CN101555359A - Grape skin red pigment preparation method - Google Patents
Grape skin red pigment preparation method Download PDFInfo
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- CN101555359A CN101555359A CNA2009101434971A CN200910143497A CN101555359A CN 101555359 A CN101555359 A CN 101555359A CN A2009101434971 A CNA2009101434971 A CN A2009101434971A CN 200910143497 A CN200910143497 A CN 200910143497A CN 101555359 A CN101555359 A CN 101555359A
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Abstract
The invention discloses a grape skin red pigment preparation method using natural grape skin as the main raw material. The method comprises the following steps of: a. extraction with acid liquid: putting fresh grape skin residue, after being cleaned, into an extraction tank, spraying and extracting with acid liquid, and collecting extraction liquid of the grape skin red pigment; b. processing with enzyme preparation: adjusting the pH value of the collected extraction liquid, adding 0.01 to 0.3 thousandth of enzyme preparation into the extraction liquid the pH value of which is adjusted, mixing evenly, standing for 0.5 to 5 hours, precisely filtrating, and obtaining fine grape skin red pigment water solution; c. absorption and separation; d. concentration and refining; and e. spray drying and obtaining red powder product. The invention adopts advanced technique and the product is purely natural. During the production process, no waste water, waste gas or waste residue are discharged, therefore, the method is pollution free and good for the environment. Raw materials have wide supply sources and the price is low, therefore, the method, having significant economic and social benefits, can be widely promoted and applied across the country.
Description
Technical field
The present invention relates to a kind of is the method that raw material is made pigment with the natural phant, and particularly a kind of is the method that main raw material is made grape skin red pigment with the natural phant Pericarpium Vitis viniferae.
Background technology
Along with the strict demand that country uses in food pigment, natural pigment will replace synthetic colour.People's also improving constantly in the grape wine production to natural grape haematochrome understanding.Extract pigment from Pericarpium Vitis viniferae and regulate a kind of method that colourity vinous can be described as most economical environmental protection.But at present the grape skin color of China can't satisfy each big grape wine requirement of enterprise, domestic each enterprise have to regulate with natural edible pigment and cabbage haematochrome color and luster of wine.And this has brought many detrimentally affects to it, as: muddiness, precipitation, smell etc., the quality that has influenced wine has increased cost again.But grape skin color is got back in the grape wine again from grape and is gone, and has not only improved quality greatly, has also improved its economic benefit.Therefore, this advantage of grape skin color is favored by each big grape wine enterprise of the whole nation.
The demand sustainable growth of grape in recent years is because the development of the blowout of grape wine industry is the Sucus Vitis viniferae grappling that is used for various drinks on the other hand on the one hand.Grape wine or Sucus Vitis viniferae mainly usefulness be pulp.And skin and seed are generally handled as waste residue.Skin and seed all are the good sources as natural extract in fact, just do not obtain enough attention.The back remaining grape waste residue of for example many grape wine company's fermentations but is not fully utilized.Therefore, from the waste residue of grape processing, carry out natural constituent and extract, become " profit source " of another product.The exploitation of natural grape haematochrome project will be the utilization and the exploitation of winery's byproduct, can turn waste into wealth! Avoided the pollution of environment when increasing economic efficiency again, the exploitation of this project will have crucial meaning.And the natural grape haematochrome be extracted as physical extraction, meet state environment protecting standard, pollution-free, nuisanceless.
Summary of the invention
Technical problem solved by the invention is, a kind of production method of grape skin red pigment is provided.Grape skin red pigment is a kind of pure natural pigment resource, can remedy the deficiency of existing natural pigment, satisfies the manufacturing demand of grape wine.
