CN112852182A - Pigment extraction process of blackcurrant raisin skin residues - Google Patents
Pigment extraction process of blackcurrant raisin skin residues Download PDFInfo
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- CN112852182A CN112852182A CN202110010018.XA CN202110010018A CN112852182A CN 112852182 A CN112852182 A CN 112852182A CN 202110010018 A CN202110010018 A CN 202110010018A CN 112852182 A CN112852182 A CN 112852182A
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- 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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- 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
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0096—Purification; Precipitation; Filtration
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Abstract
A pigment extraction process of blackcurrant raisin pomace comprises the following steps: s1: weighing dried blackcurrant grape skin residues, adding water, keeping the temperature in a water bath, soaking and softening the skin residues, and pulping the softened skin residues; s2: cooling the slurry obtained in the step S1 to 30 ℃, inoculating activated yeast for fermentation, squeezing and filtering after the fermentation is finished to obtain fermentation liquor for later use, and treating filter residues through a step S3; s3: soaking the filter residue treated by the S2 and an equal weight of ethanol solution in a water bath kettle at a constant temperature, squeezing and filtering to obtain a filtrate; s4: mixing the fermentation liquor obtained in the step S2 with the filtrate treated in the step S3, centrifuging to obtain supernatant, performing vacuum rotary evaporation to obtain high-purity concentrated solution, and recovering ethanol; s5: and (4) freeze-drying the concentrated solution obtained after the S4 treatment to obtain high-purity pigment solid powder. The invention effectively solves the problems of low purity, large acid-alcohol dosage, complex process flow, high sugar content and high cost of the existing blackcurrant peel residue pigment extraction process.
Description
Technical Field
The invention relates to the technical field of functional food processing, in particular to a pigment extraction process of dried skin residues of blackcurrant grapes (also suitable for dried fruits with high pulp fiber content, high acidity and high sugar).
Background
Blackcurrant grapes grow in the northern region of the Xinjiang Aletai mountain and are rich in vitamin C, phosphorus, magnesium, potassium, calcium, pigments and phenolic substances, wherein the blackcurrant raisins are rich in pigments, and about 91% of the total pigments exist in the fruit peel. In the processing process of the blackcurrant raisins, a large amount of small fruits, peel residues and fruit stalks can be produced through the processes of grading, removing stalks and the like, and the blackcurrant raisins cannot be eaten, so that not only is the resources wasted, but also the environmental pollution is great, and therefore, the method has great practical significance and development prospect in extracting and utilizing the pigment in the peel residues of the blackcurrant raisins.
The blackcurrant pigment contains flavonoids as main coloring components, and delphinidin and cyanidin as main anthocyanidin. In addition, it contains saccharides and acids present in natural materials. With the attention of people on the safety of the synthetic edible pigment and the continuous development of the natural pigment, the natural pigment becomes an ideal resource for replacing the synthetic edible pigment due to safety, no toxicity, rich resources and certain nutritional and pharmacological effects at home and abroad, so the research and development of the blackcurrant raisin pigment are gradually developed. The existing extraction method is that the ratio of the skin residue to the extractant is 1: and 5 (mass-to-volume ratio), wherein the extraction temperature is 50 ℃, the extraction time is 15min, and the red pigment is obtained by repeated extraction. The obtained haematochrome is adsorbed by ion exchange resin, then the impurities are removed, and after two-step elution by using ethanol-hydrochloric acid, more than 85% of the haematochrome can be recovered. Zhang Dongxue in the study on the parameters of extraction process of blackcurrant pigment, the extraction method of blackcurrant pigment is carried out by leaching with 1% hydrochloric acid and absolute ethyl alcohol as extraction solvent. Also, for example, patent publication No. CN110452209A discloses "a process for extracting blackcurrant pigment" which uses hydrochloric acid, ethanol, benzoic acid and cupric chloride to extract blackcurrant pigment. The method improves the extraction process of the blackcurrant pigment to a certain extent, but the acid-alcohol method is adopted to extract the pigment of the dry skin residue of the blackcurrant grapes, the acid-alcohol dosage is large, the process is complex, the effect on the squeezed wet skin residue is good, however, the cellulose content of the waste dry skin residue generated after the processing of the blackcurrant raisins is high, the pulp is compact, the acid-alcohol solution is difficult to permeate, the acidity and the sugar content of the skin residue are high, and the pigment solution extracted by the method is viscous and difficult to spray and store. The ion exchange resin is adopted to adsorb and remove impurities mainly containing sugar, a large amount of sugar-containing wastewater can be generated, secondary pollution is caused, the sugar in the peel residue is wasted, and meanwhile, the operations of resin adsorption, desorption and regeneration are complex, the cost is increased, a solution system is increased, concentration and drying are difficult, and the wastewater amount is increased.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide the pigment extraction process of the blackcurrant raisin pomace, which is suitable for dry fruits rich in pigment, high in cellulose content, compact in pulp, high in acid and high in saccharide, and effectively solves the problems of low purity (high sugar content), large acid and alcohol consumption, complex process, high cost (processing) and large wastewater amount in the conventional blackcurrant pomace pigment extraction process.
