CN105037310A - 一种同时提取杨梅素和二氢杨梅素的工艺 - Google Patents

一种同时提取杨梅素和二氢杨梅素的工艺 Download PDF

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CN105037310A
CN105037310A CN201510303781.6A CN201510303781A CN105037310A CN 105037310 A CN105037310 A CN 105037310A CN 201510303781 A CN201510303781 A CN 201510303781A CN 105037310 A CN105037310 A CN 105037310A
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韦小兰
陆兴国
陆曦
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LIUZHOU GREENSKY NATURAL INGREDIENTS CO Ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D311/00Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
    • C07D311/02Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
    • C07D311/04Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
    • C07D311/22Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
    • C07D311/26Benzo[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
    • C07D311/28Benzo[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
    • C07D311/30Benzo[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
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D311/00Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
    • C07D311/02Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
    • C07D311/04Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
    • C07D311/22Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
    • C07D311/26Benzo[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
    • C07D311/28Benzo[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
    • C07D311/322,3-Dihydro derivatives, e.g. flavanones
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D311/00Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
    • C07D311/02Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
    • C07D311/04Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
    • C07D311/22Benzo[b]pyrans, not hydrogenated in the carbocyclic ring with oxygen or sulfur atoms directly attached in position 4
    • C07D311/26Benzo[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
    • C07D311/40Separation, e.g. from natural material; Purification

Abstract

本发明公开了一种同时提取杨梅素和二氢杨梅素的工艺,以藤茶为原料,具体步骤如下:1)三道提取;2)澄清;3)脱色、过滤;4)粗晶形成;5)精制。本发明可以制得高纯度,高产的杨梅素和二氢杨梅素,杨梅素的收率可以达到2%,二氢杨梅素收率可以达到25%。且原料廉价易得,方法简单,对设备要求低,可广泛应用于工业化生产。

