CN101555359B - Grape skin red pigment preparation method - Google Patents
Grape skin red pigment preparation method Download PDFInfo
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- CN101555359B CN101555359B CN2009101434971A CN200910143497A CN101555359B CN 101555359 B CN101555359 B CN 101555359B CN 2009101434971 A CN2009101434971 A CN 2009101434971A CN 200910143497 A CN200910143497 A CN 200910143497A CN 101555359 B CN101555359 B CN 101555359B
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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 method of making pigment take natural phant as raw material, particularly a kind of method of making grape skin red pigment take the natural phant Pericarpium Vitis viniferae as main raw material.
Background technology
Along with the strict demand that country uses in food pigment, natural pigment will replace synthetic colour.People's also improving constantly natural grape haematochrome understanding in the grape wine production.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 the demand of each large Wine Enterprises, 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 affected wine has increased again cost.But grape skin color is got back in the grape wine again from grape and is gone, and has not only greatly improved quality, has also improved its economic benefit.Therefore, this advantage of grape skin color is favored by each large Wine Enterprises of the whole nation.
The in recent years demand sustainable growth of grape is because the development of the blowout of Grape Wine Industry is in great demand for the Sucus Vitis viniferae of 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 processed as waste residue.Skin and seed all are the good sources as natural extract in fact, just do not obtain enough attention.For example the rear remaining grape dregs of 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 utilization and the exploitation of winery's byproduct, can turn waste into wealth! Avoided again the pollution of environment when increasing economic efficiency, the exploitation of this project is of great significance tool.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 absorbing column on the aqueous solution of the refining grape skin red pigment that will obtain, after resin is saturated: wash with deionized water, until wash till the neutrality; Again clean with sour water and remove impurity, reuse the deionization washing until till the 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. concentrated and refining: through ultrafiltration, send vacuum-evaporator 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 absorbing column is preferably 15～50m among the described step c
3/ h.
Among the described step c, again clean with sour water 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 again being used for extraction liquid 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, technique is advanced, adopts the processing with enzyme preparation extraction liquid, has improved greatly the solubleness, clarity of pigment, to light, to heat and long-time stability of placing.
2, tone changes with pH value.Take on a red color to purple during water-soluble acidity, be faint blue during alkalescence, iron ion is mulberry under existing.
3, by after the processing with enzyme preparation, high by the pigment purity of column separating purification gained, HPLC result shows the purity 95% of anthocyanidin.
Three-waste free discharge, pollution-free in the production process is good to environment; Raw material sources are extensive, apply in China, and significant economic benefit 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 method of making grape skin red pigment take the natural phant Pericarpium Vitis viniferae as main raw material, 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.Technique of the present invention is advanced, is 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 significant economic benefit 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 the 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 absorbing 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, until wash till the neutrality, can be 2.5～5 sour water cleaning again with PH, remove the materials such as impurity, wash with deionized water again until till the neutrality, can be with the acid ethanol solution wash-out, the separation that contain 3 ‰, again with washed with de-ionized water to neutral.
5, concentrated and refining
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 again being used for extraction liquid 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 first 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, it is 1.5～4 that acid adding is regulated pH value, extract after 12 hours extraction filtrate and squeezes 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 the pH value of collection extraction liquid=3～6, add 0.01～0.3 ‰ zymin in the extraction liquid of pH value with regulating.
Stir, left standstill 0.5～5 hour, remove the 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 front resin of post: before the upper prop, need 2mol/LNaOH to soak after 2 hours, use distillating washing resin, until neutrality; After soaking 2 hours with 2mol/LHCL again, with distillating washing resin until neutral up to; Use again the alcohol immersion resin 2 hours, and washed neutrality with water; Use pickling, washing can upper prop after the neutrality again.
1-4% according to the per minute column volume during upper prop determines flow velocity.Until resin is filled fully; Use the impurity in the deionization washing resin instead, and then use pickling, wash until till the neutrality with deionized water again.Use again the acidic ethanol wash-out, collect stripping liquid.
After pigment washes, get final product with the method regenerating resin of processing 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 (1)
1. the manufacture method of a 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 making with extra care the aqueous solution of grape skin red pigment;
C. adsorb and separate: resin absorbing column on the aqueous solution of the refining grape skin red pigment that will obtain, after resin is saturated: wash with deionized water, until wash till the neutrality; Again clean with sour water and remove impurity, reuse the deionization washing until till the 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. concentrated and refining: through ultrafiltration, send vacuum-evaporator 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, press grape skin during extraction: the sour water spraying and extracting of solution=1: 3～5, the pH value of aqueous acid is 1.5～4;
Among the described step b, regulate the extraction liquid of pH value, its pH value is 3～6;
Tone changes with the pH value, takes on a red color to purple during water-soluble acidity, is faint blue during alkalescence, and iron ion is mulberry under existing;
The flow of resin absorbing column is 15～50m among the described step c
3/ h;
Among the described step c, again clean with sour water and remove impurity, the pH of sour water is 2.5～5;
Among the described step c, after the wastewater collection that resin column is discharged, recycle through again being used for extraction liquid after flocculation, clarification, sterilization, the adjusting pH value; The ethanol that wash-out is used, after alcohol distillation device reflow treatment, recycling elution uses;
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;
Among the described step e, during spraying drying, inlet temperature is 120～180 ℃, and temperature out is 70～90 ℃;
Described zymin is one or more in amylase, polygalacturonase, cellulase, proteolytic enzyme or the beta-glucanase;
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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| CN101555359B true CN101555359B (en) | 2013-05-01 |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101747662B (en) * | 2009-12-25 | 2013-03-13 | 江南大学 | Method for preparing hematoxylin powder dyes |
| EP2724628B1 (en) * | 2011-06-23 | 2017-08-09 | Natural Medicine Institute of Zhejiang Yangshengtang Co., Ltd. | Acerola cherry 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 |
| 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 |
| CN105219123B (en) * | 2015-10-20 | 2017-03-01 | 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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| US4452822A (en) * | 1982-05-17 | 1984-06-05 | United Vintners, Inc. | Extraction and intensification of anthocyanins from grape pomace and other material |
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2009
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Patent Citations (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 |
Non-Patent Citations (6)
| Title |
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| ALAN H. MOSKOWITZ et al.Vacuolar Contents of Fruit Subepidermal Cells from Vitis Species.《Plant Physiol.》.1981,第68卷第686-692页. |
| Comparison of Several Procedures Used for the Extraction of Anthocyanins from Red Grapes;Eugenio Revilla et al;《J. Agric. Food Chem.》;19981029;第46卷(第11期);第4592-4597页 * |
| Eugenio Revilla et al.Comparison of Several Procedures Used for the Extraction of Anthocyanins from Red Grapes.《J. Agric. Food Chem.》.1998,第46卷(第11期),第4592-4597页. |
| Vacuolar Contents of Fruit Subepidermal Cells from Vitis Species;ALAN H. MOSKOWITZ et al;《Plant Physiol.》;19811231;第68卷;第686-692页 * |
| 葡萄皮花色苷提取纯化技术及稳定性研究;郭耀东;《中国优秀硕士学位论文全文数据库 工程科技I辑》;20081115(第11期);B024-182 * |
| 郭耀东.葡萄皮花色苷提取纯化技术及稳定性研究.《中国优秀硕士学位论文全文数据库 工程科技I辑》.2008,(第11期),B024-182. |
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