CN101343298A - Preparation method for cation exchange resin secondarily purified anthocyanins pigment from purple sweet potato - Google Patents
Preparation method for cation exchange resin secondarily purified anthocyanins pigment from purple sweet potato Download PDFInfo
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- CN101343298A CN101343298A CNA2008100541806A CN200810054180A CN101343298A CN 101343298 A CN101343298 A CN 101343298A CN A2008100541806 A CNA2008100541806 A CN A2008100541806A CN 200810054180 A CN200810054180 A CN 200810054180A CN 101343298 A CN101343298 A CN 101343298A
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Abstract
The invention relates to a preparation method for purifying anthocyanins from purple sweet potato for the second time by cation exchange resin, which is characterized in that the first time purified product of the anthocyanins from purple sweet potato is adopted as the raw material; the first time purified product is adsorbed to remove impurities, eluted, frozen and dried by cation exchange resin, and a second time purified product of anthocyanins from purple sweet potato is obtained whose content is improved over twice compared with that of the first time purified product of the anthocyanins. The preparation method successfully applies the cation exchange resin to further purifying the anthocyanins from purple sweet potato, and the obtained anthocyanins from purple sweet potato have brilliant and natural color, are non-toxic without special odor, have nutrition and pharmacological and health care functions, and are a rare natural edible pigment resource. The preparation method provides possibility of purifying the product of anthocyanins from purple sweet potato with higher biological activity for the second time in large scale, and paves the way for further developing and widely applying the obtained active product.
Description
Technical field
The present invention relates to biochemical field, especially a kind of preparation method who from purified product of anthocyanins pigment from purple sweet potato, is further purified anthocyanins pigment from purple sweet potato with Zeo-karb.
Background technology
Anthocyanidin is one of the most widely used natural food colour in the world, and safe because of it, most countries all allows it to be used for the painted of food as countries such as China, Japan, the U.S., the European Community, U.S. FDA with its list in need not license licensed licenser licence tinting material.The people who uses the anthocyanogen title the earliest is Marguart (1835), and he extracts a kind of blue pigment first from cyani flos, so claim that this is an anthocyanidin.
Anthocyanogen (anthocyanin) is by anthocyanidin and sugared with the glycosidic link be combined into, belongs to the flavones polyphenolic compound.Studies show that the carbon skeleton structure of natural anthocyanogen is C
6C
3C
6, the aglycon of anthocyanogen---anthocyanidin is 2-phenyl benzene a pair of horses going side by side pyranium salt (2-phenylbenzo-pyryalium) or poly-hydroxy and the methoxy derivatives that claims yellow Jin sheep salt (flavylium), the carbon skeleton structural formula of See Figure anthocyanogen:
Most of anthocyanidin have substituted hydroxy 3,5 of the pattern aglycon on the 7-carbon potential, because B encircles substituting group on each carbon potential---and the quantity of hydroxyl and methoxyl group is different with the position, has formed various anthocyanidin, and known naturally occurring anthocyanogen has kind more than 250.Mainly from the purple grape skin of resource scarcity, black rice, black soya bean etc., the rise of Rhizoma Dioscoreae esculentae provides the important material basis for the industrialized development of anthocyanidin to anthocyanidin in the market.
Rhizoma Dioscoreae esculentae originates in Japan, and introduce China the eighties in 20th century, and the Rhizoma Dioscoreae esculentae anthocyanidin content is higher, can reach the bright potato of 60mg/100g.Natural food colour safety, nontoxic, free from extraneous odour, bright in luster that Rhizoma Dioscoreae esculentae is produced, and have certain nutrition and pharmacological action, at aspects such as food, beverage, makeup, medicine bigger application potential is arranged.China is obtaining remarkable progress aspect the Rhizoma Dioscoreae esculentae extraction pigment, extractive technique reaches its maturity, add Rhizoma Dioscoreae esculentae output height, wide adaptability, therefore compare that the cyanidin(e) that extracts in the Rhizoma Dioscoreae esculentae has advantages such as raw material sources are easy, pigment production is high, extraction cost is low with Pericarpium Vitis viniferae, black rice etc.; The acidylate group that it had in addition makes it, and generally anthocyanogen is less to inductions such as light, heat, air, and character is more stable.
