CN102532219A - Method for enriching and purifying anthocyanin in lonicera caerulea - Google Patents
Method for enriching and purifying anthocyanin in lonicera caerulea Download PDFInfo
- Publication number
- CN102532219A CN102532219A CN2010106229637A CN201010622963A CN102532219A CN 102532219 A CN102532219 A CN 102532219A CN 2010106229637 A CN2010106229637 A CN 2010106229637A CN 201010622963 A CN201010622963 A CN 201010622963A CN 102532219 A CN102532219 A CN 102532219A
- Authority
- CN
- China
- Prior art keywords
- anthocyanogen
- enriching
- lonicera edulis
- anthocyanin
- utilizing
- 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.)
- Pending
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention belongs to the field of natural organic chemistry, and relates to a method for enriching and purifying anthocyanin in lonicera caerulea by using macroporous adsorbent resin. The method is characterized in that: the anthocyanin is separated and purified by using a macroporous adsorption technology, the adsorptive selectivity to the anthocyanin is good, the adsorption speed and the resolution speed are high, and the adsorption capacity is high; the anthocyanin is extracted conveniently and fast, raw materials are rich in source, the production cost is low, the separation effect is obvious, the extraction purity is high, and an anthocyanin semifinished product containing over 35 percent of the anthocyanin and an anthocyanin finished product containing over 95 percent of the anthocyanin can be obtained; and the defects of low conventional extraction rate and low extraction purity are overcome. According to the method disclosed by the invention, the macroporous adsorbent resin which is stable in physicochemical property, large in surface area, high in exchange rate, high in mechanical strength, strong in anti-pollution capacity and high in thermal stability is used, so that the anthocyanin can be selectively adsorbed from a solution through physical adsorption, the adsorption speed and the resolution speed are high, and the adsorption capacity is high.
Description
Technical field:
The invention belongs to the natural organic chemistry field, relate to the purification process of a kind of anthocyanogen, particularly relate to a kind of method of utilizing anthocyanogen in the enriching and purifying macroporous resin Lonicera edulis Turcz..
Background technology:
Lonicera edulis Turcz. is named indigo fruit, goat milk, black bear fruit, Brachybotrys paridiformis fruit, blue fruit again, is the perennial machaka of Caprifoliaceae Lonicera.Fruit is a berry, is rich in carbohydrate, organic acid, and mineral substance, multivitamin and trace element have higher nutritive value and pharmaceutical use, are the ideal nutritive health-care foods.Fruit can be eaten raw, can be processed into beverage, is suitable for extracting natural mauve pigment.Seed contains anthocyanogen, and the complete stool leaf contains aucubin, has certain medical value.Contain Kuromanine in the Lonicera edulis Turcz., leucocyanidin glycosides, material such as catechuic acid and rue are sweet; Through the clinical trial checking cardiovascular and cerebrovascular diseases there is certain curative effect, also can prevents angiorrhexis, bring high blood pressure down; And have antiviral, anticancer and improve effects such as liver detoxification effect.
Anthocyanogen is a cyanidin(e) and the compounds of sugar with the glycosidic link be combined into, extensively is present in the enchylema of flower, fruit, stem, leaf and root organ of plant, and it is appeared by red, purplish red to different colours such as orchids.Anthocyanogen is a flavonoid---can present a red compounds of group in one type of material being the basis with flavones nuclear.In recent years, it is found that and contain a large amount of anthocyanogen in the natural phant Lonicera edulis Turcz.,, therefrom extract anthocyanogen and obtained encouraging progress because its raw material Lonicera edulis Turcz. source is wider.Name is called just to disclose in the patented claim of " preparation technology of purifying Lonicera edulis anthocyanin by using macroporous resin " carries out the technical process of resin column absorption anthocyanogen with Lonicera edulis Turcz. after alcohol extracting.Anthocyanogen extraction process in the above-mentioned patent documentation mainly is to form through cross step extractions such as resin column with acid adjustment behind the extraction using alcohol, and its separating effect is nothing like macroporous adsorbent resin processing back and is carrying out the isolating effect of silica gel column chromatography.
