CN115260143A - 从文冠木中提取杨梅素的方法 - Google Patents
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- IKMDFBPHZNJCSN-UHFFFAOYSA-N Myricetin Chemical compound C=1C(O)=CC(O)=C(C(C=2O)=O)C=1OC=2C1=CC(O)=C(O)C(O)=C1 IKMDFBPHZNJCSN-UHFFFAOYSA-N 0.000 title claims abstract description 46
- PCOBUQBNVYZTBU-UHFFFAOYSA-N myricetin Natural products OC1=C(O)C(O)=CC(C=2OC3=CC(O)=C(O)C(O)=C3C(=O)C=2)=C1 PCOBUQBNVYZTBU-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 235000007743 myricetin Nutrition 0.000 title claims abstract description 46
- 229940116852 myricetin Drugs 0.000 title claims abstract description 46
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- A61K31/335—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin
- A61K31/35—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin having six-membered rings with one oxygen as the only ring hetero atom
- A61K31/352—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin having six-membered rings with one oxygen as the only ring hetero atom condensed with carbocyclic rings, e.g. methantheline
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- C07D311/28—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 2 only
- C07D311/30—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3 with aromatic rings attached in position 2 only not hydrogenated in the hetero ring, e.g. flavones
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- C07D311/22—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
- C07D311/26—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4 with aromatic rings attached in position 2 or 3
- C07D311/40—Separation, e.g. from natural material; Purification
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Abstract
本发明涉及中药有效成分提取技术领域，提出了从文冠木中提取杨梅素的方法，包括以下步骤：S1、将文冠木药材烘烤，粉碎，过筛，得到文冠木粗粉；S2、将文冠木粗粉与逆流浸提液混合，进行低温逆流浸提，得到滤液和滤渣；S3、将滤渣与溶剂混合，加热回流提取1～3次，得到提取液；S4、合并提取液和S2中得到的滤液，加入碱性助剂，调节提取液的pH为8～9，加热煮沸后，降至室温，减压浓缩，得到浓缩液；S5、将浓缩液用一元醇水溶液在大孔吸附树脂中分离洗脱，收集洗脱液，干燥，得到杨梅素固体。通过上述技术方案，解决了现有技术中杨梅素提取率低、纯度低的问题。
Description
技术领域
本发明涉及中药有效成分提取技术领域，具体的，涉及从文冠木中提取杨梅素的方法。
背景技术