The main component of anthocyanins pigment from purple sweet potato is the Cyanidin of acylations and the derivative of peonidin; the main active group of anthocyanogen antioxygenation is the phenolic hydroxyl group in the molecule; a plurality of phenolic hydroxyl groups are arranged in the structure of anthocyanins pigment from purple sweet potato; its acyl group composition also is the fragrant acids that contains phenolic hydroxyl group; they all are hydroxyl donors, also are a kind of free-radical scavengerss simultaneously.Existing evidence isolating peonidin from Rhizoma Dioscoreae esculentae demonstrates and the suitable anti-oxidant activity of butylated hydroxy anisole (HBA), and the resistance of oxidation of the pigment that extracts from Rhizoma Dioscoreae esculentae pulp and pericarp can compare favourably with BHA, BHT.The experiment in vitro of a large amount of anti-oxidant activities shows that anthocyanins pigment from purple sweet potato shows suitable reducing power, removes ability, the anti-Fe of hydroxy radical qiao in model
2+Lecithin liposome peroxidation that causes and inhibition are by H
2O
2The ability of the erythrocyte hemolysis effect that causes.
By retrieval, find that the macroporous adsorbent resin technology is the main method of present purifying natural pigment.After macroporous adsorption resin technology is handled, can remove moisture absorption compositions such as carbohydrates a large amount of in the pigment extract, inorganic salt, phlegmatic temperament effectively, help strengthening the stability and the solubleness of product, make pigment composition highly enriched and improve the pigment quality simultaneously.However, the anthocyanogen behind the purifying only is tens percent, and the look valency is also not satisfactory.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of preparation method who adopts cation exchange resin secondarily purified anthocyanins pigment from purple sweet potato is provided, this preparation method can realize that industrialization is further purified the refining anthocyanins pigment from purple sweet potato of preparation.
Technical scheme of the present invention is:
A kind of preparation method of cation exchange resin secondarily purified anthocyanins pigment from purple sweet potato, preparation method's step is:
(1). feedstock production: a purified product of anthocyanins pigment from purple sweet potato is soluble in water, filter and to obtain clarifying clear liquid, diluting the absorbance (527nm) that this clear liquid makes this clear liquid is 10～100, regulating the pH value is 3～3.5;
(2). absorption: with sample on the clear liquid, be that 5～50 ℃, flow velocity are under 0.5～3BV/h condition, slowly on cation exchange resin column, carry out the absorption of anthocyanins pigment from purple sweet potato in temperature;
(3). removal of impurities: after absorption finishes, being the raffinate that 2.5～3.5 distilled water wash-out does not adsorb with the pH of 2～5BV/h, is colourless to effluent liquid;
(4). wash-out: using constant flow pump control flow velocity to carry out desorb with elutriant, is that wash-out is adsorbed on anthocyanins pigment from purple sweet potato on the Zeo-karb under 0.5～2BV/h condition at 5～50 ℃ of temperature, flow velocity, collects this wash-out mixed solution;
(5). reclaim elutriant: adopt the underpressure distillation mode to reclaim ethanol this wash-out mixed solution;
(6). removal of impurities again: will remove AB-8 macroporous adsorbent resin on the alcoholic acid wash-out mixed solution, the hydrochloric acid in the distilled water wash-out mixed solution with the anthocyanins pigment from purple sweet potato on the elutriant wash-out macroporous adsorbent resin, is collected this wash-out mixed solution;
(7). reclaim elutriant: adopt the underpressure distillation mode to reclaim elutriant above-mentioned wash-out mixed solution;
(8). lyophilize: the wash-out mixed solution lyophilize that will remove the part elutriant to elutriant totally, can obtain the anthocyanins pigment from purple sweet potato product.
And it is to adopt centrifugal filtration process or Plate Filtration method to filter that water-soluble anthocyanins pigment from purple sweet potato is filtered, and uses constant flow pump control flow velocity.
And described cation exchange resin column is: polar macroporous Zeo-karb D061, polar macroporous Zeo-karb D072, polarity Zeo-karb 002 * 7, polarity Zeo-karb 001 * 7 * 7 or polarity Zeo-karb 001 * 4.
And the elutriant in step (4) is 50% ethanolic soln that contains 2% hydrochloric acid.
And the elutriant in step (6) is an aqueous ethanolic solution, and its concentration is 40～95% (V/V).
Advantage of the present invention and positively effect are:
1. preparation technology of the present invention is simple relatively, product chemistry stable in properties, the scale production cost is low, the secondary refining that the Zeo-karb technology successfully is used for anthocyanins pigment from purple sweet potato, produce for the heavy industrialization of anthocyanins pigment from purple sweet potato product with higher degree and look valency is refining provide may, for the further exploitation and the widespread use of this biologically active prod of being obtained are laid a good foundation.
2. by the anthocyanins pigment from purple sweet potato product that the present invention obtained, the look valency has improved more than 2 times on original basis, has solved for a long time natural pigment because the look valency is low, the problem of less stable.We measure the total polyphenols and the general flavone content of this product in addition, find that its total polyphenols and general flavone content all increased than originally, and are advanced fairly obvious.
