CN1308322C - Method for preparing anthocyanidin - Google Patents
Method for preparing anthocyanidin Download PDFInfo
- Publication number
- CN1308322C CN1308322C CNB031399959A CN03139995A CN1308322C CN 1308322 C CN1308322 C CN 1308322C CN B031399959 A CNB031399959 A CN B031399959A CN 03139995 A CN03139995 A CN 03139995A CN 1308322 C CN1308322 C CN 1308322C
- Authority
- CN
- China
- Prior art keywords
- anthocyanidin
- acetone
- rice husk
- temperature
- preparing
- 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.)
- Expired - Fee Related
Links
Abstract
The present invention relates to a preparation method of anthocyanidin with stable color and strong coloring power. The method comprises the following steps: (1) wild rice husk is mixed with 60 to 70% of water-bearing alcohol by the proportion that each gram of wild rice husk uses 8 milliliters of 60 to 70% of water-bearing alcohol; (2) at the temperature of 60 to 64DEG C, the mixed liquid of the wild rice husk and 60 to 70% of water-bearing alcohol is extracted for 3 to 5 times by reflux; (3) after filtration and reflux, the obtained mixed liquid is extracted, and alcohol extracted liquid is obtained; (4) after alcohol in the alcohol extracting liquid is removed, anthocyanidin water solution is obtained; (5) the anthocyanidin water solution passes through resin columns; after adsorption is saturated, water is used as eluent; the flow velocity of elution columns is controlled to be 0.5 ml/min, and water washing is carried out to Molish reaction negative; (6) after the resin columns are eluted with 65 to 75% of acetone, acetone eluent is obtained; (7) at the temperature of 60 to 64DEG C, the acetone in the acetone eluent is removed. Compared with the prior art, the wild rice anthocyanidin obtained by the preparation method of the present invention has stronger coloring power than that of the original technology product; color gradation is stable, and since the temperature processing of the integral technical process does not exceed 65 DEG C, pigment stability is favorable.
Description
[affiliated technical field]
The present invention relates to a kind of method for preparing anthocyanidin, particularly a kind of method for preparing black rice husk anthocyanidin.
[background technology]
Anthocyanidin extensively is present in flower, fruit and the rhizome of plant, is the main colour developing composition in the plant, belongs to flavonoid compound.It is found that afterwards that anthocyanidin had multiple physiological action, it can regulate the perviousness of capillary vessel, keeps the integrity of cytolemma, and has powerful anti-oxidant function.Discover that further anthocyanidin has synthetic, pre-preventing thrombosis and the effects such as arteriosclerosis, anticancer enzymic activity that promote rhodopsin, has been used for ophthalmic medical field, treatment of arthritis disease and urinary tract infections at present and has been used for the production functional health product.
Anthocyanidin content in the black rice is higher, extracts the technology of natural pigment from black rice, the originally main method of recording in " foodstuff additive national standard " that adopts, and promptly with behind the extraction using alcohol, the dried powder that obtains after the extracting solution spraying drying.In the former technology not to the purge process of pigment, and in treating processes factor affecting such as high temperature, product black rice pigments color instability, tinting strength is relatively poor, basic the use in actual production.
[summary of the invention]
The product color instability that obtains for the method that solves existing preparation black rice husk anthocyanidin, the problem of tinting strength difference the invention provides the preparation method of the black rice husk anthocyanidin of a kind of colour stable, strong coloring force.
(1) with the ratio of 8 milliliter of 60～70% aqueous ethanol of every gram black rice husk black rice husk is mixed with 60～70% aqueous ethanols;
(2) under 60～64 ℃ of temperature, the mixed-liquor return of black rice husk and 60～70% aqueous ethanols is extracted 3～5 times;
(3) mixed solution of filtration refluxing extraction gained gets ethanol extract;
(4) remove ethanol in the ethanol extract, the anthocyanidin aqueous solution;
(5) with resin column on the anthocyanidin aqueous solution, wait to adsorb saturated after, water is cooked elutriant, control wash-out column flow rate is 0.5ml/min, is washed to the Molish reaction negative;
(6), get the acetone elutriant with 65～75% acetone wash-out resin columns;
(7) under 60～64 ℃ of temperature, remove the acetone in the acetone elutriant.
Compared to prior art, stronger by the black rice anthocyanidin tinting strength of preparation method's gained of the present invention, color range stable than former process products, and because whole technological process Temperature Treatment is no more than 65 ℃, pigment stability is better.
[embodiment]
The invention will be further described below in conjunction with specific embodiment.
The preparation method of anthocyanidin of the present invention may further comprise the steps.
1. from black rice husk, extract anthocyanidin:
Black rice after the shelling is ground off crust, go a meter core to get the black rice skin, ratio in 8 milliliter of 60%～70% aqueous ethanol of every gram black rice husk is mixed black rice husk with 60%～70% aqueous ethanol, aqueous ethanol is preferably 65% aqueous ethanol, under 60～64 ℃ of temperature, preferred temperature is 60 ℃, refluxing extraction 3～5 times, be preferably 3 times, each 2 hours, extracting solution got ethanol extract after filtering with plate-and-frame filter press, merge ethanol extract, under 60～64 ℃ of temperature, preferred temperature is 60 ℃, vacuum concentration, remove ethanol, obtain the anthocyanidin aqueous solution.Solution colour is red.