In order to achieve the purpose, the invention adopts the technical scheme that:
a pigment extraction process of blackcurrant raisin pomace comprises the following steps:
s1: a pretreatment stage; weighing dried skin residues of blackcurrant grapes, adding a proper amount of water, keeping the temperature of a water bath kettle at 60 ℃ for 30min, soaking and softening the skin residues, inhibiting the growth of mixed bacteria, and pulping the softened skin residues;
s2: fermenting with yeast; cooling the slurry obtained in the step S1 to 30 ℃, fermenting the slurry with activated alcohol yeast (20-30 g/100 kg of peel residue and fruit pulp), squeezing and filtering the fermented slurry to obtain a fermentation liquid for later use after the fermentation is finished, and treating filter residues with S3;
s3: extracting; keeping the temperature of the filter residue treated by the S2 and an equal weight of ethanol solution in a water bath kettle at 60 ℃ for 30min, squeezing and filtering to obtain a filtrate;
s4: centrifuging, concentrating and recovering ethanol; mixing the fermentation liquor obtained in the step S2 with the filtrate treated in the step S3, centrifuging to obtain supernatant, performing vacuum rotary evaporation to obtain high-purity concentrated solution, and recovering ethanol;
s5: drying into powder; and (4) freeze-drying the concentrated solution obtained after the treatment of S4 to obtain high-purity pigment solid powder.
And in the S1 pretreatment, the skin and the residue of the dried blackcurrant grapes are soaked in water according to the mass ratio of 1:2, 1:3 and 1: 4.
The fermentation was carried out at 30 ℃ for 3 days in S2.
The ethanol solution with medium weight in the S3 is ethanol solution with 95 percent (mass percentage).
And in the S4, the centrifugal speed is 6000rpm, the centrifugal time is 10min, and the supernatant is concentrated by 5-10 times.
The temperature of the freeze drying in the S5 is-80 ℃, and the vacuum degree is less than 10 Pa.
The invention has the beneficial effects that:
1. the slurry of the dried skin residue of blackcurrant grapes generates a large amount of CO in the alcoholic fermentation process2And ethanol (after fermentation, the ethanol content is 5-8% by mass percent), CO2The formed anaerobic environment can effectively avoid the oxidation of the pigment in the traditional extraction process, and simultaneously, a solution system formed by the produced ethanol and the existing organic acid in the skin residue is beneficial to the dissolution of the pigment in the skin residue of the blackcurrant raisin.
2. After fermentation is finished, the separated filter residue also contains a small amount of pigment (about 10% of the total pigment), and in order to improve the raw material yield, the pigment remained in the filter residue is extracted by ethanol with equal weight once, so that the steps of the traditional process are simplified, and the ethanol dosage is greatly reduced. Meanwhile, in the continuous production state, only a small amount of ethanol solution needs to be supplemented, and the ethanol produced in the fermentation process can basically make up for the loss of the ethanol (loss is 5-10%) in the process of extracting the pigment from the filter residue by using the ethanol.
3. The fermentation process removes sugar (glucose, fructose, sucrose and the like) which is difficult to separate in the traditional process in the dried skin residue of the blackcurrant raisin, simplifies the purification steps and is beneficial to preparing high-purity powdery pigment products.
Detailed Description
The present invention will be described in further detail with reference to examples.
The invention relates to a process for extracting pigment from blackcurrant raisin skin residue, which is based on blackcurrant raisin skin residue and aims at obtaining the optimal pigment extraction process by taking the pigment as the main component in the extract, and specifically, the inventor performs the following tests, wherein the specific test process is as follows:
example 1
Weighing 50g of blackcurrant raisin skin residues, adding water according to the material-water ratio of 1:2, preserving the heat of a water bath kettle at 60 ℃ for 30min, pulping, cooling to 30 ℃, and then inoculating 0.01g of activated alcohol yeast (20g of dry yeast per 100kg of skin residues) to ferment for 3 days at 30 ℃, wherein the content of ethanol produced by fermentation can reach 8% (mass percentage concentration). And (3) after fermentation, squeezing and filtering to obtain fermentation liquor for later use, adding an equal weight of ethanol solution (95% ethanol by mass percent) into solid filter residue, extracting the pigment in water bath at 60 ℃ for 30min, squeezing and filtering to obtain filtrate, mixing the filtrate with the fermentation liquor, centrifuging at 6000rpm for 10min, concentrating supernatant for 5 times, and freeze-drying to obtain blackcurrant raisin peel residue pigment powder.
