的方法，包括以下步骤：将山楂粉碎提取浓缩得浸膏A；加入石油醚淋洗，乙醇溶解过滤，经模拟移动床色谱进行分离，得到富含熊果酸的组分B和富含齐墩果酸的组分C；干燥分别得到纯度95%以上的熊果酸和纯度93%以上的齐墩果酸。本发明所述方法，采用微波辅助提取和模拟移动床色谱法分离提纯结合的工艺，确定了相关工艺参数，步骤简单，产品纯度较高，可以同时得到两种产物，将原料中的有效成分充分提取分离，节约了原料资源的同时也提高了生产效率。
Description
技术领域
本发明涉及一种从山楂中提取熊果酸和齐墩果酸的方法。
背景技术
山楂为蔷薇科植物山里红的干燥成熟果实，具有消食健胃、行气散淤、化浊降脂的功效。山楂中的主要化学成分有熊果酸、齐墩果酸、槲皮素、芦丁、金丝桃苷、枸缘酸等。其中，熊果酸和齐墩果酸为三萜类化合物，在山楂中含量较高。熊果酸又名乌苏酸，是一种五环三萜类化合物，具有抗肝炎、肿瘤、艾滋病毒、抗菌消炎、镇静等多种功效。由于其广泛的药理活性、较小的副作用和较低的毒性，近年来已成为医药保健、功能性食品开发等领域研究的热点。熊果酸在植物界中分布较广，主要分布在女贞子、山楂、白花蛇、舌草、陆英、夏枯草、山茱萸、石楠叶、山香圆叶、锁阳等植物中，以游离形式或结合成糖苷的形式存在。齐墩果酸又名土当归酸，是一种五环三萜类化合物，与熊果酸结构相似。具有保肝、护胃、强心、降糖、降血压、降血脂，以及抗菌消炎、抗氧化。调节免疫力、抑制血小板凝集等作用。近年研究表明其还具有一定的抗肿瘤、抗癌活性，是一种极具开发价值的天然活性物质。
目前，本领域中常用的熊果酸与齐墩果酸的分离纯化方法主要有：有机溶剂萃取法、沉淀法、柱色谱分步洗脱法、大孔吸附树脂法、高速逆流色谱法等。微波提取是利用不同结构的物质在微波场中吸收微波能力的差异, 使物质中的某些区域或提取体系中的某些组分被选择性加热, 从而使被提取物从物质或体系中分离, 进入介电常数较小、微波吸收能力相对差的提取剂中。这种方法的优点是对提取物具有较高的选择性、提取率高、提取速度快、溶剂用量少、安全、节能、设备简单。
模拟移动床色谱技术是将模拟移动床的设计思想引入液相制备色谱中，既保持了液相制备色谱的消耗小、分离纯度高，以及可变温操作等优点，又克服了通常液相制备色谱不能连续操作的缺点，使其具有分离能力强，设备体积小，投资成本低，并特别有利于分离热敏性高及难分离的物系等特点。
发明内容
本发明旨在提供一种能够有效地提取分离山楂中熊果酸和齐墩果酸的方法。
本发明所述的从山楂中提取熊果酸和齐墩果酸的方法，包括以下步骤：
(1) 将干燥的山楂粉碎，过20～60目筛，置于微波合成萃取仪中进行提取，加入乙醇溶液回流提取；
(2) 过滤出提取液，减压浓缩回收溶剂后得到浸膏A；
(3) 向浸膏A中加入石油醚淋洗，之后用乙醇溶液进行溶解，过滤，滤液进入模拟移动床色谱进行分离，得到富含熊果酸的组分B和富含齐墩果酸的组分C；
(4) 回收溶剂，减压干燥分别得到纯度95%以上的熊果酸和纯度93%以上的齐墩果酸。
本发明所述步骤(1)中，所述乙醇溶液可以为60%～95%乙醇溶液或无水乙醇。
本发明所述步骤(1)中，提取时，微波功率200W～400W，微波加热温度30℃～70℃，微波提取时间60s～300S，加入的乙醇溶剂与原料固液比为10:1～20:1。