Description

一种同时提取杨梅素和二氢杨梅素的工艺
技术领域
本发明涉及一种同时提取杨梅素和二氢杨梅素的工艺。
背景技术
藤茶,学名为显齿蛇葡萄[Ampelopsisgrossedentata(Hand-Mazz)W.T.Wang],为葡萄科(VitaceaeMichx)蛇葡萄属(Ampelopsis)的一种野生木质落叶藤本植物,属于典型的类茶植物,俗称山甜茶、白茶、甘露茶、白毛猴、白茶等,主要分布于我国湖南、湖北、云南、贵州、广东、广西、福建等地。藤茶原植物生长于海拔4001300m之间,集中或散生在山坡的混杂林中,野生贮量大,分布和生长规律比较清晰,为可以直接利用的野生植物资源。
主要成分粗蛋白含量为13.94%,水溶性蛋白0.55%,总氨基酸2.53%,17种氨基酸中包含8种人体必需氨基酸;总灰分6.80%,包含丰富的无机营养元素;总多酚18.5%;特别是水浸出物含量高,5次浸提总浸提率高达72.97%,其中高含量的总黄酮和二氢杨梅素体现了该植物的特点。二氢杨梅素具有保肝利胆、抗氧化、消炎、止咳的作用。在食品工业和制药工业应用非常广泛。
二氢杨梅素具有清除自由基、抗氧化、抗血栓、抗肿瘤、消炎等多种奇特功效;而二氢杨梅素是较为特殊的一种黄酮类化合物,除具有黄酮类化合物的一般特性外,还具有解除醇中毒、预防酒精肝、脂肪肝、抑制肝细胞恶化、降低肝癌的发病率等作用。是保肝护肝,解酒醒酒的良品。
杨梅素又称杨梅树皮素,杨梅(黄)酮。黄酮类化合物。黄色针状结晶(稀乙醇),熔点357~360℃。微溶于沸水,溶于乙醇,几乎不溶于氯仿和醋酸。具有降血糖作用,抗氧化作用,保肝护肝作用可望开发出降血糖药物或者作为糖尿病患者食品添加剂使用。
发明内容
本发明要解决的技术问题是克服现有的缺陷,提供了一种同时提取高纯度的二氢杨梅素和杨梅素的工艺。
本发明的目的通过以下技术方案来具体实现:
一种同时提取杨梅素和二氢杨梅素的工艺,以藤茶为原料,具体步骤如下:
1)三道提取
将新鲜原料藤茶叶500g,加入3L60%乙醇,搅拌,冷浸2小时,用100目滤布过滤后,收集滤液;向滤渣加入3L60%乙醇,搅拌,冷浸2小时;用100目滤布过滤后,收集滤液;再向第二次提取后的滤渣加入1L60%乙醇+150g维生素C,搅拌,冷浸1小时,用100目滤布过滤后,收集滤液;
2)澄清
将步骤1)中收集的三道滤液合并,加入1ml澄清剂,搅拌均匀后静置,再用抽滤罐过滤澄清液,抽滤罐铺入3g的硅藻土作为助滤剂;
3)脱色、过滤
加入10g活性炭,加入2g维生素C,升温到60摄氏度后保温,同时搅拌20分钟后放液过滤;
4)粗晶形成
滤液加冷却结晶,晶体抽滤,得到180g含量为80%的二氢杨梅素粗晶;
5)精制
将540ml的30%乙醇加热到62摄氏度,先加入粗晶量1.5倍的维生素C,再加入粗晶,搅拌溶解完全后加入3.6g的活性炭,搅拌20分钟,过滤脱色液,将滤液静置24小时,过滤结晶液得到130g,含量98%的二氢杨梅素;
再将结晶母液回收酒精,至270ml,使用碳酸氢钠将pH值调至5,常温静置24小时,过滤结晶液得到10g95%含量的杨梅素。
本发明有益效果:
本发明通过结晶、重结晶同时获得二氢杨梅素、杨梅素,提高原料的利用率;使用维生素C作为抗氧化剂,保证有效成分不受破坏;用60度酒精热回流醇提取,冷浸提取,提取率达到95%以上;提取液中添加壳聚糖和活性炭,澄清脱色,提高提取物的纯度;通过快速浓缩及快速冷却的结晶与重结晶技术分离出高含量的二氢杨梅素产品,含量达到98%以上;壳聚糖具有良好的天然高分子的生物官能性和形容性;通过添加一定比例发澄清剂,使产品纯度得到很大的提高;通过间歇浓缩操作减少有效产品受热时间,保证产品有效成分不受破坏。本发明可以制得高纯度,高产的杨梅素和二氢杨梅素,杨梅素的收率可以达到2%,二氢杨梅素收率可以达到25%。且原料廉价易得,方法简单,对设备要求低,可广泛应用于工业化生产。
具体实施方式
以下对本发明的优选实施例进行说明,应当理解,此处所描述的优选实施例仅用于说明和解释本发明,并不用于限定本发明。
实施例1:
一种同时提取杨梅素和二氢杨梅素的工艺,以藤茶为原料,具体步骤如下:
1)三道提取
将新鲜原料藤茶叶500g,加入3L60%乙醇,搅拌,冷浸2小时,用100目滤布过滤后,收集滤液;向滤渣加入3L60%乙醇,搅拌,冷浸2小时;用100目滤布过滤后,收集滤液;再向第二次提取后的滤渣加入1L60%乙醇+150g维生素C,搅拌,冷浸1小时,用100目滤布过滤后,收集滤液;
2)澄清
将步骤1)中收集的三道滤液合并,加入1ml澄清剂,搅拌均匀后静置,再用抽滤罐过滤澄清液,抽滤罐铺入3g的硅藻土作为助滤剂;
3)脱色、过滤
加入10g活性炭,加入2g维生素C,升温到60摄氏度后保温,同时搅拌20分钟后放液过滤;
4)粗晶形成
滤液加冷却结晶,晶体抽滤,得到180g含量为80%的二氢杨梅素粗晶;
5)精制
将540ml的30%乙醇加热到62摄氏度,先加入粗晶量1.5倍的维生素C,再加入粗晶,搅拌溶解完全后加入3.6g的活性炭,搅拌20分钟,过滤脱色液,将滤液静置24小时,过滤结晶液得到130g,含量98%的二氢杨梅素;
再将结晶母液回收酒精,至270ml,使用碳酸氢钠将pH值调至5,常温静置24小时,过滤结晶液得到10g95%含量的杨梅素。
以上所述仅为本发明的优选实施例而已,并不用于限制本发明,尽管参照前述实施例对本发明进行了详细的说明,对于本领域的技术人员来说,其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换。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 (1)

1.一种同时提取杨梅素和二氢杨梅素的工艺,其特征在于:以藤茶为原料,具体步骤如下:
1)三道提取
将新鲜原料藤茶叶500g,加入3L60%乙醇,搅拌,冷浸2小时,用100目滤布过滤后,收集滤液;向滤渣加入3L60%乙醇,搅拌,冷浸2小时;用100目滤布过滤后,收集滤液;再向第二次提取后的滤渣加入1L60%乙醇+150g维生素C,搅拌,冷浸1小时,用100目滤布过滤后,收集滤液;
2)澄清
将步骤1)中收集的三道滤液合并,加入1ml澄清剂,搅拌均匀后静置,再用抽滤罐过滤澄清液,抽滤罐铺入3g的硅藻土作为助滤剂;
3)脱色、过滤
加入10g活性炭,加入2g维生素C,升温到60摄氏度后保温,同时搅拌20分钟后放液过滤;
4)粗晶形成
滤液加冷却结晶,晶体抽滤,得到180g含量为80%的二氢杨梅素粗晶;
5)精制
将540ml的30%乙醇加热到62摄氏度,先加入粗晶量1.5倍的维生素C,再加入粗晶,搅拌溶解完全后加入3.6g的活性炭,搅拌20分钟,过滤脱色液,将滤液静置24小时,过滤结晶液得到130g,含量98%的二氢杨梅素;
再将结晶母液回收酒精,至270ml,使用碳酸氢钠将pH值调至5,常温静置24小时,过滤结晶液得到10g95%含量的杨梅素。
CN201510303781.6A 2015-06-05 2015-06-05 一种同时提取杨梅素和二氢杨梅素的工艺 Expired - Fee Related CN105037310B (zh)

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