For solving the problems of the technologies described above, the invention provides a kind of manufacture method of grape skin red pigment, described manufacture method may further comprise the steps:
A. sour water extraction: fresh grape skin is put into extractor after cleaning, sour water spraying and extracting, the extraction liquid of collection grape skin red pigment;
B. processing with enzyme preparation: regulate the pH value of collecting extraction liquid, add 0.01～0.3 ‰ zymin in the extraction liquid of pH value with regulating, stir, left standstill 0.5～5 hour, secondary filter obtains the aqueous solution of refining grape skin red pigment;
C. adsorb and separate: resin adsorption column on the aqueous solution of the refining grape skin red pigment that will obtain, the saturated back of resin: wash with deionized water, till washing neutrality; Clean with sour water once more and remove impurity, reuse the deionization washing till neutrality; With the acid ethanol solution wash-out, the separation that contain 3 ‰, extremely neutral with washed with de-ionized water for the third time;
D. concentrate with refining: through ultrafiltration, send vacuum-evaporator to concentrate grape skin red pigment the grape skin red pigment that elutes, ethanol steams recycling, and employing secondary alcohol deposition method is made with extra care;
E. spraying drying: add carrier in the grape skin red pigment solution after will making with extra care, adopt spraying drying, obtain the red powder product.
Among the described step a, preferably press grape skin during extraction: the sour water spraying and extracting of solution=1: 3～5, the pH value of aqueous acid are 1.5～4.
Among the described step b, regulate the extraction liquid of pH value, its pH value is preferably 3～6.
The flow of resin absorption post is preferably 15～50m among the described step c
3/ h.
Among the described step c, clean with sour water once more and remove impurity, the preferred PH of sour water is 2.5～5.
Among the described step c, after the waste water that resin column is discharged can be collected, recycle through being used for extraction liquid once more behind flocculation, clarification, sterilization, the adjusting pH value; The ethanol that wash-out is used after alcohol distillation device reflow treatment, can use by recycling elution.
In the described steps d, the vacuum tightness of described vacuum-evaporator is preferably-0.02～-0.08MPa, the temperature of described vacuum-evaporator is preferably 40～80 degree.
Among the described step e, during spraying drying, inlet temperature is preferably 120～180 ℃, and temperature out is preferably 70～90 ℃.
Described zymin can be in amylase, polygalacturonase, cellulase, proteolytic enzyme or the beta-glucanase one or more.
Described sour water can be in citric acid, oxysuccinic acid, lactic acid, acetic acid, hydrochloric acid or the sulfuric acid one or more; Described carrier can be in Sumstar 190, maltodextrin, glucose or the carboxymethyl starch one or more.
The present invention has following advantage:
1, technology advanced person adopts the processing with enzyme preparation extraction liquid, has improved the solubleness, clarity of pigment greatly, to light, to heat and long-time stability of placing.
2, tone changes with pH value.Water-solublely take on a red color to purple when acid, be faint blue during alkalescence, iron ion is mulberry under existing.
3, by after the processing with enzyme preparation, by the pigment purity height of column separating purification gained, HPLC result shows that the purity of anthocyanidin can reach 95%.
Three-waste free discharge, pollution-free in the production process is good to environment; Raw material sources are extensive, apply in China, and remarkable economic efficiency and social benefit are arranged.
Description of drawings
Fig. 1 is the manufacture method schema of the described grape skin red pigment of the embodiment of the invention.
Embodiment
As shown in Figure 1, be the manufacture method schema of the described grape skin red pigment of the embodiment of the invention.The invention discloses a kind of is the method that main raw material is made grape skin red pigment with the natural phant Pericarpium Vitis viniferae, may further comprise the steps: Pericarpium Vitis viniferae → sour water extraction → processing with enzyme preparation → filtration → resin absorption → ethanol elution → concentrating under reduced pressure → alcohol precipitation is made with extra care → concentrate drying → finished product.Grape skin red pigment is a kind of pure natural pigment resource, can remedy the deficiency of existing natural pigment, satisfies the manufacturing demand of grape wine.Technology advanced person of the present invention is an all-natural product.Three-waste free discharge, pollution-free in the production process is good to environment; Raw material sources are extensive, and are cheap, can apply in China, and remarkable economic efficiency and social benefit are arranged.
