CN104448902A - Grape skin pigment extraction technology - Google Patents
Grape skin pigment extraction technology Download PDFInfo
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- CN104448902A CN104448902A CN201310431198.4A CN201310431198A CN104448902A CN 104448902 A CN104448902 A CN 104448902A CN 201310431198 A CN201310431198 A CN 201310431198A CN 104448902 A CN104448902 A CN 104448902A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B61/00—Dyes of natural origin prepared from natural sources, e.g. vegetable sources
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Abstract
The invention discloses a grape skin pigment extraction technology. The technology comprises the following steps: 1, mixing dried grape skin powder with 95wt% ethanol, adjusting the pH value of the above obtained solution to 2-4 by using an aqueous citric acid solution, carrying out high speed pretreatment at room temperature, homogeneously extracting, and filtering; 2, mixing filter residues obtained after the filtration with 95wt% ethanol, adjusting the obtained solution to 2-4 by using the aqueous citric acid solution, homogeneously extracting, and filtering; and 3, centrifuging the obtained filtrate, collecting the obtained supernatant, and freeze-drying to obtain powder in order to obtain a grape skin pigment. The high speed pretreatment is carried out under 5000-1000rpm for above 5min, and the homogeneous extraction is carried out under 1000-4000rpm for above 10min. The invention also discloses the grape skin pigment obtained through the technology. The extraction technology has the advantages of simplicity, low requirements on a production device, high extraction efficiency, and great shortening of the extraction time, is obviously better than traditional solvent extraction methods. The obtained grape skin pigment has the advantages of good water solubility, good appearance color and stable properties, and is suitable for being used as a food additive and a health food raw material.
Description
Technical field
The invention belongs to the extractive technique field of natural pigment, be specifically related to a kind of grape skin color and extraction process thereof.
Background technology
China's brewing grape industry all produces a large amount of grape skins every year, presses out skin and counts at 20-25%, at least produces the skin slag of hundreds of thousands of ton every year.These skin slags are mainly used in feed, fertilizer industry, cause added value very low, and have suitable major part not to be utilized and contaminate environment.
Research finds in grape skin containing more natural pigment, content is generally more than 3.7% (massfraction), its haematochrome content is many at more than 300mg/100g especially, and containing abundant anthocyanogen composition, it is not only bright in colour, dye excellent, jam can be widely used in, in acidic drinks and fruit wine, and there is certain trophism compared with synthetic colour, have and improve liver, the peroxidation of defence health, prevent arteriosclerosis and improve the physiological functions such as eyesight, a kind of important natural food colour and desirable foodstuff additive, therefore its pigment to be extracted and utilization seems abnormal important.
As natural pigment, grape skin color extracting method has solvent extraction method, ultrasonic extraction, supercritical CO 2 extraction process, microwave radiation to induce extraction process and Enzymatic Extraction etc.Solvent extraction method is simple, convenient due to it, and Extracting temperature is low, quality better, uses the earliest, also extensive.Traditional is that extraction pigment has its advantage with ethanol, but shortcoming is quite a few, and pigment production is very low, easily causes waste, and the recovery of rear solvent too increases certain cost, and economic serviceability is lower; The Optimization Technology extraction time that Zhou Wenwen reports is longer, the cost of the extraction also increased to a certain extent.
Summary of the invention
Technical problem to be solved by this invention is the method overcoming traditional extraction grape skin color.Extract length consuming time, solvent consumption be large, extracted amount is low, high in cost of production shortcoming, thus provide a kind of extracting method of new grape skin color, improve traditional alcohol extraction, grape skin color extraction yield is improve while not increasing extraction cost, shorten extraction time, decrease the usage quantity of solvent, for the industry using value expanding grape skin color lays the first stone.
