CN108835635A - A method of antioxidant is extracted by grape pip - Google Patents
A method of antioxidant is extracted by grape pip Download PDFInfo
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- CN108835635A CN108835635A CN201810725332.4A CN201810725332A CN108835635A CN 108835635 A CN108835635 A CN 108835635A CN 201810725332 A CN201810725332 A CN 201810725332A CN 108835635 A CN108835635 A CN 108835635A
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- grape pip
- 10min
- antioxidant
- chitosan oligosaccharide
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- 235000009754 Vitis X bourquina Nutrition 0.000 title claims abstract description 51
- 235000012333 Vitis X labruscana Nutrition 0.000 title claims abstract description 51
- 235000014787 Vitis vinifera Nutrition 0.000 title claims abstract description 51
- 239000003963 antioxidant agent Substances 0.000 title claims abstract description 25
- 230000003078 antioxidant effect Effects 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims abstract description 19
- 240000006365 Vitis vinifera Species 0.000 title 1
- 241000219095 Vitis Species 0.000 claims abstract description 50
- 230000008901 benefit Effects 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 56
- 229920002643 polyglutamic acid Polymers 0.000 claims description 33
- 235000019441 ethanol Nutrition 0.000 claims description 28
- 239000011347 resin Substances 0.000 claims description 25
- 229920005989 resin Polymers 0.000 claims description 25
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 22
- 229920001661 Chitosan Polymers 0.000 claims description 19
- 108010020346 Polyglutamic Acid Proteins 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 230000002745 absorbent Effects 0.000 claims description 18
- 239000002250 absorbent Substances 0.000 claims description 18
- 238000000227 grinding Methods 0.000 claims description 14
- RQFQJYYMBWVMQG-IXDPLRRUSA-N chitotriose Chemical compound O[C@@H]1[C@@H](N)[C@H](O)O[C@H](CO)[C@H]1O[C@H]1[C@H](N)[C@@H](O)[C@H](O[C@H]2[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O2)N)[C@@H](CO)O1 RQFQJYYMBWVMQG-IXDPLRRUSA-N 0.000 claims description 12
- 238000001179 sorption measurement Methods 0.000 claims description 12
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 claims description 11
- 229920000168 Microcrystalline cellulose Polymers 0.000 claims description 11
- 239000012459 cleaning agent Substances 0.000 claims description 11
- 239000001341 hydroxy propyl starch Substances 0.000 claims description 11
- 235000013828 hydroxypropyl starch Nutrition 0.000 claims description 11
- 235000019813 microcrystalline cellulose Nutrition 0.000 claims description 11
- 239000008108 microcrystalline cellulose Substances 0.000 claims description 11
- 229940016286 microcrystalline cellulose Drugs 0.000 claims description 11
- 235000019482 Palm oil Nutrition 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 239000003595 mist Substances 0.000 claims description 10
- 239000002540 palm oil Substances 0.000 claims description 10
- 238000002360 preparation method Methods 0.000 claims description 10
- 238000004321 preservation Methods 0.000 claims description 10
- 239000002002 slurry Substances 0.000 claims description 10
- 239000006228 supernatant Substances 0.000 claims description 10
- 239000011148 porous material Substances 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 6
- 238000004064 recycling Methods 0.000 claims description 6
- 238000003795 desorption Methods 0.000 claims description 5
- 238000004821 distillation Methods 0.000 claims description 5
- 238000003801 milling Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- 238000010992 reflux Methods 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 239000003599 detergent Substances 0.000 claims description 3
- 244000275012 Sesbania cannabina Species 0.000 claims 2
- 239000002253 acid Substances 0.000 claims 1
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 238000000605 extraction Methods 0.000 abstract description 3
- 238000011084 recovery Methods 0.000 abstract description 3
- 238000005202 decontamination Methods 0.000 abstract description 2
- 230000003588 decontaminative effect Effects 0.000 abstract description 2
- 239000000284 extract Substances 0.000 abstract description 2
- 230000001954 sterilising effect Effects 0.000 abstract description 2
- 238000004659 sterilization and disinfection Methods 0.000 abstract description 2
- 235000006708 antioxidants Nutrition 0.000 description 15
- 241000219782 Sesbania Species 0.000 description 8
- 235000013824 polyphenols Nutrition 0.000 description 7
- 150000008442 polyphenolic compounds Chemical class 0.000 description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- WHUUTDBJXJRKMK-UHFFFAOYSA-N Glutamic acid Natural products OC(=O)C(N)CCC(O)=O WHUUTDBJXJRKMK-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 235000013922 glutamic acid Nutrition 0.000 description 2
- 239000004220 glutamic acid Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 150000003254 radicals Chemical class 0.000 description 2