In one embodiment of this invention, the grape skin red pigment extraction process adopts following steps: Pericarpium Vitis viniferae → sour water extraction → processing with enzyme preparation → filtration → resin absorption → ethanol elution → concentrating under reduced pressure → alcohol precipitation is made with extra care → concentrate drying → finished product.
1, cleans
Fresh Pericarpium Vitis viniferae is cleaned with flowing water, remove silt and impurity.
2, sour water extraction
Fresh grape skin is put into extractor after cleaning, can be by material: the sour water spraying and extracting of solution=1: 3-5, the pH value of solution can be 1.5～4, collects the extraction liquid of grape skin red pigment.
3, processing with enzyme preparation extraction liquid
PH value that regulate to collect extraction liquid can be 3～6, adds 0.01～0.3 ‰ zymin in the extraction liquid of pH value with regulating, and stirs, left standstill 0.5～5 hour, remove materials such as a large amount of sugar, pectin, Mierocrystalline cellulose, protein, secondary filter must be made with extra care the aqueous solution of grape skin red pigment.
4, adsorb and separate
With resin adsorption column on the aqueous solution of the refining grape skin red pigment that obtains, flow is to be 15～50m
3/ h after resin is saturated, washes with deionized water, till washing neutrality, can be 2.5～5 sour water cleaning again with PH, remove materials such as impurity, wash till neutrality with deionized water again, can be with the acid ethanol solution wash-out, the separation that contain 3 ‰, again with washed with de-ionized water to neutral.
5, concentrate and make with extra care
Send vacuum-evaporator to concentrate grape skin red pigment through ultrafiltration the grape skin red pigment that elutes, vacuum tightness can be for-0.02～-0.08MPa, temperature can be 40～80 degree, alcohol steams recycling, adopts the secondary alcohol precipitation to send out and makes with extra care.
6, concentrate drying
Grape skin red pigment solution after adopting the secondary alcohol precipitation refining is carried out concentrating under reduced pressure steam ethanol, add carrier and adopt spray-drying process to make finished product, inlet temperature can be 120～180 ℃, and temperature out can be 70～90 ℃, obtains the red powder product.
7, after the wastewater collection that resin column is discharged in the production, recycle through being used for extraction liquid once more behind flocculation, clarification, sterilization, the adjusting pH value; The ethanol that wash-out is used, after alcohol distillation device reflow treatment, wash-out capable of circulation is used.
Zymin is one or more in amylase, polygalacturonase, cellulase, proteolytic enzyme, the beta-glucanase in the described manufacture method; The acid of using in the solution is one or more in citric acid, oxysuccinic acid, lactic acid, acetic acid, hydrochloric acid and the sulfuric acid; Carrier is one or more in Sumstar 190, maltodextrin, glucose and the carboxymethyl starch.
In another embodiment of the present invention, after earlier fresh Pericarpium Vitis viniferae being cleaned up, utilize travelling belt to be delivered in the extractor Pericarpium Vitis viniferae that cleans up, according to Pericarpium Vitis viniferae: the volume ratio of solution=1: 3-5 adds the sour water that has mixed up, after stirring, survey pH value, adding acid, to regulate pH value be 1.5～4, extract after 12 hours extraction filtrate and squeeze in another extractor.
Add again with the solution of volume and transfer pH value, extract filtrate out, repeat lixiviate three times, merges three times filtrate, regulate pH value=3～6 of collection extraction liquid, add 0.01～0.3 ‰ zymin in the extraction liquid of pH value regulating.
Stir, left standstill 0.5～5 hour, remove materials such as a large amount of sugar, pectin, Mierocrystalline cellulose, protein, secondary filter must be made with extra care the aqueous solution of grape skin red pigment.