Summary of the invention:
The objective of the invention is to overcome shortcomings such as the routine techniques extraction yield is relatively low, dna purity is low, a kind of method of utilizing anthocyanogen in the enriching and purifying macroporous resin Lonicera edulis Turcz. is provided.
For realizing above-mentioned purpose, the technical scheme that the present invention adopts is:
A kind of method of utilizing anthocyanogen in the enriching and purifying macroporous resin Lonicera edulis Turcz., its step is following:
(1) dried Lonicera edulis Turcz. being pulverized the back extracts with alcohol heating reflux;
(2) will the extracting solution decompression recycling ethanol be got primary extract through the Lonicera edulis Turcz. extracting solution suction filtration of step (1) processing;
(3) use acid to transfer its pH value obtaining primary extract to be 2.0～2.3, to leave standstill, suction filtration and be washed with water to neutrality, the anthocyanogen crude extract;
(4) gained anthocyanogen crude extract is adsorbed with macroporous adsorbent resin;
(5) with Different concentrations of alcohol macroporous adsorbent resin is carried out wash-out, follow the tracks of with tlc and detect, collect each stepwise elution liquid of anthocyanogen;
(6) each stepwise elution liquid of anthocyanogen is concentrated recovery ethanol, get the anthocyanogen work in-process, its content is more than 35%;
(7) with silica gel column chromatography on the gained anthocyanogen work in-process, and with acetone, methyl alcohol carries out wash-out with the different volumes ratio, and tlc is followed the tracks of and detected, and collects each stepwise elution liquid of anthocyanogen;
(8) with collected anthocyanogen elutriant, adopt activated carbon decolorizing, recrystallization method refining anthocyanogen, its content is more than 95%.
In the described step (1), cross 40～80 mesh sieves after Lonicera edulis Turcz. is pulverized and carrying out organic solvent extraction.
In the described step (1), alcohol concn is 70%, extracts each 2 hours 3 times.
In the described step (1), the method for extraction is one or more in infusion method, reflux extraction, percolation, decocting method, the continuous extraction.
In the described step (1), adding the alcoholic acid volume is 15～20 times that Lonicera edulis Turcz. is pulverized volume.
In the described step (3), regulating the used acid of pH value is hydrochloric acid.
Used macroporous adsorbent resin is a kind of in Tianjin the Nankai University X-5, NKA-9, S-8, D 3520, D4006, H103, D4020, AB-8H and the NKA-II type resin that are produced in the described step (4), is adsorbed as Static Adsorption or dynamic adsorption.
Wash-out described in the described step (5) carries out wash-out for the ethanol with 30～90%.
Described in step (5) and (7), the detection method of being taked is tlc and follows the tracks of detection.
The acetone of being taked in the described step (7) and the volume of methyl alcohol are 1～7: 1.
The present invention uses macroporous absorption technology separation and purification anthocyanogen, and good to the adsorption selectivity of anthocyanogen, the fast parsing of absorption is also fast, and loading capacity is bigger; Extract convenient and swiftly, raw material sources are abundant, low production cost; Separating effect is obvious; Dna purity is high, can obtain anthocyanogen work in-process and content the anthocyanogen finished product 95% or more of content more than 35%, has overcome the shortcoming that conventional extraction yield is relatively low, dna purity is low.
The present invention selects that physico-chemical property is stable, surface-area is big, exchange velocity is very fast, physical strength is high, contamination resistance is strong, the macroporous adsorbent resin of Heat stability is good for use; Be not dissolved in acid, alkali and organic matchmaker; Better to the organism selectivity, as not existed by inorganic salts and strong ion low molecular compound influence can be adsorbed anthocyanogen selectively through physical adsorption from solution; Absorption is fast, parsing is also fast, and loading capacity is bigger.