- 210000003491 skin Anatomy 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 241000219094 Vitaceae Species 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- ADRVNXBAWSRFAJ-UHFFFAOYSA-N catechin Natural products OC1Cc2cc(O)cc(O)c2OC1c3ccc(O)c(O)c3 ADRVNXBAWSRFAJ-UHFFFAOYSA-N 0.000 description 1
- 235000005487 catechin Nutrition 0.000 description 1
- 125000004403 catechin group Chemical group 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229950001002 cianidanol Drugs 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000004851 dishwashing Methods 0.000 description 1
- 230000003670 easy-to-clean Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229930003935 flavonoid Natural products 0.000 description 1
- 150000002215 flavonoids Chemical class 0.000 description 1
- 235000017173 flavonoids Nutrition 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 235000021021 grapes Nutrition 0.000 description 1
- 201000010235 heart cancer Diseases 0.000 description 1
- 208000019622 heart disease Diseases 0.000 description 1
- 208000024348 heart neoplasm Diseases 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 235000013372 meat Nutrition 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 230000035764 nutrition Effects 0.000 description 1
- 210000000056 organ Anatomy 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 230000009759 skin aging Effects 0.000 description 1
- 210000004927 skin cell Anatomy 0.000 description 1
- 230000037394 skin elasticity Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 208000024891 symptom Diseases 0.000 description 1
- 230000002087 whitening effect Effects 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/105—Plant extracts, their artificial duplicates or their derivatives
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L5/00—Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L5/00—Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
- A23L5/20—Removal of unwanted matter, e.g. deodorisation or detoxification
- A23L5/27—Removal of unwanted matter, e.g. deodorisation or detoxification by chemical treatment, by adsorption or by absorption
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L5/00—Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
- A23L5/30—Physical treatment, e.g. electrical or magnetic means, wave energy or irradiation
- A23L5/34—Physical treatment, e.g. electrical or magnetic means, wave energy or irradiation using microwaves
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/26—Organic compounds containing oxygen
- C11D7/261—Alcohols; Phenols
- C11D7/262—Alcohols; Phenols fatty or with at least 8 carbon atoms in the alkyl or alkenyl chain
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/26—Organic compounds containing oxygen
- C11D7/268—Carbohydrates or derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/32—Organic compounds containing nitrogen
- C11D7/3245—Aminoacids
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/32—Organic compounds containing nitrogen
- C11D7/329—Carbohydrate or derivatives thereof
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
Abstract
A method of antioxidant being extracted by grape pip, the antioxidant that the present invention extracts has rigid recovery rate, and high sterilizing rate, security performance is high, and the feature of environmental protection is high, and purity is high pollutes low advantage.The present invention cleans grape pip before grape pip processing, can effectively wash the grape pulp residual on grape pip, avoid the pollution of addling of grape pulp, while playing the role of disinfection decontamination, keep the subsequent extraction to grape pip purer.
Description
Technical field
The present invention relates to food processing extractive technique fields, and in particular to a kind of side that antioxidant is extracted by grape pip
Method.
Background technique
Contain polyphenols (GPS) in grape pip, mainly there is catechin and procyanidine class.These substances can be directly
The skin of the mankind is acted on, Skin Cell regeneration and metabolism can be promoted, also can increase skin elasticity, delay skin aging is put down
Shi Jingchang table grapes seed can reduce wrinkle generation, also can whitening nourishing skin.Remove the important work that free radical is grape pip
With, the phenolic substances and flavonoids object that it contains all are natural anti-institute's oxidizing components, it can effectively clear the intracorporal free radical of people,
It can protect human body inner tissue organ, can also prevent a variety of ill symptoms such as heart disease and cancer and early ageing and occur.
Summary of the invention
Technical problem to be solved by the present invention lies in overcoming existing technological deficiency to provide, a kind of method is reasonable, nutrition is rich
A kind of method that antioxidant is extracted by grape pip rich, easy to make, easy to use.
