CN104926719B - 一种从火麻仁中提取葫芦巴碱的方法 - Google Patents

一种从火麻仁中提取葫芦巴碱的方法 Download PDF

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CN104926719B
CN104926719B CN201510418425.9A CN201510418425A CN104926719B CN 104926719 B CN104926719 B CN 104926719B CN 201510418425 A CN201510418425 A CN 201510418425A CN 104926719 B CN104926719 B CN 104926719B
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黄六仔
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    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
    • C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
    • C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
    • C07D213/60—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
    • C07D213/78—Carbon atoms having three bonds to hetero atoms, with at the most one bond to halogen, e.g. ester or nitrile radicals
    • C07D213/79—Acids; Esters
    • C07D213/80—Acids; Esters in position 3
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
    • C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
    • C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
    • C07D213/60—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
    • C07D213/78—Carbon atoms having three bonds to hetero atoms, with at the most one bond to halogen, e.g. ester or nitrile radicals
    • C07D213/79—Acids; Esters
    • C07D213/803—Processes of preparation

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Abstract

本发明公开了一种从火麻仁中提取葫芦巴碱的方法，该方法包括以下步骤：(1)用体积分数为20～30%乙醇溶液回流提取火麻仁，得提取液，将提取液减压浓缩，得浓缩物；(2)将浓缩物加水稀释至固形物质量分数占10～15%，加酸调节pH值至4.5～5.0，再固液分离除去不溶物，得澄清的水溶液；(3)将所述水溶液加入到大孔吸附树脂柱中，先用水洗涤大孔吸附树脂除去未被吸附的杂质至流出液pH值至6.5～7.0；再用体积分数为60～80%的乙醇溶液作为解吸液洗涤大孔吸附树脂，收集洗涤后的解吸液，经减压浓缩、干燥得火麻仁提取物。该方法工艺合理、有效成分含量高、提取效率高，操作简单，适合工业化生产。

Description

一种从火麻仁中提取葫芦巴碱的方法
技术领域
本发明涉及一种从火麻仁中提取葫芦巴碱的方法，属于生物医药领域。
背景技术
火麻仁，为桑科植物大麻(Cannabis sativa L.)的干燥成熟果实，《中国药典》2010版已收载，临床上主要用于肠燥便秘，血虚津亏等症。胡芦巴碱为火麻仁中的主要生物碱成分。胡芦巴碱具有抗肿瘤及降血糖的活性作用，还可以有效治疗一些皮肤病，但火麻仁中葫芦巴碱的含量低，约为0.2%。目前，国内外对火麻仁的报道主要集中脂肪酸类、大麻酚类物质等方面，对火麻仁中葫芦巴碱进行的提取研究还未见报道。
发明内容
本发明解决的技术问题是，实现火麻仁中胡芦巴碱的富集，提取其主要的有效成分胡芦巴碱，使其药用效果提升。
本发明的技术方案是，提供一种从火麻仁中提取葫芦巴碱的方法，包括以下步骤：(1)用体积分数为20～30%乙醇溶液回流提取火麻仁，得提取液，将提取液减压浓缩，得浓缩物；(2)将浓缩物加水稀释至固形物质量分数占10～15%，加酸调节pH值至4.5～5.0，再固液分离除去不溶物，得澄清的水溶液；(3)将所述水溶液加入到大孔吸附树脂柱中，先用水洗涤大孔吸附树脂除去未被吸附的杂质至流出液pH值至6.5～7.0；再用体积分数为60～80%的乙醇溶液作为解吸液洗涤大孔吸附树脂，收集洗涤后的解吸液，经减压浓缩、干燥得火麻仁提取物。
进一步地，所述大孔吸附树脂为极性大孔吸附树脂。
进一步地，所述大孔吸附树脂为XDA-8大孔吸附树脂。
进一步地，所述酸为柠檬酸。
进一步地，所述固液分离为过滤或离心。
进一步地，所述步骤(1)和步骤(3)中减压浓缩的温度为60～65℃。
进一步地，所述干燥为真空干燥或喷雾干燥，干燥至火麻仁提取物的水分不超过5%。
进一步地，所述回流提取为索氏提取。
目前类似物质的通常采用的是醇提，浓缩后用低温长时间沉淀除去杂质，主要缺陷是温度要求高（4℃左右）、时间长（静置12～48小时）、杂质去除不完全，从而导致生产周期长、成本高，而且有效成分含量低、难于产业化。本发明突出的优点是，回收有机溶剂后的浓缩液调整pH值至4.5～5.0，在此pH值下，有效成分葫芦巴碱的溶解性增大，而多糖、蛋白质、油脂等杂质被迅速沉淀出来，不需低温长时间静置，然后即可常温稀释、立即分离，极大缩短了生产周期。再使用得到酸性水溶液上大孔吸附树脂柱分离，杂质去除完全，产品有效成分高。目前常用的提取方法，提取物中目标产物的含量一般在5%，而用本发明的方法，提取物中葫芦巴碱含量能达到10～30%。本发明制备出的产品主要用于膳食补充剂、营养保健品。
本发明的优势在于：
1、本方法的提取葫芦巴碱的连贯性好，工艺简单，适合工业推广。
2、本方法工艺合理、有效成分含量高、提取效率高，操作简单，适合工业化生产。
3、本发明所制备的提取物纯度稳定，葫芦巴碱含量在10～30%之间。
4、本发明的制备方法收率高；溶剂可以回收再利用。
具体实施方式
本发明中乙醇的浓度均采用体积百分数表示。
实施例1
称取干燥火麻仁原料10kg，投入200L提取罐中，并加入20%的乙醇100L，开搅拌；打开夹套蒸汽，加热至有乙醇回流时，开始计时，提取1h；料液过400目滤袋，并向滤渣中再次投入20%乙醇100L，重复提取1h；回流提取完毕后，料液过400目滤袋，并将两次的滤液合并吸入100L外循环；打开外循环真空及蒸汽，开始回收乙醇，至馏出液乙醇含量小于5%后，放料，称重；将浓缩物加水稀释至固形物质量分数占12%，加酸调节pH值至4.8，再离心分离除去不溶物，得澄清的水溶液；滤液以25L/h的流速通过25L的XDA-8树脂柱；上柱完毕后，用纯水以50L/h的流速洗脱去树脂不吸附的杂质至流出液pH值至6.8，用60%的乙醇40L以10L/h的流速解吸，收集醇解吸液，减压回收乙醇解吸液浓缩到固形物含量达50%以上，真空干燥，得干浸膏120g，葫芦巴碱含量为15.4%。
实施例2
称取干燥火麻仁原料300kg，投入3000L提取罐中，并加入25%的乙醇2400L，开搅拌；打开夹套蒸汽，加热至有乙醇回流时，开始计时，提取1h；料液过400目滤袋，并向滤渣中再次投入25%乙醇2400L，重复提取1h；回流提取完毕后，料液过400目滤袋，并将两次的滤液合并吸入1000L外循环；打开外循环真空及蒸汽，开始回收乙醇，至馏出液乙醇含量小于5%后，放料，称重；将浓缩物加水稀释至固形物质量分数占12%，加酸调节pH值至4.6，再离心分离除去不溶物，得澄清的水溶液；滤液以1000L/h的流速通过1000L的XDA-8树脂柱；上柱完毕后，用纯水以2000L/h的流速洗脱去树脂不吸附的杂质至流出液pH值至6.7，用70%的乙醇1500L以500L/h的流速解吸，收集乙醇解吸液，减压回收乙醇解吸液浓缩到固形物含量达50%以上，真空干燥，得干浸膏3.4kg，葫芦巴碱含量为16.2%。
实施例3
称取干燥火麻仁原料250kg，投入3000L提取罐中，并加入30%的乙醇2400L，开搅拌；打开夹套蒸汽，加热至有乙醇回流时，开始计时，提取2h；料液过400目滤袋，并向滤渣中再次投入30%乙醇2400L，重复提取1h；回流提取完毕后，料液过400目滤袋，并将两次的滤液合并吸入1000L外循环；打开外循环真空及蒸汽，开始回收乙醇，至馏出液乙醇含量小于5%后，放料，称重；将浓缩物加水稀释至固形物质量分数占12%，加酸调节pH值至5.0，再离心分离除去不溶物，得澄清的水溶液；滤液以1000L/h的流速通过1000L的XDA-8树脂柱；上柱完毕后，用纯水以2000L/h的流速洗脱去树脂不吸附的杂质至流出液pH值至6.9，用80%的乙醇1500L以500L/h的流速解吸，收集乙醇解吸液，减压回收乙醇解吸液浓缩到固形物含量达50%以上，真空干燥，得干浸膏2.9kg，葫芦巴碱含量为15.6%。