3.263g of finished product is finally obtained, the content of anthocyanin (calculated by cyanidin-o-glucoside) is 0.125g, the purity of the product is 3.831%, and the purity of the anthocyanin (calculated by cyanidin-o-glucoside) is 4.73 times of that of the acid-alcohol method.
Example 2
Weighing 50g of blackcurrant raisin skin residues, adding water according to the material-water ratio of 1:3, preserving the heat of a water bath kettle at 60 ℃ for 30min, pulping, cooling to 30 ℃, and then inoculating 0.01g of activated alcohol yeast (20g of dry yeast per 100kg of skin residues) to ferment for 3 days at 30 ℃, wherein the content of ethanol produced by fermentation can reach 6% (mass percentage concentration). And (3) after fermentation, squeezing and filtering to obtain fermentation liquor for later use, adding an equal weight of ethanol solution (95% ethanol by mass percent) into solid filter residue, extracting the pigment in water bath at 60 ℃ for 3min, squeezing and filtering to obtain filtrate, mixing the filtrate with the fermentation liquor, centrifuging at 6000rpm for 10min, concentrating the supernatant by 10 times, and freeze-drying to obtain blackcurrant raisin skin residue pigment powder.
4.148g of finished product is finally obtained, the content of anthocyanin (calculated by cyanidin-o-glucoside) is 0.112g, the product purity is 2.070%, and the purity of the anthocyanin (calculated by cyanidin-o-glucoside) is 2.56 times of that of the acid-alcohol method.
Example 3
Weighing 50g of blackcurrant raisin skin residues, adding water according to the material-water ratio of 1:4, preserving the heat of a water bath kettle at 60 ℃ for 30min, pulping, cooling to 30 ℃, and then inoculating 0.01g of activated alcohol yeast (20g of dry yeast per 100kg of skin residues) to ferment for 3 days at 30 ℃, wherein the content of ethanol produced by fermentation can reach 5% (mass percentage concentration). And (3) after fermentation, squeezing and filtering to obtain fermentation liquor for later use, adding an equal weight of ethanol solution (95% ethanol by mass percent) into solid filter residue, extracting the pigment in water bath at 60 ℃ for 30min, squeezing and filtering to obtain filtrate, mixing the filtrate with the fermentation liquor, centrifuging at 6000rpm for 10min, concentrating the supernatant by 10 times, and freeze-drying to obtain blackcurrant raisin skin residue pigment powder.
7.037g of finished product is finally obtained, the content of anthocyanin (calculated by cyanidin-o-glucoside) is 0.119g, the purity of the product is 1.691%, and the purity of the anthocyanin (calculated by cyanidin-o-glucoside) is 2.08 times of that of the acid-alcohol method.
And (4) supplementary notes:
pigment content determination method (measured by cyanidin-o-glucoside)
Dilutions were prepared at pH 1 and pH 4.5, and 0.5ml of pigment from feed-water ratio 1:3 and 1:4 was diluted 25-fold and 0.5ml of pigment from feed-water ratio 1:5 was diluted 50-fold, shaken and left to stand in the dark for 30min, and the absorbance was measured at 520nm and 700nm, and the pigment content (in terms of cyanidin-o-glucoside) was calculated by the pH differential method.
Acid alcohol extraction of blackcurrant raisin skin residue pigment (conventional extraction method for comparison)
Weighing 50g of blackcurrant raisin skin residues, adding water according to the material-water ratio of 1:2, preserving heat at 60 ℃ for 30min, pulping, adding an acid-alcohol solution (95% ethanol and 1% hydrochloric acid in mass percent) according to the material-liquid ratio of 1:5, preserving heat at 60 ℃ for 30min, filtering to obtain a filtrate for later use, leaching the filter residues twice according to the extraction conditions, combining the three filtrates, centrifuging at 6000rpm for 10min, taking supernatant, concentrating by 40 times, and freeze-drying to obtain the pigment. 12.346g of finished product is finally obtained, the content of anthocyanin (calculated by cyanidin-o-glucoside) is 0.100g, and the purity of the product is 0.810%.
The invention has the advantages that:
by adopting the method, the purity of the pigment (calculated by cyanidin-o-glucoside) is improved by 2-4.7 times, the extraction steps are simplified, the dosage of an organic solvent is reduced, the sugar in impurities is effectively utilized, the pollution emission is reduced, and the utilization rate of raw materials is improved.
Large amount of CO is generated after fermentation of blackcurrant grape dry skin and residue slurry2And ethanol, CO2The oxidation of the pigment can be avoided, most of the pigment contained in the skin residue of the blackcurrant raisin is dissolved in the fermentation liquor formed by ethanol and the existing organic acid in the skin residue, a small amount of pigment exists in the filter residue after fermentation, squeezing and filtration, and the filter residue can be extracted once by an ethanol method, so that the using amount of the ethanol is greatly reduced, and the ethanol (5-8%) produced in the fermentation process basically compensates for the loss of the ethanol (5-10% of the normal loss) in the extraction process.