文冠木属无患子科，别名文官果、土木瓜、木瓜、温旦革子以木材及枝叶供药用，多分布于东北、华北、西北等地，味微甘、涩、苦、具有消肿止痛，燥血，干黄水的功效，可用于风湿性关节炎，风湿内热，麻风病等。文冠木中含有黄酮、香豆素及其苷类化合物，其中所含黄酮成分包括：二氢杨梅素、杨梅素、槲皮素、芦丁、二氢槲皮素、文冠木素和儿茶精。
杨梅素又名杨梅树皮素、杨梅黄酮、杨梅酮等，是一种多羟基黄酮醇化合物，易溶于甲醇、乙醇、丙酮、乙酸乙酯等有机溶剂，大剂量给药时具有祛风除湿、温经止痛、活血通络等功效。目前，杨梅素的制备方法主要是在天然藤茶和葡萄科蛇葡萄属植物中通过溶剂进行提取，由于在提取过程中易受到其它成分的干扰，特别是二氢杨梅素的干扰，导致提取的杨梅素的提取率和纯度较低，因此迫切的需要开发出一种制备高提取率、高纯度杨梅素的方法。
发明内容
本发明提出从文冠木中提取杨梅素的方法，解决了相关技术中杨梅素提取率低、纯度低的问题。
本发明的技术方案如下：
从文冠木中提取杨梅素的方法，其特征在于，包括以下步骤：
S1、将文冠木药材烘烤，粉碎，过筛，得到文冠木粗粉；
S2、将文冠木粗粉与逆流浸提液混合，进行低温逆流浸提，得到滤液和滤渣；
S3、将滤渣与溶剂混合，加热回流提取1～3次，得到提取液；
S4、合并提取液和S2中得到的滤液，加入碱性助剂，调节提取液的pH为8～9，加热煮沸后，降至室温，减压浓缩，得到浓缩液；
S5、将浓缩液用一元醇水溶液在大孔吸附树脂中分离洗脱，收集洗脱液，干燥，得到杨梅素固体。
作为进一步的技术方案，所述S1中烘烤温度为80～100℃。
作为进一步的技术方案，所述S1中文冠木粗粉的含水量≤2％。
作为进一步的技术方案，所述S2中文冠木粗粉与逆流浸提液的质量比为1:100～500。
作为进一步的技术方案，所述S2中逆流浸提液由质量比为4:1:500～1000的蔗糖酯、土耳其红油和乙醇混合组成。
作为进一步的技术方案，所述S2中低温逆流浸提的温度为25～35℃，时间为20～40min。
作为进一步的技术方案，所述S3中溶剂包括醇类、丙酮中的一种。
作为进一步的技术方案，所述S3中滤渣与溶剂的质量比为1:5～20。
作为进一步的技术方案，所述S4中碱性助剂为糖精钠。
作为进一步的技术方案，所述S5中一元醇水溶液包括体积分数45～65％的一元醇水溶液。
本发明的工作原理及有益效果为：
1、本发明采用低温逆流浸提法，将蔗糖酯、土耳其红油和乙醇作为逆流浸提液，由于在浸提溶剂中添加了蔗糖酯和土耳其红油，同时蔗糖酯和土耳其红油配伍使用，具有协同效应，使提取出的杨梅素具有高的提取率和纯度。
2、本发明通过在杨梅素的提取过程中加入糖精钠，将二氢杨梅素进一步转换为杨梅素，从而提高了杨梅素的提取率和纯度。
具体实施方式
下面将结合本发明实施例，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例，都涉及本发明保护的范围。
实施例1
S1、将1kg文冠木药材在80℃烘烤，烘烤至水分含量≤2％，粉碎，过筛，得到文冠木粗粉；
S2、将文冠木粗粉与逆流浸提液混合，在25℃进行逆流浸提40min，得到滤液和滤渣，所述文冠木粗粉与逆流浸提液的质量比为1:500，逆流浸提液由质量比为4:1:500的蔗糖酯、土耳其红油和乙醇混合组成；
S3、将滤渣与乙醇混合，加热回流提取1次，合并提取液和S2中得到滤液，加入糖精钠，调节提取液的pH为8，加热煮沸后，降至室温，减压浓缩，得到浓缩液，所述滤渣与乙醇的质量比为1:5；
S4、将浓缩液用体积分数为45％的乙醇水溶液在D101型大孔吸附树脂中分离洗脱，收集洗脱液，60℃干燥，得到6.8g杨梅素固体。
实施例2
S1、将1kg文冠木药材在85℃烘烤，烘烤至水分含量≤2％，粉碎，过筛，得到文冠木粗粉；
S2、将文冠木粗粉与逆流浸提液混合，在30℃进行逆流浸提30min，得到滤液和滤渣，所述文冠木粗粉与逆流浸提液的质量比为1:300，逆流浸提液由质量比为4:1:700的蔗糖酯、土耳其红油和乙醇混合组成；
S3、将滤渣与乙醇混合，加热回流提取3次，合并提取液和滤液，加入糖精钠，调节提取液的pH为9，加热煮沸后，降至室温，减压浓缩，得到浓缩液，所述滤渣与乙醇的质量比为1:8；
S4、将浓缩液用体积分数为50％的乙醇水溶液在D101型大孔吸附树脂中分离洗脱，收集洗脱液，60℃干燥，得到6.6g杨梅素固体。
实施例3
S1、将1kg文冠木药材在90℃烘烤，烘烤至水分含量≤2％，粉碎，过筛，得到文冠木粗粉；
S2、将文冠木粗粉与逆流浸提液混合，在35℃进行逆流浸提20min，得到滤液和滤渣，所述文冠木粗粉与逆流浸提液的质量比为1:100，逆流浸提液由质量比为4:1:1000的蔗糖酯、土耳其红油和乙醇混合组成；
S3、将滤渣与甲醇混合，加热回流提取2次，合并提取液和滤液，加入糖精钠，调节提取液的pH为8，加热煮沸后，降至室温，减压浓缩，得到浓缩液，所述滤渣与甲醇的质量比为1:10；