Embodiment:
Embodiment 1: a kind of method of utilizing anthocyanogen in the enriching and purifying macroporous resin Lonicera edulis Turcz., and its step is following:
(1) dried Lonicera edulis Turcz. is pulverized the back and cross 60 mesh sieves, amass 15 times alcohol reflux 3 times, each 2 hours with the Lonicera edulis Turcz. powder;
(2) will the extracting solution decompression recycling ethanol be got primary extract through the Lonicera edulis Turcz. extracting solution suction filtration of step (1) processing;
(3) use acid to transfer its pH value obtaining primary extract to be 2.3, to leave standstill, suction filtration, decompression and solvent recovery get the Lonicera edulis Turcz. crude extract;
(4) with gained Lonicera edulis Turcz. crude extract with adsorbing on the macroporous adsorption resin chromatography post, used macroporous resin is the NKA-II type resin that Tianjin Nankai University is produced;
(5) in macroporous adsorbent resin layer post, carry out gradient elution successively with 30%, 40%, 50%, 60%, 70%, 80%, 90% ethanol, follow the tracks of with tlc and detect, collect each stepwise elution liquid of anthocyanogen;
(6) each stepwise elution liquid of anthocyanogen is concentrated recovery ethanol, obtaining content is 35% anthocyanogen work in-process;
(7) with silica gel column chromatography on the gained anthocyanogen work in-process, and use acetone, methyl alcohol carries out gradient elution with 1: 1,2: 1,3: 1,4: 1,5: 1,6: 1,7: 1 volume ratio successively, and tlc is followed the tracks of and detected, and collects each stepwise elution liquid of anthocyanogen;
(8), adopt activated carbon decolorizing, recrystallization method to make with extra care and obtain content 95% anthocyanogen with collected anthocyanogen elutriant.
Case study on implementation 2: a kind of method of utilizing anthocyanogen in the enriching and purifying macroporous resin Lonicera edulis Turcz., its step is following:
(1) dried Lonicera edulis Turcz. is pulverized the back and cross 80 mesh sieves, amass 20 times alcohol reflux 3 times, each 2 hours with the Lonicera edulis Turcz. powder;
(2) will the extracting solution decompression recycling ethanol be got primary extract through the Lonicera edulis Turcz. extracting solution suction filtration of step (1) processing;
(3) use acid to transfer its pH value obtaining primary extract to be 2.2, to leave standstill, suction filtration, decompression and solvent recovery get the Lonicera edulis Turcz. crude extract;
(4) gained anthocyanogen crude extract is adsorbed with macroporous adsorbent resin, used macroporous resin is the D4006 type resin that Tianjin Nankai University is produced;
(5) carry out wash-out with 30%, 50%, 70%, 90% ethanol at macroporous adsorbent resin, follow the tracks of with tlc and detect, collect each stepwise elution liquid of anthocyanogen;
(6) each stepwise elution liquid of anthocyanogen is concentrated recovery ethanol, obtain content 35.8% anthocyanogen work in-process;
(7) with silica gel column chromatography on the gained anthocyanogen work in-process, and use acetone, methyl alcohol carries out gradient elution with 1: 1,2: 1,3: 1,4: 1,5: 1,6: 1,7: 1 volume ratio successively, and tlc is followed the tracks of and detected, and collects each stepwise elution liquid of anthocyanogen;
(8), adopt activated carbon decolorizing, recrystallization method to make with extra care and obtain content 95% anthocyanogen with collected anthocyanogen elutriant.