The following technical solution is employed for the technical problems to be solved by the invention to realize：
A method of antioxidant being extracted by grape pip, which is characterized in that include the following steps：
(1) grape pip is put into cleaning agent and is cleaned, and be stirred 15-30 minutes, and cleaned up with clear water；
(2) grape pip cleaned up is ground with low temperature low speed burrstone mill, collects the grape pip slurries of grinding；
(3) the grape pip slurries for collecting step 2, are added the concentration 65%-75% ethyl alcohol of 5 times of parts by weight, and stirring is equal
After even, the microwave treatment 5-10min under microwave frequency 2250MHz, power 600W stands 10-20 minutes, continues microwave treatment 5-
10min stands 10-20 minutes, continues microwave treatment 5-10min, coprocessing 3 times, obtains reaction solution；
(4) reaction solution is heated to reflux state, added to centrifuge, is centrifuged under the speed of 3000r/min
10min stands 30 minutes, takes supernatant liquor；
(5) supernatant liquor macroporous absorbent resin mixed bed is adsorbed into 5-8h, 35-45 DEG C of adsorption temp, recycles distillation
Then water washing macroporous absorbent resin desorbs 3-5h with 70% ethyl alcohol, 40-50 DEG C of desorption temperature, gained ethyl alcohol stripping liquid is passed through
It is concentrated under reduced pressure to recycle ethyl alcohol, cooled to room temperature after recycling to ethyl alcohol, residue is sent into freeze drier, dry
Micro mist is made through micronizer to get antioxidant in obtained solid.
Further, macroporous absorbent resin mixed bed big pore adsorption resin is selected from D312, XDA- in the step (5)
8, any two kinds in LSA-21, LSA-30, LS-46, XDA-6, LS-300, LS-306, D101, DM130.
Further, in the step (5) the preferred XDA-8 of macroporous absorbent resin mixed bed big pore adsorption resin and
Two kinds of DM130.
The cleaning agent is made of the raw material of following weight：Chitosan oligosaccharide -10-15 parts of polyglutamic acid, hydroxypropyl starch ether
1-5 parts, 0.5-2 parts of microcrystalline cellulose, 0.1-1 parts of D-sorbite, preparation method are：Hydroxypropyl starch ether is heated to 115-
10min is ground in 125 DEG C of heat preservations, adds microcrystalline cellulose and D-sorbite, continues to grind 15min in 115-125 DEG C of heat preservation, so
Chitosan oligosaccharide-polyglutamic acid is added afterwards, sealing and standing 3h in -10 DEG C of environment is transferred to after being sufficiently mixed, finally utilizes ultramicro grinding
Micro mist is made to get detergent in machine.
The specific preparation method of the chitosan oligosaccharide-polyglutamic acid is：It is straight that deionized water is added dropwise under grinding into chitosan oligosaccharide
To being completely dissolved, food-grade polyglutamic acid is added after standing 5min, continues that deionized water is added dropwise under milling until poly
Glutamic acid is completely dissolved, and utilizes microwave treater microwave reflow treatment 10min, continues microwave reflow treatment after standing 5min
Then sesbania gum and hydrogenated palm oil is added in 10min, microwave reflow treatment 10min again after being sufficiently mixed, gained mixture in
Moisture is ground at 70-80 DEG C to volatilize to get chitosan oligosaccharide-polyglutamic acid.
The chitosan oligosaccharide, food-grade polyglutamic acid, sesbania gum and hydrogenated palm oil mass ratio be 5-10:10-15:1-
5:0.5-2。
The beneficial effects of the invention are as follows：
(1) antioxidant that the present invention extracts has rigid recovery rate, and high sterilizing rate, security performance is high, and the feature of environmental protection is high, pure
Degree is high, pollutes low advantage；
(2) present invention cleans grape pip before grape pip processing, can effectively wash the grape on grape pip
Meat residual, avoids the pollution of addling of grape pulp, while playing the role of disinfection decontamination, keeps the subsequent extraction to grape pip purer
It is pure；
(3) present invention is using made of chitosan oligosaccharide-polyglutamic acid, hydroxypropyl starch ether, microcrystalline cellulose, D-sorbite
Cleaning agent can effectively remove remaining pulp and spot on grape pip, while safe green, easy to clean, be not easy to remain；
(4) present invention is purified using ethyl alcohol, safer compared to propyl alcohol, methanol equal solvent, is also more convenient recycling, has
Conducive to environmental protection, while microwave treatment is used, ethyl alcohol can be made to merge more evenly with solution to be extracted, dramatically speed up Polyphenols antioxygen
The leaching velocity of compound matter improves the recovery rate of Polyphenols antioxidant；
(5) present invention isolates and purifies Polyphenols antioxidant using macroporous absorbent resin mixed bed, is improving
The time required to greatly shortening purifying while gained Polyphenols antioxidant purity, the Polyphenols antioxygen in purification process is reduced
The loss amount of compound matter.