本发明所述步骤(3)中， 模拟移动床色谱填充的吸附剂为非极性大孔吸附树脂，水洗区为纯化水，解吸剂为30～80%乙醇，其用量为树脂体积的1～3倍；树脂吸附再生溶剂为95%乙醇或2～4%氢氧化钠水溶液；吸附区流速1～2BV/h；水洗区流速1～3BV/h；解吸区流速2～4BV/h；再生区流速2～3BV/h；切换时间为600～900s；温度控制在40℃～60℃；压力控制在0.2MPa～0.6MPa。
本发明所述步骤(3)中，用于溶解浸膏A的乙醇溶液可以为95%乙醇溶液。
进一步地，本发明所述步骤(1)中，微波加热温度50℃～70℃，微波提取时间100s～200S，加入的乙醇溶剂与原料的液固比为15:1～20:1。
进一步地，本发明所述步骤(3)中，模拟移动床色谱的切换时间优选750～850s。
进一步地，本发明所述步骤(3)中，模拟移动床色谱填充的非极性大孔吸附树脂吸附剂可以为HPD-100或D101。
进一步地，本发明所述步骤(3)中，解吸区流速为4BV/h。
虽然模拟移动床技术可以应用于天然产物或药物的分离提纯已在本领域中有共识，但因模拟移动床大的结构特点是将化工中的连续、逆流、精馏、回流等要素都集中进了系统，它是一个多自由度、动态、相互关联的非线性系统。因此，对于它的预测、优化与控制是较复杂的问题，尤其是针对某一天然产物品种，分离参数的预测是一个十分复杂的问题。
本发明所述的熊果酸及齐墩果酸提取方法，采用微波辅助提取和模拟移动床色谱法分离提纯结合的工艺，确定了相关工艺参数，步骤简单，产品纯度较高，可以同时得到两种产物，将原料中的有效成分充分提取分离，节约了原料资源的同时也提高了生产效率。
具体实施方式
实施例1
将3Kg干燥的山楂（熊果酸质量百分含量0.28%，齐墩果酸质量百分含量0.042%）粉碎后过40目筛，以固液比1:16加入提取80%乙醇溶液，在功率250W、温度50℃条件下微波提取2min。过滤出提取液，减压浓缩回收溶剂后得到浸膏A；向浸膏A中加入适量石油醚淋洗，再加入适量95%乙醇使浸膏A恰好溶解，过滤，滤液进入模拟移动床色谱进行分离。吸附剂为HPD-100大孔吸附树脂，解吸剂为40%乙醇水溶液，其用量为树脂体积的3倍，水洗区为纯化水，树脂吸附再生溶剂为95%乙醇，吸附区流速2BV/h，解吸区流速4BV/h，水洗区流速3BV/h，再生区流速3BV/h，切换时间为760s，温度50℃，压力0.5MPa。分离得到富含熊果酸的组分B和富含齐墩果酸的组分C。将组分B和C分别回收溶剂，减压干燥，分别得到含量95.8%的熊果酸产品6.57g和含量94.3%的齐墩果酸产品0.93g。
实施例2
将5Kg干燥的山楂（熊果酸质量百分含量0.28%，齐墩果酸质量百分含量0.042%）粉碎后过60目筛，以固液比1:15加入提取溶剂无水乙醇，在功率300W、温度70℃条件下微波提取2.5min。过滤出提取液，减压浓缩回收溶剂后得到浸膏A；向浸膏A中加入适量石油醚淋洗，再加入95%乙醇进行溶解，过滤，滤液进入模拟移动床色谱进行分离。吸附剂为D101大孔吸附树脂，解吸剂为60%乙醇水溶液，其用量为树脂体积的3倍，水洗区为纯化水，树脂吸附再生溶剂为95%乙醇，吸附区流速2BV/h，解吸区流速4BV/h，水洗区流速3BV/h，再生区流速3BV/h，切换时间为780s，温度50℃，压力0.5MPa。分离得到富含熊果酸的组分B和富含齐墩果酸的组分C。将组分B和C分别回收溶剂，减压干燥，分别得到含量96.4%的熊果酸产品10.60g和含量93.8%的齐墩果酸产品1.61g。