Case study on implementation 3: a kind of method of utilizing anthocyanogen in the enriching and purifying macroporous resin Lonicera edulis Turcz., its step is following:
(1) dried Lonicera edulis Turcz. is pulverized the back and cross 40 mesh sieves, the ethanol that the Lonicera edulis Turcz. powder is long-pending 20 times returns and extracts each 2 hours 3 times;
(2) will be through the Lonicera edulis Turcz. extracting solution suction filtration of step (1) processing, the extracting solution decompression recycling ethanol gets primary extract;
(3) obtaining primary extract is transferred its pH value 2.0 with acid, leave standstill suction filtration, decompression and solvent recovery gets the anthocyanogen crude extract;
(4) with gained anthocyanogen crude extract with the macroporous adsorption resin chromatography pillar, on adsorb, used macroporous resin is the NKA-9 type resin that Tianjin Nankai University is produced;
(5) in the macroporous adsorption resin chromatography pillar, carry out gradient elution successively with 40%, 60%, 80% ethanol, follow the tracks of with tlc and detect, collect each stepwise elution liquid of anthocyanogen;
(6) each stepwise elution liquid of anthocyanogen is concentrated recovery ethanol, obtain content 36.7% anthocyanogen work in-process;
(7) with silica gel column chromatography on the gained anthocyanogen work in-process, and use acetone, methyl alcohol carries out gradient elution with 1: 1,2: 1,3: 1,4: 1,5: 1,6: 1,7: 1 volume ratio successively, and tlc is followed the tracks of and detected, and collects each stepwise elution liquid of anthocyanogen;
(8), adopt activated carbon decolorizing, recrystallization method to make with extra care and obtain content 96.2% anthocyanogen with collected pattern elutriant.
Claims (10)
1. a method of utilizing anthocyanogen in the enriching and purifying macroporous resin Lonicera edulis Turcz. is characterized in that, its step is following:
(1) dried Lonicera edulis Turcz. being pulverized the back extracts with alcohol heating reflux;
(2) the Lonicera edulis Turcz. extracting liquid filtering that will handle through (1) reclaims ethanol and gets primary extract;
(3) with institute results primary extract with adjust pH to 2-2.3, separate, the collecting precipitation thing, and be washed with water to neutrality, obtain the crude extract of anthocyanogen.
(4) gained anthocyanogen crude extract is adsorbed with macroporous adsorbent resin;
(5) with the different concentration ethanol aqueous solution macroporous adsorbent resin is carried out wash-out, collect each stepwise elution liquid of anthocyanogen;
(6) the anthocyanogen elutriant is concentrated the recovery eluent, get the anthocyanogen work in-process;
(7) with silica gel column chromatography on the gained anthocyanogen work in-process, and with methyl alcohol, acetone carries out wash-out with the different volumes ratio, collects each stepwise elution liquid of anthocyanogen;
(8) collected anthocyanogen elutriant is carried out the purified anthocyanogen.
2. its speciality of method of anthocyanogen in the enriching and purifying macroporous resin Lonicera edulis Turcz. of utilizing according to claim 1 and 2 is: in the described step (1), cross 40～80 mesh sieves behind the Lonicera edulis Turcz. powder and carry out the alcohol heating reflux extraction again.
3. the method for utilizing anthocyanogen in the enriching and purifying macroporous resin Lonicera edulis Turcz. according to claim 1 and 2 is characterized in that: in affiliated step (1), the ethanol alcoholic degree is 70%, can extract each 2 hours 3 times.
4. the method for utilizing anthocyanogen in the enriching and purifying macroporous resin Lonicera edulis Turcz. according to claim 3; It is characterized in that: in the described step (1); The method of extracting is pickling process, reflux extraction, one or more in percolation, decocting method, the continuous extraction.
5. the method for utilizing anthocyanogen in the enriching and purifying macroporous resin Lonicera edulis Turcz. according to claim 3 is characterized in that; Under step (1) in, add volume that ethanol gets and be long-pending 15～20 times of Lonicera edulis Turcz. powder.
6. the method for utilizing anthocyanogen in the enriching and purifying macroporous resin Lonicera edulis Turcz. according to claim 5 is characterized in that: in described step (3), regulating the used acid of pH value is hydrochloric acid.