2. purifying anthocyanidin:
With resin column on the anthocyanidin aqueous solution behind the vacuum concentration, polymeric adsorbent can be AB-8 type macroporous adsorbent resin, also can select D4006 type macroporous adsorbent resin for use, wait to adsorb saturated after, water is cooked elutriant, control resin column flow velocity is 0.5 ml/min, is washed to till the Molish reaction negative, and at this moment the resin in the adsorption column is absorption anthocyanidin resin, use 65～75% acetone wash-outs then, be preferably 70% acetone, be eluted to the resin column effluent colourless till, the acetone elutriant, with the acetone elutriant at 60～64 ℃ of following vacuum concentration of temperature, preferred temperature is 60 ℃, then with the lyophilize of gained solution, gets anthocyanidin purifying thing.
Because the black rice anthocyanidin tinting strength of preparation method's gained of the present invention is stronger than former process products, color range stable, and because whole technological process Temperature Treatment is no more than 65 ℃, pigment stability is better.
Although the present invention describes with reference to specific embodiment, this description and not meaning that is construed as limiting the present invention.With reference to description of the invention, other distortion of the disclosed embodiments all can be expected for those skilled in the art.Therefore, such distortion can not break away from affiliated claim restricted portion and spirit.
Claims (10)
1. method for preparing anthocyanidin, it may further comprise the steps:
(1) with the ratio of 8 milliliter of 60～70% aqueous ethanol of every gram black rice husk black rice husk is mixed with 60～70% aqueous ethanols;
(2) under 60～64 ℃ of temperature, the mixed-liquor return of black rice husk and 60～70% aqueous ethanols is extracted 3～5 times;
(3) mixed solution of filtration refluxing extraction gained gets ethanol extract;
(4) remove ethanol in the ethanol extract, the anthocyanidin aqueous solution;
(5) with resin column on the anthocyanidin aqueous solution, wait to adsorb saturated after, water is cooked elutriant, control wash-out column flow rate is 0.5ml/min, is washed to the Molish reaction negative;
(6), get the acetone elutriant with 65～75% acetone wash-out resin columns;
(7) under 60～64 ℃ of temperature, remove the acetone in the acetone elutriant.
2. the method for preparing anthocyanidin according to claim 1 is characterized in that the aqueous ethanol in the step (1) is 65% aqueous ethanol.
3. the method for preparing anthocyanidin according to claim 1 is characterized in that the temperature in the step (2) is 60 ℃.
4. the method for preparing anthocyanidin according to claim 3 is characterized in that step (2) comprises that the mixed-liquor return with black rice husk and 60～70% aqueous ethanols extracts each 2 hours 3～5 times.
5. the method for preparing anthocyanidin according to claim 4 is characterized in that the number of times that the mixed-liquor return of black rice husk and 60～70% aqueous ethanols is extracted is 3 times.
6. the method for preparing anthocyanidin according to claim 1 is characterized in that adopting in the step (3) plate-and-frame filter press to filter the mixed solution of refluxing extraction gained.
7. the method for preparing anthocyanidin according to claim 1 is characterized in that step (4) is included under 60 ℃ of the temperature, adopts the vacuum concentration method that ethanol is removed.
8. the method for preparing anthocyanidin according to claim 1 is characterized in that the resin column in the step (5) can be selected AB-8 type macroporous adsorbent resin and D4006 type macroporous adsorbent resin.
9. the method for preparing anthocyanidin according to claim 1 is characterized in that step (7) is included in 60 ℃ of temperature and adopts the vacuum concentration method that acetone is removed down.
