CN104974194A - Technology for extracting polyphenol from grape peel residues - Google Patents
Technology for extracting polyphenol from grape peel residues Download PDFInfo
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- CN104974194A CN104974194A CN201510372659.4A CN201510372659A CN104974194A CN 104974194 A CN104974194 A CN 104974194A CN 201510372659 A CN201510372659 A CN 201510372659A CN 104974194 A CN104974194 A CN 104974194A
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Abstract
The invention discloses a technology for extracting polyphenol from grape peel residues, and belongs to the technical field of plant polyphenol extraction. The extraction technology comprises the following five steps: grape peel residue powder preparation, nitrogen gas protection, ultrasonic extraction, separation, and condensation and drying. The extraction technology solves the problems that in the prior art the effective components are badly destroyed during the extraction process, the product yield and purity are low, the production cost is high, and the environment is polluted, and has the advantages of high utilization rate of raw materials and high extraction rate.
Description
Technical field
The present invention relates to plant polyphenol extractive technique field, specifically a kind of extraction process of grape skin polyphenol.
Background technology
Grape is the treasure in fruit, has the good reputation of " fruit queen ", and it is delicious salubrious again and nutritious, also has the effects such as benefiting vital QI and blood, strengthening the bones and muscles, the meridian dredging, is therefore loved by the people.Grape is one of fruit that output is maximum in the world, and annual production is 6,500 ten thousand tons, and wherein 80% for wine brewing.
Polyphenol substance is the general name that hydroxyl is connected directly between phenols on phenyl ring and polymkeric substance.They have different physiological roles and pharmacological action, as having oxidation-resistance, interior free yl can be eliminated, anti-ageing, reducing blood-fat, hypotensive, preventing cardiovascular disease, anti-cancer and cancer-preventing, the effect such as antibacterial, have broad application prospects in fields such as grease, food, medicine, daily use chemicals.The waste (skin, seed, stalk) produced in Grape processing process accounts for about 20% of fresh fruit gross weight, the research deepened continuously both at home and abroad finds, containing a large amount of monomer polyphenol and Condenced Phenols class functional substance in grape skin, there is good medical treatment, health-care effect.
At present, China's Wine Grape waste (being commonly called as grape skin) major part is as fertilizer, feed or burn material, even refuse treatment, and not only causing environmental pollution, be also the significant wastage to raw material, and utilization ratio is very low.Grape skin comprehensive utilization has become the value-added new direction of grape wine secondary industry.
Summary of the invention
The object of the present invention is to provide a kind of extraction process of grape skin polyphenol, to solve the problem proposed in above-mentioned background technology.
For achieving the above object, the invention provides following technical scheme:
An extraction process for grape skin polyphenol, comprises the following steps:
Step one, grape skin powder preparation: wine grape pomace is separated postlyophilization through washing, skin seed, then pulverized 100 ~ 150 mesh sieves with plant pulverizer and collected powder, be Pericarpium Vitis viniferae ground-slag;
Step 2, nitrogen protection: the Pericarpium Vitis viniferae ground-slag of step one is placed in extraction kettle, adds aqueous ethanolic solution by solid-liquid ratio 1:5 ~ 9 and fully mix, use vacuum pump deoxidation, then pass into pure nitrogen gas;
Step 3, supersound extraction: after passing into nitrogen, carries out ultrasonic extraction under the constant temperature of 60 ~ 85 DEG C, and extract 2 times, extraction time is 20 ~ 35min, merges 2 times and extracts the grape skin solution obtained containing residue;
Step 4, is separated: by separator by carrying out filtering containing the grape skin polyphenol solution of residue in step 3, centrifugal, discard filter residue, obtain supernatant liquor;
Step 5, concentrate drying: carry out concentrated frozen drying to supernatant liquor, vacuum tightness remains on as 10Pa ~ 20Pa, continues 10 ~ 12 hours, obtains grape skin polyphenol finished product.
As the preferred technical solution of the present invention, the ridity that lyophilize described in step one reaches is 96%.