Specific embodiment
In order to be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention, below into
One step illustrates the present invention.
Embodiment 1
A method of antioxidant being extracted by grape pip, which is characterized in that include the following steps：
(1) grape pip is put into cleaning agent and is cleaned, and be stirred 15 minutes, and cleaned up with clear water；
(2) grape pip cleaned up is ground with low temperature low speed burrstone mill, collects the grape pip slurries of grinding；
(3) 65% ethyl alcohol of concentration of 5 times of parts by weight is added in the grape pip slurries for collecting step 2, after mixing evenly,
The microwave treatment 5min under microwave frequency 2250MHz, power 600W stands 10 minutes, continues microwave treatment 5min, stands 10 points
Clock continues microwave treatment 5min, coprocessing 3 times, obtains reaction solution；
(4) reaction solution is heated to reflux state, added to centrifuge, is centrifuged under the speed of 3000r/min
10min stands 30 minutes, takes supernatant liquor；
(5) supernatant liquor macroporous absorbent resin mixed bed is adsorbed into 5h, 35 DEG C of adsorption temp, recycles distillation water washing
Macroporous absorbent resin, then with 70% ethyl alcohol desorb 3h, 40-50 DEG C of desorption temperature, by gained ethyl alcohol stripping liquid through being concentrated under reduced pressure
To recycle ethyl alcohol, cooled to room temperature after recycling to ethyl alcohol, residue is sent into freeze drier, dry obtained solid
Micro mist is made to get antioxidant through micronizer.
Further, in the step (5) macroporous absorbent resin mixed bed big pore adsorption resin be XDA-8 and
Two kinds of DM130.
The cleaning agent is made of the raw material of following weight：10 parts of chitosan oligosaccharide-polyglutamic acid, 1 part of hydroxypropyl starch ether,
0.5 part of microcrystalline cellulose, 0.1 part of D-sorbite, preparation method are：Hydroxypropyl starch ether is heated to 115 DEG C of heat preservation grindings
10min adds microcrystalline cellulose and D-sorbite, continues to grind 15min in 115 DEG C of heat preservations, chitosan oligosaccharide-poly is then added
Glutamic acid is transferred to sealing and standing 3h in -10 DEG C of environment, micro mist finally is made to get clear using micronizer after being sufficiently mixed
Clean dose.
The specific preparation method of the chitosan oligosaccharide-polyglutamic acid is：It is straight that deionized water is added dropwise under grinding into chitosan oligosaccharide
To being completely dissolved, food-grade polyglutamic acid is added after standing 5min, continues that deionized water is added dropwise under milling until poly
Glutamic acid is completely dissolved, and utilizes microwave treater microwave reflow treatment 10min, continues microwave reflow treatment after standing 5min
Then sesbania gum and hydrogenated palm oil is added in 10min, microwave reflow treatment 10min again after being sufficiently mixed, gained mixture in
Moisture is ground at 70 DEG C to volatilize to get chitosan oligosaccharide-polyglutamic acid.
The chitosan oligosaccharide, food-grade polyglutamic acid, sesbania gum and hydrogenated palm oil mass ratio be 5:10:1:0.5.