10. the method for preparing anthocyanidin according to claim 1 is characterized in that after the step (7) the lyophilize of gained solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031399959A CN1308322C (en) | 2003-07-30 | 2003-07-30 | Method for preparing anthocyanidin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031399959A CN1308322C (en) | 2003-07-30 | 2003-07-30 | Method for preparing anthocyanidin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1580052A CN1580052A (en) | 2005-02-16 |
| CN1308322C true CN1308322C (en) | 2007-04-04 |
Family
ID=34579186
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB031399959A Expired - Fee Related CN1308322C (en) | 2003-07-30 | 2003-07-30 | Method for preparing anthocyanidin |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1308322C (en) |
Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100432091C (en) * | 2007-01-25 | 2008-11-12 | 天津大学 | Method of extracting natural coloring matter anthocyanins in black rice |
| CN101305797B (en) * | 2008-07-17 | 2011-11-16 | 江西国亿生物科技有限公司 | Carotin preparation method and its carotin products |
| CN101723996B (en) * | 2009-12-03 | 2013-03-20 | 中山大学 | Method for separating high-purity anthocyanin monomers from black rice |
| CN101747661B (en) * | 2009-12-22 | 2012-12-05 | 晨光生物科技集团股份有限公司 | Technology for improving ang-kak red pigment quality by utilizing enzyme preparation |
| CN102093329A (en) * | 2011-02-23 | 2011-06-15 | 熊金良 | Method for extracting anthocyanin from melampodium paludosum |
| CN102277008B (en) * | 2011-06-28 | 2013-09-04 | 安徽省科学技术研究院 | Extraction and preparation method of natural Fragaria ananassa Duch haematochrome |
| CN102659871A (en) * | 2012-05-08 | 2012-09-12 | 魏有良 | Method for extracting and refining anthocyanin in black rice |
| CN104262314B (en) * | 2014-09-12 | 2016-08-17 | 长春海涛天然色素有限公司 | Black rice anthocyanin preparation technology |
| CN105018314B (en) * | 2015-08-06 | 2017-07-11 | 墨江地道酒业有限公司 | A kind of purple rice wine rich in anthocyanidin and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1294131A (en) * | 1999-10-20 | 2001-05-09 | 中国科学院沈阳应用生态研究所 | Process for extracting anthoxyanin from cowbeery |
| WO2002017945A1 (en) * | 2000-08-31 | 2002-03-07 | Hauser, Inc. | Efficient method for producing compositions enriched in anthocyanins |
-
2003
- 2003-07-30 CN CNB031399959A patent/CN1308322C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1294131A (en) * | 1999-10-20 | 2001-05-09 | 中国科学院沈阳应用生态研究所 | Process for extracting anthoxyanin from cowbeery |
| WO2002017945A1 (en) * | 2000-08-31 | 2002-03-07 | Hauser, Inc. | Efficient method for producing compositions enriched in anthocyanins |
Non-Patent Citations (4)
| Title |
|---|
| 农牧产品开发 生吉萍 田辉莉 郭晓莲，25，26，黑米色素的提取和特性 1999 * |
| 广州食品工业科技 高爱红 袁海波 童华荣，75.78，天然食用色素——花青素应用研究进展 2001 * |
| 福建农业大学学报 苏金为，233.237，黑米色素的提取和组分分析 1999 * |
| 福建农业大学学报 苏金为，233.237，黑米色素的提取和组分分析 1999;广州食品工业科技 高爱红 袁海波 童华荣，75.78，天然食用色素——花青素应用研究进展 2001;农牧产品开发 生吉萍 田辉莉 郭晓莲，25，26，黑米色素的提取和特性 1999 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1580052A (en) | 2005-02-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105949163B (en) | The method for extraction and purification of anthocyanidin in a kind of Black Box Tracing pomace | |
| CN107556364B (en) | Method for extracting abalone protein peptide by subcritical water assisted enzymolysis and product | |
| CN107281252B (en) | Preparation method of vaccinium myrtillus extract | |
| JP6931930B2 (en) | Improved process for producing fucoxanthin and / or polysaccharides from microalgae | |
| CN1308322C (en) | Method for preparing anthocyanidin | |
| CN103130762B (en) | A kind of method extracting anthocyanidin from indigo fruit | |
| CN102212091A (en) | High-purity geniposide as well as preparation and clinical application of preparations thereof | |
| CN109097413B (en) | Method for preparing indigo pigment with different colors based on vaccinium bracteatum leaves | |
| CN1212320C (en) | Resin process of extracting proanthocyanidin from graup seed | |
| CN115011654A (en) | Method for preparing isoquercitrin by carrying out enzymolysis on sophora flower buds | |
| CN113173902B (en) | Continuous production method of oligomeric proanthocyanidins with uniform polymerization degree | |
| CN103183616B (en) | Method for preparing chlorogenic acid from leaves of lonicera hypoglauca miq | |
| CN110818547B (en) | A method for extracting curcumin and gingerol from rhizoma Zingiberis recens | |
| CN106138130B (en) | Mango seed flavone extract and preparation method thereof | |
| CN111690267A (en) | Novel black carrot pigment refining method | |
| CN101343298A (en) | Preparation method for cation exchange resin secondarily purified anthocyanins pigment from purple sweet potato | |
| CN111423404A (en) | Method for separating rutin and quercetin from black tartary buckwheat | |
| CN100418543C (en) | Double resin process for preparing high quality active gingko leaf component extract | |
| CN1272331C (en) | Method of extracting effective components in kudzu vine root | |
| CN114315566A (en) | Method for simultaneously preparing rosemary oil soluble and fat soluble antioxidant | |
| CN109432814B (en) | Hexamethylphosphoric triamide aqueous two-phase system and application thereof | |
| CN109400660B (en) | Crocin standard prepared from fructus Gardeniae by using novel filler, and its preparation method | |
| CN106880652A (en) | A kind of extracting method of mango leaf polyphenol | |
| CN107118244B (en) | Preparation method of anthocyanin standard substance | |
| CN104497632A (en) | Method for purifying red pigment of red after-wood by using macroporous resin-active carbon composite adsorbent |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20070404 Termination date: 20180730 |