Filtrate is directly crossed post, the processing of crossing the preceding resin of post: before the upper prop, need 2mol/LNaOH to soak after 2 hours, use distillating washing resin, till neutrality; After soaking 2 hours with 2mol/LHCL again, with distillating washing resin up to neutrality up to; Use the alcohol immersion resin again 2 hours, and washed neutrality with water; Use pickling again, washing can upper prop after the neutrality.
1-4% according to the per minute column volume during upper prop determines flow velocity.Till resin is filled fully; Use the impurity in the deionization washing resin instead, and then use pickling, wash till neutrality with deionized water again.Use the acidic ethanol wash-out again, collect stripping liquid.
After pigment washes, get final product with the method regenerating resin of handling new resin.After this resin regeneration, can be repeatedly used.
Send vacuum-evaporator to concentrate grape skin red pigment through ultrafiltration the grape skin red pigment that elutes, vacuum tightness is-0.02～-0.08MPa, temperature is 40～80 degree, alcohol steams recycling, adopts the secondary alcohol precipitation to send out and makes with extra care.
Grape skin red pigment solution after adopting the secondary alcohol precipitation refining is carried out concentrating under reduced pressure steam ethanol, add carrier and adopt spray-drying process to make finished product, inlet temperature is 120～180 ℃, and temperature out is 70～90 ℃, obtains the red powder finished product.
Claims (10)
1, a kind of manufacture method of grape skin red pigment is characterized in that, described manufacture method may further comprise the steps:
A. sour water extraction: fresh grape skin is put into extractor after cleaning, sour water spraying and extracting, the extraction liquid of collection grape skin red pigment;
B. processing with enzyme preparation: regulate the pH value of collecting extraction liquid, add 0.01～0.3 ‰ zymin in the extraction liquid of pH value with regulating, stir, left standstill 0.5～5 hour, secondary filter obtains the aqueous solution of refining grape skin red pigment;
C. adsorb and separate: resin adsorption column on the aqueous solution of the refining grape skin red pigment that will obtain, the saturated back of resin: wash with deionized water, till washing neutrality; Clean with sour water once more and remove impurity, reuse the deionization washing till neutrality; With the acid ethanol solution wash-out, the separation that contain 3 ‰, extremely neutral with washed with de-ionized water for the third time;
D. concentrate with refining: through ultrafiltration, send vacuum-evaporator to concentrate grape skin red pigment the grape skin red pigment that elutes, ethanol steams recycling, and employing secondary alcohol deposition method is made with extra care;
E. spraying drying: add carrier in the grape skin red pigment solution after will making with extra care, adopt spraying drying, obtain the red powder product.
2, according to the described manufacture method of claim 1, it is characterized in that, among the described step a, press grape skin during extraction: the sour water spraying and extracting of solution=1: 3～5, the pH value of aqueous acid are 1.5～4.
According to the described manufacture method of claim 1, it is characterized in that 3, among the described step b, regulate the extraction liquid of pH value, its pH value is 3～6.
According to the described manufacture method of claim 1, it is characterized in that 4, the flow of resin absorption post is 15～50m among the described step c
3/ h.
According to the described manufacture method of claim 1, it is characterized in that 5, among the described step c, clean with sour water once more and remove impurity, the PH of sour water is 2.5～5.
6, according to the described manufacture method of claim 1, it is characterized in that, among the described step c, after the wastewater collection that resin column is discharged, recycle through being used for extraction liquid once more behind flocculation, clarification, sterilization, the adjusting pH value; The ethanol that wash-out is used, after alcohol distillation device reflow treatment, recycling elution uses.
7, according to the described manufacture method of claim 1, it is characterized in that, in the described steps d, the vacuum tightness of described vacuum-evaporator is-0.02～-0.08MPa, the temperature of described vacuum-evaporator is 40～80 degree.
According to the described manufacture method of claim 1, it is characterized in that 8, among the described step e, during spraying drying, inlet temperature is 120～180 ℃, temperature out is 70～90 ℃.
9, according to the described manufacture method of claim 1, described zymin is one or more in amylase, polygalacturonase, cellulase, proteolytic enzyme or the beta-glucanase.