Embodiment 2
A method of antioxidant being extracted by grape pip, which is characterized in that include the following steps：
(1) grape pip is put into cleaning agent and is cleaned, and be stirred 25 minutes, and cleaned up with clear water；
(2) grape pip cleaned up is ground with low temperature low speed burrstone mill, collects the grape pip slurries of grinding；
(3) 70% ethyl alcohol of concentration of 5 times of parts by weight is added in the grape pip slurries for collecting step 2, after mixing evenly,
The microwave treatment 8min under microwave frequency 2250MHz, power 600W stands 15 minutes, continues microwave treatment 8min, stands 15 points
Clock continues microwave treatment 8min, coprocessing 3 times, obtains reaction solution；
(4) reaction solution is heated to reflux state, added to centrifuge, is centrifuged under the speed of 3000r/min
10min stands 30 minutes, takes supernatant liquor；
(5) supernatant liquor macroporous absorbent resin mixed bed is adsorbed into 7h, 40 DEG C of adsorption temp, recycles distillation water washing
Then macroporous absorbent resin desorbs 4h with 70% ethyl alcohol, 45 DEG C of desorption temperature, gained ethyl alcohol stripping liquid is concentrated under reduced pressure to return
Ethyl alcohol is received, cooled to room temperature after recycling to ethyl alcohol, residue is sent into freeze drier, and dry obtained solid is through super
Micro mist is made to get antioxidant in atomizer.
Further, in the step (5) macroporous absorbent resin mixed bed big pore adsorption resin be XDA-8 and
Two kinds of DM130.
The cleaning agent is made of the raw material of following weight：13 parts of chitosan oligosaccharide-polyglutamic acid, 3 parts of hydroxypropyl starch ether,
1.2 parts of microcrystalline cellulose, 0.5 part of D-sorbite, preparation method are：Hydroxypropyl starch ether is heated to 115-125 DEG C of heat preservation
10min is ground, microcrystalline cellulose and D-sorbite are added, continues to grind 15min in 120 DEG C of heat preservations, chitosan oligosaccharide-is then added
Polyglutamic acid is transferred to sealing and standing 3h in -10 DEG C of environment, micro mist finally is made using micronizer, i.e., after being sufficiently mixed
Obtain detergent.
The specific preparation method of the chitosan oligosaccharide-polyglutamic acid is：It is straight that deionized water is added dropwise under grinding into chitosan oligosaccharide
To being completely dissolved, food-grade polyglutamic acid is added after standing 5min, continues that deionized water is added dropwise under milling until poly
Glutamic acid is completely dissolved, and utilizes microwave treater microwave reflow treatment 10min, continues microwave reflow treatment after standing 5min
Then sesbania gum and hydrogenated palm oil is added in 10min, microwave reflow treatment 10min again after being sufficiently mixed, gained mixture in
Moisture is ground at 75 DEG C to volatilize to get chitosan oligosaccharide-polyglutamic acid.
The chitosan oligosaccharide, food-grade polyglutamic acid, sesbania gum and hydrogenated palm oil mass ratio be 8:13:3:1.2.
Embodiment 3
A method of antioxidant being extracted by grape pip, which is characterized in that include the following steps：
(1) grape pip is put into cleaning agent and is cleaned, and be stirred 30 minutes, and cleaned up with clear water；
(2) grape pip cleaned up is ground with low temperature low speed burrstone mill, collects the grape pip slurries of grinding；
(3) 75% ethyl alcohol of concentration of 5 times of parts by weight is added in the grape pip slurries for collecting step 2, after mixing evenly,
The microwave treatment 10min under microwave frequency 2250MHz, power 600W stands 20 minutes, continues microwave treatment 10min, stands 20
Minute, continue microwave treatment 10min, coprocessing 3 times, obtains reaction solution；
(4) reaction solution is heated to reflux state, added to centrifuge, is centrifuged under the speed of 3000r/min
10min stands 30 minutes, takes supernatant liquor；
(5) supernatant liquor macroporous absorbent resin mixed bed is adsorbed into 8h, 45 DEG C of adsorption temp, recycles distillation water washing
Then macroporous absorbent resin desorbs 5h with 70% ethyl alcohol, 50 DEG C of desorption temperature, gained ethyl alcohol stripping liquid is concentrated under reduced pressure to return
Ethyl alcohol is received, cooled to room temperature after recycling to ethyl alcohol, residue is sent into freeze drier, and dry obtained solid is through super
Micro mist is made to get antioxidant in atomizer.
Further, in the step (5) macroporous absorbent resin mixed bed big pore adsorption resin be XDA-8 and
Two kinds of DM130.