实施例3
将8Kg干燥的山楂（熊果酸质量百分含量0.28%，齐墩果酸质量百分含量0.042%）粉碎后过40目筛，以固液比1:20加入提取溶剂无水乙醇，在功率350W、温度70℃条件下微波提取2min。过滤出提取液，减压浓缩回收溶剂后得到浸膏A；向浸膏A中加入适量石油醚淋洗，再加入95%乙醇进行溶解，过滤，滤液进入模拟移动床色谱进行分离。吸附剂为HPD-100大孔吸附树脂，解吸剂为80%乙醇水溶液，其用量为树脂体积的3倍，水洗区为纯化水，树脂吸附再生溶剂为95%乙醇，吸附区流速2BV/h，解吸区流速4BV/h，水洗区流速3BV/h，再生区流速3BV/h，切换时间为800s，温度50℃，压力0.5MPa。分离得到富含熊果酸的组分B和富含齐墩果酸的组分C。将组分B和C分别回收溶剂，减压干燥，分别得到含量95.3%的熊果酸产品16.92g和含量93.4%的齐墩果酸产品2.60g。
Claims (5)
1. 一种从山楂中提取熊果酸和齐墩果酸的方法，其特征在于包括以下步骤：
(1) 将干燥的山楂粉碎，过20～60目筛，置于微波合成萃取仪中进行提取，加入乙醇溶液回流提取；提取时，微波加热温度50℃～70℃，微波提取时间100s～200S，加入的乙醇溶剂与原料的液固比为15:1～20:1；
(2) 过滤出提取液，减压浓缩回收溶剂后得到浸膏A；
(3) 向浸膏A中加入石油醚淋洗，之后用乙醇溶液进行溶解，过滤，滤液进入模拟移动床色谱进行分离，得到富含熊果酸的组分B和富含齐墩果酸的组分C；模拟移动床色谱填充的吸附剂为非极性大孔吸附树脂，水洗区为纯化水，解吸剂为30～80%乙醇，其用量为树脂体积的1～3倍；树脂吸附再生溶剂为95%乙醇或2～4%氢氧化钠水溶液；吸附区流速1～2BV/h；水洗区流速1～3BV/h；解吸区流速2～4BV/h；再生区流速2～3BV/h；切换时间为600～900s；温度控制在40℃～60℃；压力控制在0.2MPa～0.6MPa；
(4) 回收溶剂，减压干燥分别得到纯度95%以上的熊果酸和纯度93%以上的齐墩果酸。
2.如权利要求1所述的一种从山楂中提取熊果酸和齐墩果酸的方法，其特征在于：本发明所述步骤(1)中，所述乙醇溶液可以为60%～95%乙醇溶液或无水乙醇。
3. 如权利要求1或2所述的一种从山楂中提取熊果酸和齐墩果酸的方法，其特征在于：本发明所述步骤(3)中，模拟移动床色谱的切换时间优选750～850s。
4. 如权利要求1-3中任一项所述的一种从山楂中提取熊果酸和齐墩果酸的方法，其特征在于：所述步骤(3)中，模拟移动床色谱填充的非极性大孔吸附树脂吸附剂为HPD-100或D101。
5. 如权利要求4中任一项所述的一种从山楂中提取熊果酸和齐墩果酸的方法，其特征在于：所述步骤(3)中，解吸区流速为4BV/h。
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| CN110563793A (zh) * | 2019-09-25 | 2019-12-13 | 广东科贸职业学院 | 微波萃取枇杷叶中的熊果酸和齐墩果酸的方法 |
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