The invention provides a kind of Extraction Conditions of Grape Skin Pigments, comprise the steps:
(1) grape skin powder of drying is mixed with 95wt% ethanol, adjust pH value to 2-4 with aqueous citric acid solution, under room temperature, high speed pre-treatment, homogeneous extracts, and filters;
(2) mixed with 95wt% ethanol by the filter residue after filtration, regulate pH value to 2-4 with aqueous citric acid solution, under room temperature, homogeneous extracts, and filters;
(3) by centrifugal for the filtrate of step (1) and (2), collect supernatant liquor, lyophilize is powdered, namely obtains grape skin color;
Wherein, high speed pre-treatment described in step (1) is with 5000-10000 rev/min of process more than 5 minutes, is preferably 5-20 minute; Homogeneous in step (1) or (2) is extracted as with 1000-4000 rev/min of process more than 10 minutes, is preferably 10-60 minute.
Wherein, the size of described grape skin powder is preferably and can crosses 100 object sieves.
Wherein, described grape skin powder can obtain according to this area ordinary method, is obtained in the present invention by following step: get fresh Pericarpium Vitis viniferae through washing, dry, grinding and sieving; Described sieving was preferably 100 mesh sieves.
In step (1), the mass volume ratio of described grape skin powder and described 95wt% ethanol is preferably 1g/mL ~ 1g/10mL, is more preferably 1g/5mL ~ 1g/10mL.
In step (2), the mass volume ratio of described filter residue and described 95wt % ethanol is preferably 1g/mL ~ 1g/10mL, is more preferably 1g/5mL ~ 1g/10mL.
The present invention is not particularly limited for the concentration of the aqueous citric acid solution of step (1) or (2), as long as citric acid solid can be made to dissolve, the concentration as aqueous citric acid solution can be 0.1mol/L.
In the embodiment that the present invention one is better, described high speed pre-treatment is with 9000-10000 rev/min of process 5-10 minute, and step (1) and the homogeneous described in step (2) are extracted as with 3000 revs/min of process 10-30 minute.
In the present invention, described high speed pre-treatment and described homogeneous extract and all can carry out in clarifixator.
In step (3), described centrifugal rotating speed is preferably 200-2000 rev/min, is more preferably 1000 revs/min.The described centrifugal time is preferably more than 5 minutes, is more preferably 5-30 minute, is 5-15 minute best.
In the present invention one preferably embodiment, described centrifugal condition is: with 1000 revs/min of centrifugal 5-15 minute.
Preferably, the supernatant liquor of step (3) is first carried out concentrated lyophilize again.The operation steps of described concentrated employing this area routine, the general mode adopting vacuum concentration, thus be more conducive to lyophilize.Generally be concentrated into solid content in described supernatant liquor and reach more than 30%.
Present invention also offers and a kind ofly extracted the grape skin color obtained by above-mentioned technique.
Room temperature of the present invention is that this area is understood the routine of room temperature, refers generally to 5-40 DEG C.
On the basis meeting this area general knowledge, above-mentioned each optimum condition can arbitrary combination, obtains the preferred embodiments of the invention.
All commercially, and chemical reagent purity used is at least food grade for the reagent that the present invention uses, raw material and equipment.
Positive progressive effect of the present invention is:
(1) extraction of grape skin color of the present invention be high-shear homogenizing machine auxiliary under carry out in two stages, it is less that the small-particle of Pericarpium Vitis viniferae becomes by the high speed pre-treatment of first stage, make it more easily be distributed in equably in solution, reach extraction effect relatively more even, extraction comparison is thorough; And extract the stage compared with the homogeneous under low rate, also comparatively standing extraction or other extracting method have higher pigment extraction yield.
(2) the present invention's aqueous citric acid solution regulates pH value, decreases the pungency utilizing the acid such as hydrochloric acid, and citric acid can be used as acidic flavoring agent and the sanitas of pigment simultaneously, adds the reliability of pigment as feed utilisation.
(3) extraction process of the present invention is simple, and require low to production unit, extraction efficiency is high, and extraction time is short, is obviously better than traditional solvent extraction method.And described extraction process can at room temperature be carried out, do not need to carry out heating and extract.
(4) the grape skin color good water solubility of present invention process extraction, product appearance color and luster is good, and proterties is stablized, and is suitable for as foodstuff additive and healthy food material.
4, accompanying drawing explanation
Fig. 1 is the process flow sheet of extracting method of the present invention.