3. the present invention also can measure the resistance of oxidation of the anthocyanins pigment from purple sweet potato that obtained.Experiment showed, that the anthocyanins pigment from purple sweet potato that is obtained has very strong oxidation-resistance, liver function protecting and transaminase lowering are had positive effect, oncogene is had very strong restraining effect, cardiovascular disordeies such as hypertension are also had the excellent prevention effect.
Embodiment
The invention will be further described below by specific embodiment, and following examples are descriptive, is not determinate, can not limit protection scope of the present invention with this.
The Zeo-karb that is adopted among the present invention is respectively: polar macroporous Zeo-karb D061, polar macroporous Zeo-karb D072, polarity Zeo-karb 002 * 7, polarity Zeo-karb 001 * 7 * 7 and polarity Zeo-karb 001 * 4.The present invention is that example is narrated with polar macroporous Zeo-karb D061 only, and the mode of operation and the D061 of other Zeo-karb are basic identical.
A kind of preparation method of cation exchange resin secondarily purified anthocyanins pigment from purple sweet potato, the step of its preparation method is:
(1). feedstock production: the raw material that the present invention adopts is a purified product of anthocyanins pigment from purple sweet potato.This purified product is soluble in water, filter to remove insolubles, its filter type can adopt centrifugal filtration process or Plate Filtration method to filter, can obtain clarifying clear liquid after the filtration, suitably dilute this clear liquid, making the absorbance (527nm) of this clear liquid is 10～100, and regulating the pH value is 3～3.5;
With the wet method dress post in distilled water of the polar macroporous Zeo-karb D061 resin after handling, glass column 1.7 * 42cm, wherein resin is adorned post height 38cm, the about 250ml of resin volume.
(2). absorption: with sample on the clear liquid, be that 20 ℃, flow velocity are 1.0 column volumes per hour under the condition of (BV/h), slowly on cation exchange resin column, carry out the absorption of anthocyanins pigment from purple sweet potato, and use constant flow pump control flow velocity in temperature; When absorbance in the effluent liquid reach the sample introduction absorbance 1/10 the time think and stop sample introduction by the breakthrough point that reaches absorption that applied sample amount is 1000ml;
(3). removal of impurities: after absorption finishes, being the raffinate that 3 distilled water wash-out does not adsorb with the pH of 2.0BV/h, is colourless to effluent liquid;
(4). wash-out: use constant flow pump control flow velocity to carry out desorb with elutriant, in temperature is that 20 ℃, flow velocity are that wash-out is adsorbed on anthocyanins pigment from purple sweet potato on the Zeo-karb under the 0.5BV/h condition, collect this wash-out mixed solution, this elutriant is 50% ethanolic soln that contains 2% hydrochloric acid.
(5). reclaim elutriant: adopt the underpressure distillation mode to reclaim ethanol this wash-out mixed solution;
(6). removal of impurities again: will remove AB-8 macroporous adsorbent resin on the alcoholic acid wash-out mixed solution, hydrochloric acid in the distilled water wash-out mixed solution, with the anthocyanins pigment from purple sweet potato on elutriant (ethanol-water solution, its concentration are 40～95% (V/V)) the wash-out macroporous adsorbent resin, collect this wash-out mixed solution;
(7). reclaim elutriant: adopt the underpressure distillation mode to reclaim elutriant this wash-out mixed solution;
(8). lyophilize: the wash-out mixed solution that will remove the part eluent adopt lyophilize to elutriant totally, can obtain the anthocyanins pigment from purple sweet potato product.
The present invention can represent that by the result that the content of the prepared anthocyanins pigment from purple sweet potato of Zeo-karb D061 is measured with look valency method concrete measuring method and result calculate and carry out as follows:
Refining back Rhizoma Dioscoreae esculentae pigment obtains Rhizoma Dioscoreae esculentae pigment dry powder through carrying out vacuum lyophilization 24 hours.Accurate weighing is once made with extra care and secondary refining product 1.000g pigment product respectively, after citric acid-disodium hydrogen phosphate buffer solution dissolving with pH=3.0, constant volume is in the volumetric flask of 100mL, the elimination insolubles, get the 1mL pigment solution and be diluted to suitable multiple, under the 527nm wavelength, record absorbance, calculate the look valency according to formula 1.
Wherein:
A: absorbance
B: extension rate
W: pigment quality
Record product look valency according to formula 1 experimental technique:
A purified product
The secondary refining product
The secondary refining product improves 2.19 times than a purified product look valency.