As the preferred technical solution of the present invention, the power of described step 3 supersound extraction is 280 ~ 350W, and frequency is 20 ~ 25kHz.
As the preferred technical solution of the present invention, in described aqueous ethanolic solution, the concentration of ethanol is 40% (v/v) ~ 70% (v/v).
In sum, the invention has the beneficial effects as follows: the present invention carries out intensified by ultrasonic wave process to leaching process, is utilize hyperacoustic Mechanical Crushing and cavatition, accelerates polyphenol extractive substance from grape skin to the speed of solvent diffusion, shorten extraction time, increase the extraction yield of effective constituent.The condition extracted, had both ensured that low-temperature short-time that is volatile, easily material spoiled, easy to change extracted, in turn ensure that the time, obtained reservation and the high extraction high density tea juice of color, smell and taste.It is simple that the present invention has technique, Extracting temperature is low, the rate of recovery is high, oxidation loss is little, joint time, energy-conservation, extraction yield advantages of higher, avoid the use of noxious solvent simultaneously, there is good commercial introduction and be worth.Pass into pure nitrogen gas, oxidizable grape skin polyphenol is obtained to supersound extraction and protects, significantly improve in this condition leaching yield, and quality of finished is high.When the protection of nitrogen makes supersound extraction grape skin polyphenol, not only reduce leaching temperature and shorten leaching time, and being conducive to reducing energy waste and reducing production cost.Utilize method of the present invention, extract grape skin polyphenol, extraction yield can reach more than 28%, and purity reaches more than 96%.
Embodiment
By the following examples the present invention is further elaborated:
Embodiment 1
An extraction process for grape skin polyphenol, comprises the following steps:
Step one, grape skin powder preparation: wine grape pomace is separated postlyophilization through washing, skin seed, then pulverized 100 mesh sieves with plant pulverizer and collected powder, be Pericarpium Vitis viniferae ground-slag;
Step 2, nitrogen protection: the Pericarpium Vitis viniferae ground-slag of step one is placed in extraction kettle, adds aqueous ethanolic solution by solid-liquid ratio 1:6 and fully mix, use vacuum pump deoxidation, then pass into pure nitrogen gas;
Step 3, supersound extraction: after passing into nitrogen, carries out ultrasonic extraction under the constant temperature of 60 DEG C, and extract 2 times, extraction time is 25min, merges 2 times and extracts the grape skin solution obtained containing residue;
Step 4, is separated: by separator by carrying out filtering containing the grape skin polyphenol solution of residue in step 3, centrifugal, discard filter residue, obtain supernatant liquor;
Step 5, concentrate drying: carry out concentrated frozen drying to supernatant liquor, vacuum tightness remains on as 15Pa, continues 10 hours, obtains grape skin polyphenol finished product.
Wherein, the ridity that lyophilize described in step one reaches is 96%.
Wherein, the power of described step 3 supersound extraction is 280 ~ 350W, and frequency is 22kHz.
Wherein, in described aqueous ethanolic solution, the concentration of ethanol is 65% (v/v).
Embodiment 2
An extraction process for grape skin polyphenol, comprises the following steps:
Step one, grape skin powder preparation: wine grape pomace is separated postlyophilization through washing, skin seed, then pulverized 120 mesh sieves with plant pulverizer and collected powder, be Pericarpium Vitis viniferae ground-slag;
Step 2, nitrogen protection: the Pericarpium Vitis viniferae ground-slag of step one is placed in extraction kettle, adds aqueous ethanolic solution by solid-liquid ratio 1:5 and fully mix, use vacuum pump deoxidation, then pass into pure nitrogen gas;
Step 3, supersound extraction: after passing into nitrogen, carries out ultrasonic extraction under the constant temperature of 85 DEG C, and extract 2 times, extraction time is 20min, merges 2 times and extracts the grape skin solution obtained containing residue;
Step 4, is separated: by separator by carrying out filtering containing the grape skin polyphenol solution of residue in step 3, centrifugal, discard filter residue, obtain supernatant liquor;
Step 5, concentrate drying: carry out concentrated frozen drying to supernatant liquor, vacuum tightness remains on as 10Pa, continues 10 hours, obtains grape skin polyphenol finished product.