Claims (8)

1.一种从火麻仁中提取葫芦巴碱的方法，其特征在于，包括以下步骤：
(1)用体积分数为20～30%乙醇溶液回流提取火麻仁，得提取液，将提取液减压浓缩，得浓缩物；
(2)将浓缩物加水稀释至固形物质量分数占10～15%，加酸调节pH值至4.5～5.0，再固液分离除去不溶物，得澄清的水溶液；
(3)将所述水溶液加入到大孔吸附树脂柱中，先用水洗涤大孔吸附树脂除去未被吸附的杂质至流出液pH值至6.5～7.0；再用体积分数为60～80%的乙醇溶液作为解吸液洗涤大孔吸附树脂，收集洗涤后的解吸液，经减压浓缩、干燥得火麻仁提取物。
2.如权利要求1所述的方法，其特征在于，所述大孔吸附树脂为极性大孔吸附树脂。
3.如权利要求1所述的方法，其特征在于，所述大孔吸附树脂为XDA-8大孔吸附树脂。
4.如权利要求1所述的方法，其特征在于，所述酸为柠檬酸。
5.如权利要求1所述的方法，其特征在于，所述固液分离为过滤或离心。
6.如权利要求1所述的方法，其特征在于，所述步骤(1)和步骤(3)中减压浓缩的温度均为60～65℃。
7.如权利要求1所述的方法，其特征在于，所述干燥为真空干燥或喷雾干燥，干燥至火麻仁提取物的水分不超过5%。
8.如权利要求1所述的方法，其特征在于，所述回流提取为索氏提取。
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CN105381030B (zh) * 2015-12-22 2020-04-14 江南大学 一种葫芦巴碱粗提取物的制备方法
CN109463582A (zh) * 2017-09-08 2019-03-15 汉义生物科技（北京）有限公司 一种含有火麻仁提取物的饮料及其制备方法
CN109517024A (zh) * 2018-12-19 2019-03-26 湖南杰萃生物技术有限公司 一种从蒲公英中提取蒲公英羽扇豆醇的方法
CN115385901A (zh) * 2022-08-24 2022-11-25 乔穗桃 一种从半夏中同时分离夏佛塔苷和胡芦巴碱的方法

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