5, embodiment
Further illustrate the present invention by embodiment below, but the present invention is not limited, the raw material in embodiment is conventional commercial product.
Embodiment 1
1) getting new fresh hide through washing post-drying to constant weight, finally pulverizing 100 mesh sieve and making grape skin powder, and taking above-mentioned grape skin powder 100 grams, for subsequent use.
2) 95wt% ethanol (grape skin powder: 95wt% ethanol=1g: 5mL) is added, and regulate pH value to 2.0 with the citric acid solution of 0.1 mol/L, under room temperature, with 10000 revs/min of high speed pre-treatment 5 minutes, then filter after extracting 30 minutes with 3000 revs/min of homogeneous.
3) filtrate is collected, 95wt% ethanol (filter residue: 95wt% ethanol=1g: 5mL) is added in filter residue, and regulate pH value to 2.0 with the citric acid solution of 0.1 mol/L, under room temperature, filter after extracting 30 minutes with 3000 revs/min of homogeneous.
4) twice filtrate is merged, at room temperature, centrifugal 10 minutes with 1000 revs/min, go precipitation, carry out lyophilize after collecting supernatant powdered, namely obtain grape skin color 3.26 grams, color: red-purple.
Embodiment 2
1) getting new fresh hide through washing post-drying to constant weight, pulverizing 100 mesh sieves, and making grape skin powder, and taking above-mentioned grape skin powder 100 grams, for subsequent use.
2) 95wt% ethanol (grape skin powder: 95wt% ethanol=1g: 7mL) is added, and regulate pH value to 3.0 with the citric acid solution of 0.1 mol/L, under room temperature, with 10000 revs/min of high speed pre-treatment 10 minutes, then filter after extracting 20 minutes with 3000 revs/min of homogeneous.
3) filtrate is collected, 95wt% ethanol (filter residue: 95wt% ethanol=1g: 7mL) is added in filter residue, and regulate pH value to 3.0 with the citric acid solution of 0.1 mol/L, filter extract 20 minutes with 3000 revs/min of homogeneous under room temperature after.
4) twice filtrate is merged, at room temperature, centrifugal 15 minutes with 1000 revs/min, go precipitation, carry out lyophilize after collecting supernatant powdered, namely obtain grape skin color 3.35 grams, color: red-purple.
Embodiment 3
1) getting new fresh hide through washing post-drying to constant weight, pulverizing 100 mesh sieves, and making grape skin powder, and taking above-mentioned grape skin powder 100 grams, for subsequent use.
2) 95wt% ethanol (grape skin powder: 95wt% ethanol=1g: 10mL) is added, and regulate pH value to 4.0 with the citric acid solution of 0.1 mol/L, under room temperature, with 10000 revs/min of high speed pre-treatment 10 minutes, then filter after extracting 10 minutes with 3000 revs/min of homogeneous.
3) filtrate is collected, 95wt% ethanol (filter residue: 95wt% ethanol=1g: 10mL) is added in filter residue, and by the citric acid solution adjust ph to 4.0 of 0.1 mol/L, filter extract 10 minutes with 3000 revs/min of homogeneous under room temperature after.
4) twice filtrate is merged, at room temperature, centrifugal 15 minutes with 1000 revs/min, go precipitation, carry out lyophilize after collecting supernatant powdered, namely obtain grape skin color 3.31 grams, color: red-purple.
Embodiment 4
1) getting new fresh hide through washing post-drying to constant weight, finally pulverizing 100 mesh sieve and making grape skin powder, and taking above-mentioned grape skin powder 100 grams, for subsequent use.
2) 95wt% ethanol (grape skin powder: 95wt% ethanol=1g: 10mL) is added, and regulate pH value to 2.0 with the citric acid solution of 0.1 mol/L, under room temperature, 5000 revs/min of high speed pre-treatment 20 minutes, then filter after extracting 60 minutes with 1000 revs/min of homogeneous.