Wherein, the ridity that lyophilize described in step one reaches is 96%.
Wherein, the power of described step 3 supersound extraction is 280 ~ 350W, and frequency is 20kHz.
Wherein, in described aqueous ethanolic solution, the concentration of ethanol is 40% (v/v).
Embodiment 3
An extraction process for grape skin polyphenol, comprises the following steps:
Step one, grape skin powder preparation: wine grape pomace is separated postlyophilization through washing, skin seed, then pulverized 150 mesh sieves with plant pulverizer and collected powder, be Pericarpium Vitis viniferae ground-slag;
Step 2, nitrogen protection: the Pericarpium Vitis viniferae ground-slag of step one is placed in extraction kettle, adds aqueous ethanolic solution by solid-liquid ratio 1:9 and fully mix, use vacuum pump deoxidation, then pass into pure nitrogen gas;
Step 3, supersound extraction: after passing into nitrogen, carries out ultrasonic extraction under the constant temperature of 60 DEG C, and extract 2 times, extraction time is 35min, merges 2 times and extracts the grape skin solution obtained containing residue;
Step 4, is separated: by separator by carrying out filtering containing the grape skin polyphenol solution of residue in step 3, centrifugal, discard filter residue, obtain supernatant liquor;
Step 5, concentrate drying: carry out concentrated frozen drying to supernatant liquor, vacuum tightness remains on as 10Pa ~ 20Pa, continues 12 hours, obtains grape skin polyphenol finished product.
Wherein, the ridity that lyophilize described in step one reaches is 96%.
Wherein, the power of described step 3 supersound extraction is 280 ~ 350W, and frequency is 25kHz.
Wherein, in described aqueous ethanolic solution, the concentration of ethanol is 70% (v/v).
Below by way of test, detect the content of grape skin polyphenol in embodiment 1-3, concrete grammar is as follows: the grape skin polyphenol finished product that the preparation method getting 1g embodiment 1 prepares, dissolve by suitable quantity of water, adding alcohol concn is again that 50% ethanolic soln is settled to 25mL, draw 1mL chromogenic assay absorbancy, replicate(determination) 3 times, calculate total phenol content, finally calculating polyphenol extracted amount is 26.547mg/g, it is simple that visible the present invention has technique, Extracting temperature is low, the rate of recovery is high, oxidation loss is little, during joint, energy-conservation, extraction yield advantages of higher, avoid the use of noxious solvent simultaneously, there is good commercial introduction be worth.Embodiment 2,3 has the technique effect same with embodiment.
In addition, be to be understood that, although this specification sheets is described according to embodiment, but not each embodiment only comprises an independently technical scheme, this narrating mode of specification sheets is only for clarity sake, those skilled in the art should by specification sheets integrally, and the technical scheme in each embodiment also through appropriately combined, can form other embodiments that it will be appreciated by those skilled in the art that.
Claims (4)
1. an extraction process for grape skin polyphenol, is characterized in that comprising the following steps:
Step one, grape skin powder preparation: wine grape pomace is separated postlyophilization through washing, skin seed, then pulverized 100 ~ 150 mesh sieves with plant pulverizer and collected powder, be Pericarpium Vitis viniferae ground-slag;
Step 2, nitrogen protection: the Pericarpium Vitis viniferae ground-slag of step one is placed in extraction kettle, adds aqueous ethanolic solution by solid-liquid ratio 1:5 ~ 9 and fully mix, use vacuum pump deoxidation, then pass into pure nitrogen gas;
Step 3, supersound extraction: after passing into nitrogen, carries out ultrasonic extraction under the constant temperature of 60 ~ 85 DEG C, and extract 2 times, extraction time is 20 ~ 35min, merges 2 times and extracts the grape skin solution obtained containing residue;
Step 4, is separated: by separator by carrying out filtering containing the grape skin polyphenol solution of residue in step 3, centrifugal, discard filter residue, obtain supernatant liquor;
Step 5, concentrate drying: carry out concentrated frozen drying to supernatant liquor, vacuum tightness remains on as 10Pa ~ 20Pa, continues 10 ~ 12 hours, obtains grape skin polyphenol finished product.
