CN104530749A - Method for extracting natural pigment from bark - Google Patents
Method for extracting natural pigment from bark Download PDFInfo
- Publication number
- CN104530749A CN104530749A CN201410730362.6A CN201410730362A CN104530749A CN 104530749 A CN104530749 A CN 104530749A CN 201410730362 A CN201410730362 A CN 201410730362A CN 104530749 A CN104530749 A CN 104530749A
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- CN
- China
- Prior art keywords
- extraction
- solution
- bark
- myricae rubrae
- rotary evaporators
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B61/00—Dyes of natural origin prepared from natural sources, e.g. vegetable sources
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic 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
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- 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
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0096—Purification; Precipitation; Filtration
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention relates to a method for extracting natural pigments from bark. By a reflux method, flavonol in waxberry bark is extracted. An ethanol buffer solution is used as an extraction solvent with the solid-liquid rate being 1:10. Heat reflux extraction is carried out twice, 3h for each time; and through separation, concentration, layered extraction and freeze-drying, flavonol in waxberry bark is obtained. The extraction rate reaches more than 89%.
Description
Technical field
The present invention relates to a kind of method extracting natural pigment, particularly a kind of method extracting natural pigment from bark.
Background technology
Red bayberry is the subtropical fruit tree originating in China, containing abundant anthocyanogen and polyphenolic compound in red bayberry.The good fruit that red bayberry is not still eaten raw, also has medical care effect.Existing large quantity research shows, the pharmaceutical use of red bayberry is high, and its fruit, benevolence, leaf, Pi Junke are used as medicine.The chemical composition of Cortex Myricae Rubrae, Folium Myricae rubrae and red bayberry fruit stone etc. also has been reported.It is reported that separation obtains flavones and tannin from Cortex Myricae Rubrae, the research in past finds, containing abundant polyphenol, flavonoid compound in Cortex Myricae Rubrae, and such as ampelopsin, Myricitroside etc.
Summary of the invention
The present invention proposes a kind of method extracting natural pigment from shell, the method has the features such as extraction yield is high, aftertreatment is simple, foreign matter content is low.
In order to reach above-mentioned purpose, the concrete technical scheme of employing is:
(1) pick out clean Cortex Myricae Rubrae, be placed in 60 DEG C of baking ovens and dry, pulverized with micronizer mill, then it is sieved;
(2) accurately take the poplar bark powder of 15g, and the massfraction adding 150g is wherein the ethanolic soln of 95%, extraction temperature at 80-85 DEG C, circumfluence distillation 2 times, each 3h;
(3) after above-mentioned solution cooling, with the speed of 400r/min through centrifugation;
(4) liquid after separation is gone out after residue, evaporate 2-3h through Rotary Evaporators, recycling design;
(5) concentrated solution is dissolved in the distilled water of 150mL, the low-pole material such as wax, pigment, grease of going out with sherwood oil in solution, then carries out layering extraction with saturated silicagel column;
(6) solution after extraction goes out desolventizing through Rotary Evaporators, obtains Cortex Myricae Rubrae extract sample, i.e. flavonol through lyophilize.
Specific embodiments
From bark, extract a method for natural pigment, method is:
(1) pick out clean Cortex Myricae Rubrae, be placed in 60 DEG C of baking ovens and dry, pulverized with micronizer mill, then it is sieved;
(2) accurately take the poplar bark powder of 15g, and the massfraction adding 150g is wherein the ethanolic soln of 95%, extraction temperature at 80-85 DEG C, circumfluence distillation 2 times, each 3h;
(3) after above-mentioned solution cooling, with the speed of 400r/min through centrifugation;
(4) liquid after separation is gone out after residue, evaporate 2-3h through Rotary Evaporators, recycling design;
(5) concentrated solution is dissolved in the distilled water of 150mL, the low-pole material such as wax, pigment, grease of going out with sherwood oil in solution, then carries out layering extraction with saturated silicagel column;
(6) solution after extraction goes out desolventizing through Rotary Evaporators, obtains Cortex Myricae Rubrae extract sample, i.e. flavonol, and detect its extraction yield through lyophilize.
Example 1
Pick out clean Cortex Myricae Rubrae, be placed in 60 DEG C of baking ovens and dry, pulverized with micronizer mill, then it is sieved; Accurately take the poplar bark powder of 15g, and the massfraction adding 150g is wherein the ethanolic soln of 95%, extraction temperature at 80 DEG C, circumfluence distillation 2 times, each 3h; After above-mentioned solution cooling, with the speed of 400r/min through centrifugation; Liquid after separation is gone out after residue, evaporate 2h through Rotary Evaporators, recycling design; Concentrated solution is dissolved in the distilled water of 150mL, the low-pole material such as wax, pigment, grease of going out with sherwood oil in solution, then carries out layering extraction with saturated silicagel column; Solution after extraction goes out desolventizing through Rotary Evaporators, obtains Cortex Myricae Rubrae extract sample, i.e. flavonol through lyophilize, and detects its extraction rate reached more than 89%.