3) filtrate is collected, 95wt% ethanol (filter residue: 95wt% ethanol=1g: 10mL) is added in filter residue, and by the citric acid solution adjust ph to 2.0 of 0.1 mol/L, under room temperature, filter after extracting 60 minutes with 1000 revs/min of homogeneous.
4) merge twice filtrate, at room temperature, centrifugal 30 minutes with 200 revs/min, go precipitation, being concentrated into solid content after collecting supernatant is 30%, and lyophilize is powdered, namely obtains grape skin color 3.30 grams, color: red-purple.
Claims (5)
1. an extraction process for grape skin color, comprises the steps:
(1) grape skin powder of drying is mixed with 95wt% ethanol, adjust pH value to 2-4 with aqueous citric acid solution, under room temperature, high speed pre-treatment, homogeneous extracts, and filters;
(2) mixed with 95wt% ethanol by the filter residue after filtration, regulate pH value to 2-4 with aqueous citric acid solution, under room temperature, homogeneous extracts, and filters;
(3) by centrifugal for the filtrate of step (1) and (2), collect supernatant liquor, lyophilize is powdered, namely obtains grape skin color;
Wherein, described high speed pre-treatment is with 5000-10000 rev/min of process more than 5 minutes; Homogeneous in step (1) or (2) is extracted as with 1000-4000 rev/min of process more than 10 minutes.
2. the extraction process as described in claim 1, is characterized in that: the described high speed pretreated time is 5-20 minute; The time that step (1) or (2) middle homogeneous extract is 10-60 minute.
3. the extraction process as described in claim 1, it is characterized in that: described high speed pre-treatment is for processing 5-10 minute with 9000-10000 rev/min, and step (1) and the homogeneous described in step (2) are extracted as with 3000 revs/min of process 10-30 minute.
4. the extraction process as described in claim 1, is characterized in that: described grape skin powder is of a size of can cross 100 object sieves; Described grape skin powder is preferably obtained by following method: get fresh Pericarpium Vitis viniferae through washing, dry, grinding and sieving.
5. the extraction process according to any one of Claims 1 to 4, is characterized in that: in step (1), and the mass volume ratio of described grape skin powder and described 95wt% ethanol is 1g/mL ~ 1g/10mL, is preferably 1g/5mL ~ 1g/10mL; In step (2), the mass volume ratio of described filter residue and described 95wt% ethanol is 1g/mL ~ 1g/10mL, is preferably 1g/5mL ~ 1g/10mL.
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| CN201310431198.4A CN104448902A (en) | 2013-09-22 | 2013-09-22 | Grape skin pigment extraction technology |
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| CN201310431198.4A CN104448902A (en) | 2013-09-22 | 2013-09-22 | Grape skin pigment extraction technology |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104804467A (en) * | 2015-05-15 | 2015-07-29 | 湖南农业大学 | Davidii foex pigment preparation method |
| CN105385188A (en) * | 2015-12-09 | 2016-03-09 | 重庆三零三科技有限公司 | Preparation method of mulberry red pigment |
| CN106634028A (en) * | 2016-12-09 | 2017-05-10 | 新疆维吾尔自治区产品质量监督检验研究院 | High-efficiency grape skin pigment extraction process |
| CN107183443A (en) * | 2017-05-11 | 2017-09-22 | 邸翀 | Amur grape beverage and preparation method and application |
| 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 |
-
2013
- 2013-09-22 CN CN201310431198.4A patent/CN104448902A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104804467A (en) * | 2015-05-15 | 2015-07-29 | 湖南农业大学 | Davidii foex pigment preparation method |
| CN105385188A (en) * | 2015-12-09 | 2016-03-09 | 重庆三零三科技有限公司 | Preparation method of mulberry red pigment |
| CN106634028A (en) * | 2016-12-09 | 2017-05-10 | 新疆维吾尔自治区产品质量监督检验研究院 | High-efficiency grape skin pigment extraction process |
| CN107183443A (en) * | 2017-05-11 | 2017-09-22 | 邸翀 | Amur grape beverage and preparation method and application |
| CN107183443B (en) * | 2017-05-11 | 2020-11-10 | 邸翀 | Wild grape beverage and preparation method and application thereof |
| 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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