2. the extraction process of a kind of grape skin polyphenol as claimed in claim 1, is characterized in that: the ridity that lyophilize described in step one reaches is 96%.
3. the extraction process of a kind of grape skin polyphenol as claimed in claim 1, is characterized in that: the power of described step 3 supersound extraction is 280 ~ 350W, and frequency is 20 ~ 25kHz.
4. the extraction process of a kind of grape skin polyphenol as claimed in claim 1, is characterized in that: in described aqueous ethanolic solution, the concentration of ethanol is 40% (v/v) ~ 70% (v/v).
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105348331A (en) * | 2015-11-05 | 2016-02-24 | 广西大学 | Extraction method of plant polyphenol |
| CN108354962A (en) * | 2018-04-26 | 2018-08-03 | 江苏大学 | A method of based on nitrogen protection and ultrasound assisted extraction polyphenol from rapeseed |
| CN114031431A (en) * | 2021-12-28 | 2022-02-11 | 燕山大学 | Humic acid-rich pig manure compost prepared from wine grape skin residues and method and application thereof |
Citations (3)
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| CN103223261A (en) * | 2013-04-22 | 2013-07-31 | 华南理工大学 | Apparatus and method for pulsed electric field-assisted countercurrent extraction of grape skin residue polyphenol |
| CN103224538A (en) * | 2013-04-22 | 2013-07-31 | 华南理工大学 | Method for extracting grape skin residue polyphenols by synergy of ultrasound and pulsed electric field |
| CN104706834A (en) * | 2013-12-13 | 2015-06-17 | 中国农业科学院农产品加工研究所 | Polyphenol preparation method and beverage production method |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103223261A (en) * | 2013-04-22 | 2013-07-31 | 华南理工大学 | Apparatus and method for pulsed electric field-assisted countercurrent extraction of grape skin residue polyphenol |
| CN103224538A (en) * | 2013-04-22 | 2013-07-31 | 华南理工大学 | Method for extracting grape skin residue polyphenols by synergy of ultrasound and pulsed electric field |
| CN104706834A (en) * | 2013-12-13 | 2015-06-17 | 中国农业科学院农产品加工研究所 | Polyphenol preparation method and beverage production method |
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| 令博，等: "葡萄皮渣多酚超声波辅助提取工艺响应面法优化及抗氧化活性研究", 《食品科学》 * |
| 闫万理，等: "葡萄皮渣中多酚超声波提取工艺优化研究", 《伊犁师范学院学报（自然科学版）》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105348331A (en) * | 2015-11-05 | 2016-02-24 | 广西大学 | Extraction method of plant polyphenol |
| CN108354962A (en) * | 2018-04-26 | 2018-08-03 | 江苏大学 | A method of based on nitrogen protection and ultrasound assisted extraction polyphenol from rapeseed |
| CN114031431A (en) * | 2021-12-28 | 2022-02-11 | 燕山大学 | Humic acid-rich pig manure compost prepared from wine grape skin residues and method and application thereof |
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Inventor after: Yang Jing Inventor before: Wu Caiying |
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Effective date of registration: 20171208 Address after: 518131 room 1403-1404 of Xinwei mansion, No. 121, Jihui Road, Longhua, New District, Shenzhen, Guangdong Province, 1403-1404 room Applicant after: Shenzhen City Heng Shan Tang Biotechnology Co. Ltd. Address before: 530004 Nanning East Road, the Guangxi Zhuang Autonomous Region, No. 100 Applicant before: Guangxi University |
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