CN101857538A - Method for extracting frangula emodin from giant knotweed - Google Patents
Method for extracting frangula emodin from giant knotweed Download PDFInfo
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- CN101857538A CN101857538A CN201010197882A CN201010197882A CN101857538A CN 101857538 A CN101857538 A CN 101857538A CN 201010197882 A CN201010197882 A CN 201010197882A CN 201010197882 A CN201010197882 A CN 201010197882A CN 101857538 A CN101857538 A CN 101857538A
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- giant knotweed
- emodin
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- chloroform
- mother liquor
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Abstract
The invention relates to a method for extracting frangula emodin from giant knotweed, which adopts water as a solvent to substitute the traditional organic solvent. The frangula emodin is extracted through the procedures such as decoction, water extraction, concentration, crystallization, re-crystallization and the like. The method has low cost and simple process, and is environment-friendly and toxic-free.
Description
Technical field
The present invention relates to a kind of extraction method for emodin, more particularly, the present invention relates to a kind of method for emodin of from giant knotweed, extracting.
Background technology
Giant knotweed is for being the dry rhizome and the root of polygonaceae plant giant knotweed.This product mostly is cylindrical short section or irregular sheet, long 1-7cm, diameter 0.5-2.5cm.The crust brown has vertical wrinkle and mark of fibrous root, and tangent plane skin zone is thinner, the woody part broadness, and pale brown look, the ray irradiation shape, skin zone and woody part are more easily separated.Have in the rhizome marrow every or be empty shape, matter is hard, gas is little, mildly bitter flavor, puckery.
Polygoni cuspidati,radix and rhizome contain dissociated anthraquinone and anthracene is joined glucoside, is mainly Schuttgelb, rheochrysidin, chrysophanol etc.Big yellow be the crystallization of orange-yellow minute hand shape (crystallization is orange in the acetone, and crystallization be a yellow in the methyl alcohol), 256 ℃～257 ℃ of fusing points have the special reaction of anthraquinone, and are water-soluble hardly, are dissolved in ethanol and alkaline solution.Schuttgelb can be used as cathartic, rushes down activity down though have, because easy oxidized destruction in the body, in fact discharge function is very weak, as being combined into glycoside with sugar, then can bring into play discharge function.Schuttgelb-1-O-β-D-glucoside and Schuttgelb-8-O-β-D-glucoside then is Schuttgelb and glucose bonded glycosides, and the two is a bonded position difference, is present in simultaneously in rheum officinale and the giant knotweed.Other has antibiotic, cough-relieving, effect such as antitumor, hypotensive.
Clinically, with the pure product treatment of Schuttgelb cancer, be mainly used in tumours such as leukemia, cancer of the stomach, the most frequently used then being used for is antibacterial.It to a lot of bacteriums such as various staphylococcus, Hemolytic streptococcus, diphtheria corynebacterium, comma bacillus, intestinal bacteria, Pseudomonas aeruginosa, dermatophytes, Bacillus subtilus, Mycobacterium phlei, gonococcus, charcoal should bacillus, careless shape bacterium, Corynebacterium diphtheriae, dysentery bacterium etc. all have restraining effect.Wherein more effective to staphylococcus, gonococcus, suis.This product is also effective to fungi, virus, protozoon.Simultaneously, also have effects such as diuresis, cholagogic, spasmolysis, the inhibition immunologic function that brings high blood pressure down.
Modern age, clinical almost each section all used, as treat encephalitis B and parotitis, typhoid fever, dysentery, urinary tract infections, gonorrhoea, pneumonia, cellulitis, suppurative dermatosis, otitis media, vasculitis etc., with the treatment of other drug compatibility acute and subacute appendicitis, burn, poliomyelitis, eczema and some fungus-caused skin infectionss, can treat hepatitis, pinworm, stomatitis, lip ulcer, maldigestion, hypertension and arteriosclerosis etc. in addition, therefore, Schuttgelb is used extremely wide clinically.
It not only can be used for medical treatment the physiologically active decision of Schuttgelb, can also be used for health care and daily chemicals, if any the people it is used for hair care and skin care product, also has the people that it is enrolled in the natural pigment and goes.Abroad, people it as laxative.