7. the method for utilizing anthocyanogen in the enriching and purifying macroporous resin Lonicera edulis Turcz. according to claim 6 is characterized in that: be adsorbed as Static Adsorption or dynamic adsorption described in the step (4): the wash-out described in the step (5) carries out wash-out for the aqueous ethanolic solution with 30～90%.
8. the method for utilizing anthocyanogen in the enriching and purifying macroporous resin Lonicera edulis Turcz. according to claim 7 is characterized in that: in step (5) and (7), adopt tlc to follow the tracks of in the elution process and detect.
9. the method for utilizing anthocyanogen in the enriching and purifying macroporous resin Lonicera edulis Turcz. according to claim 8 is characterized in that: in the step (7) the acetone that adopts and methyl alcohol to get volume ratio be 1～7: 1.
10. the method for utilizing anthocyanogen in the enriching and purifying macroporous resin Lonicera edulis Turcz. according to claim 7 is characterized in that: in step (8), adopt activated carbon decolorizing, recrystallization method to make with extra care.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010106229637A CN102532219A (en) | 2010-12-20 | 2010-12-20 | Method for enriching and purifying anthocyanin in lonicera caerulea |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010106229637A CN102532219A (en) | 2010-12-20 | 2010-12-20 | Method for enriching and purifying anthocyanin in lonicera caerulea |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102532219A true CN102532219A (en) | 2012-07-04 |
Family
ID=46340376
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010106229637A Pending CN102532219A (en) | 2010-12-20 | 2010-12-20 | Method for enriching and purifying anthocyanin in lonicera caerulea |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102532219A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103073912A (en) * | 2012-12-13 | 2013-05-01 | 大兴安岭林格贝有机食品有限责任公司 | Method for preparing purified azalea from rhododendron dauricum |
| CN105418572A (en) * | 2015-11-06 | 2016-03-23 | 大兴安岭林格贝寒带生物科技股份有限公司 | Method for extracting whortleberry anthocyanidin in microwave countercurrent mode and adsorbing and purifying whortleberry anthocyanidin through macroporous adsorbent resin |
| CN106117285A (en) * | 2016-06-14 | 2016-11-16 | 吉林大学 | High-pressure pulse electric auxiliary acidization ethanol extraction Lonicera edulis anthocyanin technique |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1068609A (en) * | 1963-08-09 | 1967-05-10 | Chibret Lab | Process for the isolation of anthocyanidin glycosides |
| CN101434972A (en) * | 2008-12-12 | 2009-05-20 | 东北林业大学 | Process for preparing Lonicera edulis anthocyanin by solid state biological reaction |
| CN101463056A (en) * | 2007-12-20 | 2009-06-24 | 东北林业大学 | Preparation technique for purifying Lonicera edulis anthocyanin by using macroporous resin |
-
2010
- 2010-12-20 CN CN2010106229637A patent/CN102532219A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1068609A (en) * | 1963-08-09 | 1967-05-10 | Chibret Lab | Process for the isolation of anthocyanidin glycosides |
| CN101463056A (en) * | 2007-12-20 | 2009-06-24 | 东北林业大学 | Preparation technique for purifying Lonicera edulis anthocyanin by using macroporous resin |
| CN101434972A (en) * | 2008-12-12 | 2009-05-20 | 东北林业大学 | Process for preparing Lonicera edulis anthocyanin by solid state biological reaction |
Non-Patent Citations (2)
| Title |
|---|
| MONICA JORDHEIM，等: "Anthocyanins in Caprifoliaceae", 《BIOCHEMICAL SYSTEMATICS ECOLOGY》, vol. 35, no. 3, 31 March 2007 (2007-03-31) * |