10, according to the described manufacture method of claim 1, described sour water is one or more in citric acid, oxysuccinic acid, lactic acid, acetic acid, hydrochloric acid or the sulfuric acid; Described carrier is one or more in Sumstar 190, maltodextrin, glucose or the carboxymethyl starch.
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| CN2009101434971A CN101555359B (en) | 2009-05-27 | 2009-05-27 | Grape skin red pigment preparation method |
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| CN2009101434971A CN101555359B (en) | 2009-05-27 | 2009-05-27 | Grape skin red pigment preparation method |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102835713A (en) * | 2011-06-23 | 2012-12-26 | 浙江养生堂天然药物研究所有限公司 | Acerola juice powder and its preparation method |
| CN101747662B (en) * | 2009-12-25 | 2013-03-13 | 江南大学 | Method for preparing hematoxylin powder dyes |
| CN103103063A (en) * | 2013-01-29 | 2013-05-15 | 新疆西部牧业股份有限公司 | Technology for producing distilled wine by use of grape skin residue |
| CN103160137A (en) * | 2011-12-08 | 2013-06-19 | 上海蓝普生物科技有限公司 | Grape-skin pigment and extraction process for same |
| CN104073021A (en) * | 2014-06-26 | 2014-10-01 | 南通润启时装有限公司 | Preparation and application of grape natural dye |
| CN105219123A (en) * | 2015-10-20 | 2016-01-06 | 江南大学 | A kind of method improving grape skin red pigment stability |
| CN105639606A (en) * | 2016-02-22 | 2016-06-08 | 陈兹佳 | Dip for eating of mutton and preparation method of dip |
| CN114869822A (en) * | 2022-06-10 | 2022-08-09 | 茅台学院 | Method for preparing mirror-surface lip glaze by extracting pigment from grape skin residues for wine making |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4452822A (en) * | 1982-05-17 | 1984-06-05 | United Vintners, Inc. | Extraction and intensification of anthocyanins from grape pomace and other material |
-
2009
- 2009-05-27 CN CN2009101434971A patent/CN101555359B/en active Active
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101747662B (en) * | 2009-12-25 | 2013-03-13 | 江南大学 | Method for preparing hematoxylin powder dyes |
| CN102835713A (en) * | 2011-06-23 | 2012-12-26 | 浙江养生堂天然药物研究所有限公司 | Acerola juice powder and its preparation method |
| CN102835713B (en) * | 2011-06-23 | 2016-06-29 | 浙江养生堂天然药物研究所有限公司 | A kind of Acerola cherry fruit powder and manufacture method thereof |
| TWI637693B (en) * | 2011-06-23 | 2018-10-11 | 浙江養生堂天然藥物研究所有限公司 | Coniferous cherry fruit powder and manufacturing method thereof |
| CN103160137A (en) * | 2011-12-08 | 2013-06-19 | 上海蓝普生物科技有限公司 | Grape-skin pigment and extraction process for same |
| CN103103063A (en) * | 2013-01-29 | 2013-05-15 | 新疆西部牧业股份有限公司 | Technology for producing distilled wine by use of grape skin residue |
| CN103103063B (en) * | 2013-01-29 | 2015-02-18 | 新疆西部牧业股份有限公司 | Technology for producing distilled wine by use of grape skin residue |
| CN104073021A (en) * | 2014-06-26 | 2014-10-01 | 南通润启时装有限公司 | Preparation and application of grape natural dye |
| CN105219123A (en) * | 2015-10-20 | 2016-01-06 | 江南大学 | A kind of method improving grape skin red pigment stability |
| CN105639606A (en) * | 2016-02-22 | 2016-06-08 | 陈兹佳 | Dip for eating of mutton and preparation method of dip |
| CN114869822A (en) * | 2022-06-10 | 2022-08-09 | 茅台学院 | Method for preparing mirror-surface lip glaze by extracting pigment from grape skin residues for wine making |
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