Past rheum officinale rope is many to be extracted from rheum officinale or giant knotweed with organic solvents such as benzene, pyridines, not only costs an arm and a leg but also causes environmental pollution to cause that human body poisons.
Summary of the invention
The present invention is intended to overcome the defective of Schuttgelb extraction in the past, provides a kind of cost lower, and technology is simple, can not cause environmental pollution to cause the extracting method that human body is poisoned.
In order to realize that with above-mentioned goal of the invention the present invention utilizes poach, chloroform extraction method to extract the rheum officinale rope from giant knotweed, its concrete technical scheme is as follows:
A kind of method for emodin of extracting from giant knotweed is characterized in that: comprise following processing step:
A, get dry giant knotweed rhizome and be ground into powder, add in the entry and boil, extract 25-55min, filter and also collect filtrate;
Filter residue after B, the filtration is according to steps A water extraction 2-5 time, and merging filtrate concentrates;
C, 75% ethanol sedimentation that adding 1.5-3.5 doubly measures in concentrated solution are placed 8-15h and are spent the night, and remove impurity, and underpressure distillation is reclaimed ethanol and obtained mother liquor;
D, add chloroform in mother liquor, jolting is placed to chloroform layer and the safran precipitation occurs and separate out, and leaches precipitation, with chloroform extraction 2 times, merges precipitation as above-mentioned method, with acetone recrystallization 2 times, safran needle crystal.
The mass volume ratio of giant knotweed rhizome powder and water is 1 in steps A: 7-1: 16.
The mass volume ratio of filter residue and water is 1 in step B: 5-1: 12.
The volume ratio of mother liquor and chloroform is 1 in step D: 0.5-1: 1.5.
The useful technique effect that the present invention brings: what the present invention adopted is that solvent extracts Schuttgelb with water from giant knotweed, and to compare cost lower with organic solvent, and technology is simple, environmental protection and nontoxic.
Embodiment
Embodiment 1
A, dry giant knotweed rhizome is ground into powder, gets 500g and add in the 4000ml water and boil, extract 29min, filter and also collect filtrate;
B, the filter residue after filtering according to steps A with the water extraction of 6 times of amounts 3 times, merging filtrate, concentrated;
C, add 75% ethanol sedimentation of 1.7 times of amounts in concentrated solution, place 9h and spend the night, remove impurity, underpressure distillation is reclaimed ethanol and is obtained mother liquor;
D, add the chloroform of 0.7 times of amount in mother liquor, jolting is placed to chloroform layer and the safran precipitation occurs and separate out, and leaches precipitation, with chloroform extraction 2 times, merges precipitation as above-mentioned method, with acetone recrystallization 2 times, safran needle crystal.
Embodiment 2
A, dry giant knotweed rhizome is ground into powder, gets 750g and add in the 7500ml water and boil, extract 32min, filter and also collect filtrate;
B, the filter residue after filtering according to steps A with the water extraction of 7 times of amounts 4 times, merging filtrate, concentrated;
C, add 75% ethanol sedimentation of 2 times of amounts in concentrated solution, place 11h and spend the night, remove impurity, underpressure distillation is reclaimed ethanol and is obtained mother liquor;
D, add the chloroform of 0.9 times of amount in mother liquor, jolting is placed to chloroform layer and the safran precipitation occurs and separate out, and leaches precipitation, with chloroform extraction 2 times, merges precipitation as above-mentioned method, with acetone recrystallization 2 times, safran needle crystal.
Embodiment 3
A, dry giant knotweed rhizome is ground into powder, gets 1000g and add in the 12000ml water and boil, extract 38min, filter and also collect filtrate;
B, the filter residue after filtering according to steps A with the water extraction of 10 times of amounts 4 times, merging filtrate, concentrated;
C, add 75% ethanol sedimentation of 2.4 times of amounts in concentrated solution, place 13h and spend the night, remove impurity, underpressure distillation is reclaimed ethanol and is obtained mother liquor;
D, add the chloroform of 1.2 times of amounts in mother liquor, jolting is placed to chloroform layer and the safran precipitation occurs and separate out, and leaches precipitation, with chloroform extraction 2 times, merges precipitation as above-mentioned method, with acetone recrystallization 2 times, safran needle crystal.