S4、将浓缩液用体积分数为60％的甲醇水溶液在D101型大孔吸附树脂中分离洗脱，收集洗脱液，60℃干燥，得到6.2g杨梅素固体。
实施例4
S1、将1kg文冠木药材在100℃烘烤，烘烤至水分含量≤2％，粉碎，过筛，得到文冠木粗粉；
S2、将文冠木粗粉与逆流浸提液混合，在30℃进行逆流浸提40min，得到滤液和滤渣，所述文冠木粗粉与逆流浸提液的质量比为1:400，逆流浸提液由质量比为4:1:900的蔗糖酯、土耳其红油和乙醇混合组成；
S3、将滤渣与丙酮混合，加热回流提取3次，合并提取液和滤液，加入糖精钠，调节提取液的pH为8，加热煮沸后，降至室温，减压浓缩，得到浓缩液，所述滤渣与丙酮的质量比为1:20；
S4、将浓缩液用体积分数为65％的甲醇水溶液在D101型大孔吸附树脂中分离洗脱，收集洗脱液，60℃干燥，得到6.3g杨梅素固体。
实施例5
S1、将1kg文冠木药材在95℃烘烤，烘烤至水分含量≤2％，粉碎，过筛，得到文冠木粗粉；
S2、将文冠木粗粉与逆流浸提液混合，在35℃进行逆流浸提40min，得到滤液和滤渣，所述文冠木粗粉与逆流浸提液的质量比为1:350，逆流浸提液由质量比为4:1:750的蔗糖酯、土耳其红油和乙醇混合组成；
S3、将滤渣与丙酮混合，加热回流提取1次，合并提取液和滤液，加入糖精钠，调节提取液的pH为9，加热煮沸后，降至室温，减压浓缩，得到浓缩液，所述滤渣与丙酮的质量比为1:18；
S4、将浓缩液用体积分数为50％的甲醇水溶液在D101型大孔吸附树脂中分离洗脱，收集洗脱液，60℃干燥，得到6.5g杨梅素固体。
对比例1
与实施例3的区别仅在于S2中逆流浸提液为乙醇，得到4.3g杨梅素固体。
对比例2
与实施例3的区别仅在于S2中逆流浸提液中不添加蔗糖酯，得到4.9g杨梅素固体。
对比例3
与实施例3的区别仅在于S2中逆流浸提液中不添加土耳其红油，得到5.1g杨梅素固体。
对比例4
与实施例3的区别仅在于S4中碱性助剂为碳酸氢钠，得到5.8g杨梅素固体。
提取率＝(杨梅素固体的质量/文冠木药材的质量)×100％
将实施例1～5与对比例1～4制备的杨梅素固体采用高效液相色谱法(HPLC)测定杨梅素的纯度，测试结果见表1。
表1杨梅素的提取率、纯度
由表1可以看出，实施例1～5从文冠木中提取出的杨梅素具有高的提取率和纯度。而对比例1中使用单一组分的乙醇作为逆流浸提液，对比例2使用土耳其红油和乙醇作为逆流浸提液，对比例3使用蔗糖酯和乙醇作为逆流提取溶剂，导致提取效果较差，提取出的杨梅素的提取率和纯度均不如实施例，同时，将对比例1～3与实施例3提取出的杨梅素提取率和纯度对比后，发现蔗糖酯和土耳其红油二者配伍使用，具有协同效果，提高了从文冠木中提取出的杨梅素的提取率和纯度。
对比例4与实施例3的区别仅在于将碱性助剂等量替换为碳酸氢钠，导致对比例4提取出的杨梅素的提取率和纯度不如实施例3。
以上仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。
Claims (10)
1.从文冠木中提取杨梅素的方法，其特征在于，包括以下步骤：
S1、将文冠木药材烘烤，粉碎，过筛，得到文冠木粗粉；
S2、将文冠木粗粉与逆流浸提液混合，进行低温逆流浸提，得到滤液和滤渣；
S3、将滤渣与溶剂混合，加热回流提取1～3次，得到提取液；
S4、合并提取液和S2中得到的滤液，加入碱性助剂，调节提取液的pH为8～9，加热煮沸后，降至室温，减压浓缩，得到浓缩液；
S5、将浓缩液用一元醇水溶液在大孔吸附树脂中分离洗脱，收集洗脱液，干燥，得到杨梅素固体。
2.根据权利要求1所述的从文冠木中提取杨梅素的方法，其特征在于，所述S1中烘烤温度为80～100℃。
3.根据权利要求1所述的从文冠木中提取杨梅素的方法，其特征在于，所述S1中文冠木粗粉的含水量≤2％。
4.根据权利要求1所述的从文冠木中提取杨梅素的方法，其特征在于，所述S2中文冠木粗粉与逆流浸提液的质量比为1:100～500。
5.根据权利要求1所述的从文冠木中提取杨梅素的方法，其特征在于，所述S2中逆流浸提液由质量比为4:1:500～1000的蔗糖酯、土耳其红油和乙醇混合组成。
6.根据权利要求1所述的从文冠木中提取杨梅素的方法，其特征在于，所述S2中低温逆流浸提的温度为25～35℃，时间为20～40min。
7.根据权利要求1所述的从文冠木中提取杨梅素的方法，其特征在于，所述S3中溶剂包括醇类、丙酮中的一种。
8.根据权利要求1所述的从文冠木中提取杨梅素的方法，其特征在于，所述S3中滤渣与溶剂的质量比为1:5～20。
9.根据权利要求1所述的从文冠木中提取杨梅素的方法，其特征在于，所述S4中碱性助剂为糖精钠。
10.根据权利要求1所述的从文冠木中提取杨梅素的方法，其特征在于，所述S5中一元醇水溶液包括体积分数45～65％的一元醇水溶液。
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