| 卢钰，等: "花色苷研究进展", 《山东农业大学学报（自然科学版）》, vol. 35, no. 2, 20 June 2004 (2004-06-20), pages 315 - 320 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103073912A (en) * | 2012-12-13 | 2013-05-01 | 大兴安岭林格贝有机食品有限责任公司 | Method for preparing purified azalea from rhododendron dauricum |
| CN103073912B (en) * | 2012-12-13 | 2015-08-26 | 大兴安岭林格贝寒带生物科技股份有限公司 | A kind of Folium Cuculus polioephalus prepares the method for purifying azalea |
| CN105418572A (en) * | 2015-11-06 | 2016-03-23 | 大兴安岭林格贝寒带生物科技股份有限公司 | Method for extracting whortleberry anthocyanidin in microwave countercurrent mode and adsorbing and purifying whortleberry anthocyanidin through macroporous adsorbent resin |
| CN105418572B (en) * | 2015-11-06 | 2019-02-12 | 大兴安岭林格贝寒带生物科技股份有限公司 | It is extracted using microwave counter current, the method for macroporous absorbent resin adsorption and purification whortle anthocyanidin |
| CN106117285A (en) * | 2016-06-14 | 2016-11-16 | 吉林大学 | High-pressure pulse electric auxiliary acidization ethanol extraction Lonicera edulis anthocyanin technique |
| CN106117285B (en) * | 2016-06-14 | 2019-01-11 | 吉林大学 | High-pressure pulse electric auxiliary acidization ethyl alcohol extracts Lonicera edulis anthocyanin technique |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102106931B (en) | Method for producing diverse extracts of berry tea | |
| CN102078339B (en) | Method for enriching and purifying common phellinus fungus general flavone in common phellinus fungus | |
| CN101074188B (en) | Method for enriching and purifying veralkcohol from peanut root by macporous adsorptive resin | |
| CN102070688A (en) | Method for enriching and purifying icariin in epimedium herb | |
| CN101812137A (en) | Method for enriching agaric polysaccharide in purified black agaric by using macroporous absorption resin | |
| CN102093458B (en) | Method for enriching and purifying betulin in birch barks | |
| CN102093328B (en) | Method for enriching and purifying procyanidin in pine bark | |
| CN107245113A (en) | Corn silk polysaccharide extract with antitumaous effect and preparation method thereof | |
| CN104892717B (en) | A kind of technical grade preparative liquid chromatography separation method of momordica glycoside V | |
| CN102060693B (en) | Method for enriching and purifying ferulic acid in cimicifugae foetidae | |
| CN102532219A (en) | Method for enriching and purifying anthocyanin in lonicera caerulea | |
| CN102070569B (en) | Method for enriching and purifying 3,4-divanillyltetrahydrofuran in nettle | |
| CN104711300B (en) | The preparation method of icariine | |
| CN102070685A (en) | Method for enriching and purifying arctiin from burdock | |
| CN103059037B (en) | A kind of method of Chelidonine in enriching and purifying greater celandine | |
| CN104262314B (en) | Black rice anthocyanin preparation technology | |
| CN101732391B (en) | Method for enriching and purifying cardiac glycoside of wormseed mustard herb | |
| CN102920727B (en) | Method for preparing extracts rich in vitexin rhamnoside and vitexin glucoside | |
| CN101775016B (en) | Method for enriching and purifying folic acid in houseleek by macroporous absorbent resin | |
| CN102690359B (en) | A kind of method extracting starch and cucurbitacin from Fructus Momordicae tuber | |
| CN101747402B (en) | Method for enriching and purifying malol in sedum kamtschaticum | |
| CN103110689A (en) | Novel method for extracting astragaloside from radix astragali | |
| CN102070443B (en) | Method for enriching and purifying veratric acid in globeflower | |
| CN107213180A (en) | A kind of separating and extracting process of pseudo-ginseng flavones | |
| CN107235988A (en) | A kind of extracting method of qinghaosu and Artemisitene |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20120704 |