Embodiment 4
A, dry giant knotweed rhizome is ground into powder, gets 1300g and add in the 19500ml water and boil, extract 50min, filter and also collect filtrate;
B, the filter residue after filtering according to steps A with the water extraction of 11 times of amounts 3 times, merging filtrate, concentrated;
C, add 75% ethanol sedimentation of 3.2 times of amounts in concentrated solution, place 14h and spend the night, remove impurity, underpressure distillation is reclaimed ethanol and is obtained mother liquor;
D, add the chloroform of 1.4 times of amounts in mother liquor, jolting is placed to chloroform layer and the safran precipitation occurs and separate out, and leaches precipitation, with chloroform extraction 2 times, merges precipitation as above-mentioned method, with acetone recrystallization 2 times, safran needle crystal.
Claims (4)
1. one kind is extracted method for emodin from giant knotweed, it is characterized in that: comprise following processing step:
A, get dry giant knotweed rhizome and be ground into powder, add in the entry and boil, extract 25-55min, filter and also collect filtrate;
Filter residue after B, the filtration is according to steps A water extraction 2-5 time, and merging filtrate concentrates;
C, 75% ethanol sedimentation that adding 1.5-3.5 doubly measures in concentrated solution are placed 8-15h and are spent the night, and remove impurity, and underpressure distillation is reclaimed ethanol and obtained mother liquor;
D, add chloroform in mother liquor, jolting is placed to chloroform layer and the safran precipitation occurs and separate out, and leaches precipitation, with chloroform extraction 2 times, merges precipitation as above-mentioned method, with acetone recrystallization 2 times, safran needle crystal.
2. a kind of method for emodin of extracting from giant knotweed according to claim 1, it is characterized in that: the mass volume ratio of giant knotweed rhizome powder and water is 1 in steps A: 7-1: 16.
3. a kind of method for emodin of extracting from giant knotweed according to claim 1, it is characterized in that: the mass volume ratio of filter residue and water is 1 in step B: 5-1: 12.
4. a kind of method for emodin of extracting from giant knotweed according to claim 1, it is characterized in that: the volume ratio of mother liquor and chloroform is 1 in step D: 0.5-1: 1.5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010197882A CN101857538A (en) | 2010-06-10 | 2010-06-10 | Method for extracting frangula emodin from giant knotweed |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010197882A CN101857538A (en) | 2010-06-10 | 2010-06-10 | Method for extracting frangula emodin from giant knotweed |
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| CN101857538A true CN101857538A (en) | 2010-10-13 |
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| CN201010197882A Pending CN101857538A (en) | 2010-06-10 | 2010-06-10 | Method for extracting frangula emodin from giant knotweed |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103193613A (en) * | 2013-03-30 | 2013-07-10 | 浙江工业大学 | Method for separating emodin by means of co-crystallization |
| CN104447270A (en) * | 2014-12-05 | 2015-03-25 | 湖南农业大学 | Method of purifying rheum emodin from by-product after extracting resveratrol from polygonum cuspidatum |
| CN109608321A (en) * | 2019-01-14 | 2019-04-12 | 淮海工学院 | A kind of preparation method of natural origin rheum emodin |
-
2010
- 2010-06-10 CN CN201010197882A patent/CN101857538A/en active Pending
Non-Patent Citations (3)
| Title |
|---|
| 刘晓秋等: "虎杖化学成分研究(Ⅰ)", 《中国中药杂志》 * |
| 张喜云等: "以水为溶媒从虎杖中提取大黄素", 《天津药学》 * |
| 谢扬等: "虎杖活性成分及其提取分离方法研究概况", 《时珍国医国药》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103193613A (en) * | 2013-03-30 | 2013-07-10 | 浙江工业大学 | Method for separating emodin by means of co-crystallization |
| CN104447270A (en) * | 2014-12-05 | 2015-03-25 | 湖南农业大学 | Method of purifying rheum emodin from by-product after extracting resveratrol from polygonum cuspidatum |
| CN109608321A (en) * | 2019-01-14 | 2019-04-12 | 淮海工学院 | A kind of preparation method of natural origin rheum emodin |
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Application publication date: 20101013 |