Claims (5)
1. the preparation method of a cation exchange resin secondarily purified anthocyanins pigment from purple sweet potato, it is characterized in that: preparation method's step is:
(1). feedstock production: a purified product of anthocyanins pigment from purple sweet potato is soluble in water, filter and to obtain clarifying clear liquid, diluting the absorbance (527nm) that this clear liquid makes this clear liquid is 10～100, regulating the pH value is 3～3.5;
(2). absorption: with sample on the clear liquid, be that 5～50 ℃, flow velocity are under 0.5～3BV/h condition, slowly on cation exchange resin column, carry out the absorption of anthocyanins pigment from purple sweet potato in temperature;
(3). removal of impurities: after absorption finishes, being the raffinate that 2.5～3.5 distilled water wash-out does not adsorb with the pH of 2～5BV/h, is colourless to effluent liquid;
(4). wash-out: using constant flow pump control flow velocity to carry out desorb with elutriant, is that wash-out is adsorbed on anthocyanins pigment from purple sweet potato on the Zeo-karb under 0.5～2BV/h condition at 5～50 ℃ of temperature, flow velocity, collects this wash-out mixed solution;
(5). reclaim elutriant: adopt the underpressure distillation mode to reclaim ethanol this wash-out mixed solution;
(6). removal of impurities again: will remove AB-8 macroporous adsorbent resin on the alcoholic acid wash-out mixed solution, the hydrochloric acid in the distilled water wash-out mixed solution with the anthocyanins pigment from purple sweet potato on the elutriant wash-out macroporous adsorbent resin, is collected this wash-out mixed solution;
(7). reclaim elutriant: adopt the underpressure distillation mode to reclaim elutriant above-mentioned wash-out mixed solution;
(8). lyophilize: the wash-out mixed solution lyophilize that will remove the part elutriant to elutriant totally, can obtain the anthocyanins pigment from purple sweet potato product.
2. the preparation method of cation exchange resin secondarily purified anthocyanins pigment from purple sweet potato according to claim 1, it is characterized in that: it is to adopt centrifugal filtration process or Plate Filtration method to filter that water-soluble anthocyanins pigment from purple sweet potato is filtered, and uses constant flow pump control flow velocity.
3. the preparation method of cation exchange resin secondarily purified anthocyanins pigment from purple sweet potato according to claim 1, it is characterized in that: described cation exchange resin column is: polar macroporous Zeo-karb D061, polar macroporous Zeo-karb D072, polarity Zeo-karb 002 * 7, polarity Zeo-karb 001 * 7 * 7 or polarity Zeo-karb 001 * 4.
4. the preparation method of cation exchange resin secondarily purified anthocyanins pigment from purple sweet potato according to claim 1, it is characterized in that: the elutriant in step (4) is 50% ethanolic soln that contains 2% hydrochloric acid.
5. the preparation method of cation exchange resin secondarily purified anthocyanins pigment from purple sweet potato according to claim 1, it is characterized in that: the elutriant in step (6) is an aqueous ethanolic solution, its concentration is 40～95% (V/V).
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102391667A (en) * | 2011-08-30 | 2012-03-28 | 河南中大生物工程有限公司 | Purification method of purple sweet potato pigment |
| CN102604424A (en) * | 2012-02-27 | 2012-07-25 | 河北科技大学 | Method for extracting anthocyanins from purple sweet potato |
| CN104356106A (en) * | 2014-10-21 | 2015-02-18 | 山东省科学院生物研究所 | Extraction and purification method of purple potato anthocyanin |
| CN112314945A (en) * | 2020-10-29 | 2021-02-05 | 安徽卡伦拜瑞健康科技有限公司 | Method for preparing high-activity cranberry extract by sectional extraction method |
| CN112326567A (en) * | 2020-10-09 | 2021-02-05 | 天津科技大学 | Optimized extraction method of pumpkin antioxidant active ingredients and verification method of antioxidant activity |
-
2008
- 2008-08-20 CN CNA2008100541806A patent/CN101343298A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102391667A (en) * | 2011-08-30 | 2012-03-28 | 河南中大生物工程有限公司 | Purification method of purple sweet potato pigment |
| CN102391667B (en) * | 2011-08-30 | 2014-02-12 | 河南中大生物工程有限公司 | Purification method of purple sweet potato pigment |
| CN102604424A (en) * | 2012-02-27 | 2012-07-25 | 河北科技大学 | Method for extracting anthocyanins from purple sweet potato |
| CN104356106A (en) * | 2014-10-21 | 2015-02-18 | 山东省科学院生物研究所 | Extraction and purification method of purple potato anthocyanin |
| CN104356106B (en) * | 2014-10-21 | 2016-06-01 | 山东省科学院生物研究所 | The extracting and purifying method of a kind of purple potato anthocyanidin |
| CN112326567A (en) * | 2020-10-09 | 2021-02-05 | 天津科技大学 | Optimized extraction method of pumpkin antioxidant active ingredients and verification method of antioxidant activity |
| CN112314945A (en) * | 2020-10-29 | 2021-02-05 | 安徽卡伦拜瑞健康科技有限公司 | Method for preparing high-activity cranberry extract by sectional extraction method |
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Open date: 20090114 |