Example 2
Pick out clean Cortex Myricae Rubrae, be placed in 60 DEG C of baking ovens and dry, pulverized with micronizer mill, then it is sieved; Accurately take the poplar bark powder of 15g, and the massfraction adding 150g is wherein the ethanolic soln of 95%, extraction temperature at 83 DEG C, circumfluence distillation 2 times, each 3h; After above-mentioned solution cooling, with the speed of 400r/min through centrifugation; Liquid after separation is gone out after residue, evaporate 2.5h through Rotary Evaporators, recycling design; Concentrated solution is dissolved in the distilled water of 150mL, the low-pole material such as wax, pigment, grease of going out with sherwood oil in solution, then carries out layering extraction with saturated silicagel column; Solution after extraction goes out desolventizing through Rotary Evaporators, obtains Cortex Myricae Rubrae extract sample, i.e. flavonol through lyophilize, and detects its extraction rate reached more than 89%.
Example 3
Pick out clean Cortex Myricae Rubrae, be placed in 60 DEG C of baking ovens and dry, pulverized with micronizer mill, then it is sieved; Accurately take the poplar bark powder of 15g, and the massfraction adding 150g is wherein the ethanolic soln of 95%, extraction temperature at 85 DEG C, circumfluence distillation 2 times, each 3h; After above-mentioned solution cooling, with the speed of 400r/min through centrifugation; Liquid after separation is gone out after residue, evaporate 3h through Rotary Evaporators, recycling design; Concentrated solution is dissolved in the distilled water of 150mL, the low-pole material such as wax, pigment, grease of going out with sherwood oil in solution, then carries out layering extraction with saturated silicagel column; Solution after extraction goes out desolventizing through Rotary Evaporators, obtains Cortex Myricae Rubrae extract sample, i.e. flavonol through lyophilize, and detects its extraction rate reached more than 89%.
Claims (1)
1. from bark, extract a method for natural pigment, it is characterized in that:
(1) pick out clean Cortex Myricae Rubrae, be placed in 60 DEG C of baking ovens and dry, pulverized with micronizer mill, then it is sieved;
(2) accurately take the poplar bark powder of 15g, and the massfraction adding 150g is wherein the ethanolic soln of 95%, extraction temperature at 80-85 DEG C, circumfluence distillation 2 times, each 3h;
(3) after above-mentioned solution cooling, with the speed of 400r/min through centrifugation;
(4) liquid after separation is gone out after residue, evaporate 2-3h through Rotary Evaporators, recycling design;
(5) concentrated solution is dissolved in the distilled water of 150mL, the low-pole material such as wax, pigment, grease of going out with sherwood oil in solution, then carries out layering extraction with saturated silicagel column;
(6) solution after extraction goes out desolventizing through Rotary Evaporators, obtains Cortex Myricae Rubrae extract sample, i.e. flavonol through lyophilize.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410730362.6A CN104530749A (en) | 2014-12-04 | 2014-12-04 | Method for extracting natural pigment from bark |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410730362.6A CN104530749A (en) | 2014-12-04 | 2014-12-04 | Method for extracting natural pigment from bark |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104530749A true CN104530749A (en) | 2015-04-22 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410730362.6A Pending CN104530749A (en) | 2014-12-04 | 2014-12-04 | Method for extracting natural pigment from bark |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104530749A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105037313A (en) * | 2015-06-26 | 2015-11-11 | 湖南医药学院 | Method for simply separating myricetrin and catechin in bark of waxberry tree |
| CN106046852A (en) * | 2016-07-15 | 2016-10-26 | 广西顺帆投资有限公司 | Method for extracting dye based on waxberry tree barks |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1872848A (en) * | 2005-05-30 | 2006-12-06 | 广州汉方现代中药研究开发有限公司 | Method for distilling myricetin from plant |
| CN101838255A (en) * | 2010-05-07 | 2010-09-22 | 湖州四丰生物科技有限公司 | Myricetin extraction process |
-
2014
- 2014-12-04 CN CN201410730362.6A patent/CN104530749A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1872848A (en) * | 2005-05-30 | 2006-12-06 | 广州汉方现代中药研究开发有限公司 | Method for distilling myricetin from plant |
| CN101838255A (en) * | 2010-05-07 | 2010-09-22 | 湖州四丰生物科技有限公司 | Myricetin extraction process |
Non-Patent Citations (1)
| Title |
|---|
| 刘同方 等: ""杨梅素植物来源及提取分离方法研究进展"", 《安徽农业科学》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105037313A (en) * | 2015-06-26 | 2015-11-11 | 湖南医药学院 | Method for simply separating myricetrin and catechin in bark of waxberry tree |
| CN105037313B (en) * | 2015-06-26 | 2017-09-26 | 湖南医药学院 | A kind of method of myricetrin and catechin compounds in separation Chinese waxmyrtle bark |
| CN106046852A (en) * | 2016-07-15 | 2016-10-26 | 广西顺帆投资有限公司 | Method for extracting dye based on waxberry tree barks |
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| PB01 | Publication | ||
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| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20150422 |