During the fermentation process, sugar which is difficult to separate from the skin residue is converted into alcohol, the sugar which is difficult to separate from the skin residue of the blackcurrant raisin is removed, the viscosity of the concentrated solution is reduced, and the method is favorable for preparing a high-purity powdery pigment product by freeze drying and is easy to store.
Claims (6)
1. A pigment extraction process of blackcurrant raisin skin residues is characterized by comprising the following steps:
s1: a pretreatment stage; weighing dried skin residues of blackcurrant grapes, adding a proper amount of water, keeping the temperature of a water bath kettle at 60 ℃ for 30min, soaking and softening the skin residues, and pulping the softened skin residues;
s2: fermenting with yeast; cooling the slurry obtained in the step S1 to 30 ℃, fermenting the slurry by activated yeast, squeezing and filtering the slurry to obtain a fermentation liquid for later use after the fermentation is finished, and treating filter residues by the step S3;
s3: extracting; keeping the temperature of the filter residue treated by the S2 and an equal weight of ethanol solution in a water bath kettle at 60 ℃ for 30min, squeezing and filtering to obtain a filtrate;
s4: centrifuging, concentrating and recovering ethanol; mixing the fermentation liquor obtained in the step S2 with the filtrate treated in the step S3, centrifuging to obtain supernatant, performing vacuum rotary evaporation to obtain high-purity concentrated solution, and recovering ethanol;
s5: drying into powder; and (4) freeze-drying the concentrated solution obtained after the treatment of S4 to obtain high-purity pigment solid powder.
2. The pigment extraction process of the blackcurrant raisin pomace according to claim 1, wherein the blackcurrant raisin pomace in the pretreatment of S1 is soaked in water according to the mass ratio of 1:2, 1:3 and 1: 4.
3. The process for extracting pigment from blackcurrant raisin pomace according to claim 1, wherein the fermentation in S2 is carried out at 30 ℃ for 3 days.
4. The pigment extraction process of the blackcurrant raisin pomace according to claim 1, wherein in the step S4, the centrifugal speed is 6000rpm, the centrifugal time is 10min, and the supernatant is concentrated by a factor of 5-10.
5. The pigment extraction process of the dried skin residue of the blackcurrant grapes according to claim 1, wherein the ethanol solution with the medium weight in the S3 is a 95% ethanol solution (by mass percentage).
6. The process for extracting pigment from blackcurrant raisin pomace according to claim 1, wherein the temperature of the freeze drying in the S5 is-80 ℃ and the vacuum degree is less than 10 Pa.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113817553A (en) * | 2021-06-22 | 2021-12-21 | 努丽扎提·木拉提别克 | Production method of antioxidant blackcurrant-raisin fruit wine |
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| CN1657569A (en) * | 2005-02-28 | 2005-08-24 | 大连轻工业学院 | Process for preparating solid natural edible pigment from black plum |
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| CN106046852A (en) * | 2016-07-15 | 2016-10-26 | 广西顺帆投资有限公司 | Method for extracting dye based on waxberry tree barks |
| CN107011309A (en) * | 2017-04-21 | 2017-08-04 | 沈阳市皇冠蓝莓产业有限公司 | A kind of preparation method of Anthocyanin from Blueberry |
| CN107501365A (en) * | 2017-07-17 | 2017-12-22 | 长沙湘资生物科技有限公司 | A kind of method that raspberry glycosides and anthocyanin are extracted from raspberry |
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- 2021-01-05 CN CN202110010018.XA patent/CN112852182A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1657569A (en) * | 2005-02-28 | 2005-08-24 | 大连轻工业学院 | Process for preparating solid natural edible pigment from black plum |
| CN105130941A (en) * | 2015-08-31 | 2015-12-09 | 桂林茗兴生物科技有限公司 | Preparation method of grape seed extract |
| CN106046852A (en) * | 2016-07-15 | 2016-10-26 | 广西顺帆投资有限公司 | Method for extracting dye based on waxberry tree barks |
| CN107011309A (en) * | 2017-04-21 | 2017-08-04 | 沈阳市皇冠蓝莓产业有限公司 | A kind of preparation method of Anthocyanin from Blueberry |
| CN107501365A (en) * | 2017-07-17 | 2017-12-22 | 长沙湘资生物科技有限公司 | A kind of method that raspberry glycosides and anthocyanin are extracted from raspberry |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113817553A (en) * | 2021-06-22 | 2021-12-21 | 努丽扎提·木拉提别克 | Production method of antioxidant blackcurrant-raisin fruit wine |
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