The cleaning agent is made of the raw material of following weight：15 parts of chitosan oligosaccharide-polyglutamic acid, 5 parts of hydroxypropyl starch ether,
2 parts of microcrystalline cellulose, 1 part of D-sorbite, preparation method are：Hydroxypropyl starch ether is heated to 125 DEG C of heat preservation grindings
10min adds microcrystalline cellulose and D-sorbite, continues to grind 15min in 125 DEG C of heat preservations, chitosan oligosaccharide-poly is then added
Glutamic acid is transferred to sealing and standing 3h in -10 DEG C of environment, micro mist finally is made to get clear using micronizer after being sufficiently mixed
Clean dose.
The specific preparation method of the chitosan oligosaccharide-polyglutamic acid is：It is straight that deionized water is added dropwise under grinding into chitosan oligosaccharide
To being completely dissolved, food-grade polyglutamic acid is added after standing 5min, continues that deionized water is added dropwise under milling until poly
Glutamic acid is completely dissolved, and utilizes microwave treater microwave reflow treatment 10min, continues microwave reflow treatment after standing 5min
Then sesbania gum and hydrogenated palm oil is added in 10min, microwave reflow treatment 10min again after being sufficiently mixed, gained mixture in
Moisture is ground at 80 DEG C to volatilize to get chitosan oligosaccharide-polyglutamic acid.
The chitosan oligosaccharide, food-grade polyglutamic acid, sesbania gum and hydrogenated palm oil mass ratio be 10:15:5:2.
Control group 1
This control group content and 2 content of embodiment are essentially identical, and something in common no longer repeats, the difference is that：Step 1
Middle grape pip cleaning is cleaned with common dish washing liquid.
Control group 2
This control group content and 2 content of embodiment are essentially identical, and something in common no longer repeats, the difference is that：Step 3
In only with 70% ethyl alcohol purification of concentration, without using microwave treatment.
Control group 3
This control group content and 2 content of embodiment are essentially identical, and something in common no longer repeats, the difference is that：Step 2
In do not use low temperature low speed burrstone mill grind.
The extraction effect of the extracting method of the present invention of table 1
The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (6)
1. a kind of method for extracting antioxidant by grape pip, which is characterized in that include the following steps：
(1) grape pip is put into cleaning agent and is cleaned, and be stirred 15-30 minutes, and cleaned up with clear water；
(2) grape pip cleaned up is ground with low temperature low speed burrstone mill, collects the grape pip slurries of grinding；
(3) the concentration 65%-75% ethyl alcohol of 5 times of parts by weight is added in the grape pip slurries for collecting step 2, after mixing evenly,
The microwave treatment 5-10min under microwave frequency 2250MHz, power 600W stands 10-20 minutes, continues microwave treatment 5-
10min stands 10-20 minutes, continues microwave treatment 5-10min, coprocessing 3 times, obtains reaction solution；
(4) reaction solution is heated to reflux state, added to centrifuge, 10min is centrifuged under the speed of 3000r/min, it is quiet
It sets 30 minutes, takes supernatant liquor；
(5) supernatant liquor macroporous absorbent resin mixed bed is adsorbed into 5-8h, 35-45 DEG C of adsorption temp, recycles distillation washing
Wash macroporous absorbent resin, then with 70% ethyl alcohol desorb 3-5h, 40-50 DEG C of desorption temperature, by gained ethyl alcohol stripping liquid through depressurizing
To recycle ethyl alcohol, cooled to room temperature after recycling to ethyl alcohol, residue is sent into freeze drier for concentration, dry gained
Micro mist is made through micronizer to get antioxidant in solid.
2. the method according to claim 1 for extracting antioxidant by grape pip, it is characterised in that：The step (5)
Middle macroporous absorbent resin mixed bed big pore adsorption resin be selected from D312, XDA-8, LSA-21, LSA-30, LS-46, XDA-6,
Any two kinds in LS-300, LS-306, D101, DM130.
3. the method according to claim 2 for extracting antioxidant by grape pip, it is characterised in that：The step (5)
The preferred XDA-8 of middle macroporous absorbent resin mixed bed big pore adsorption resin and two kinds of DM130.
4. the method according to claim 1 for extracting antioxidant by grape pip, it is characterised in that：The cleaning agent by
The raw material of following weight is made：Chitosan oligosaccharide -10-15 parts of polyglutamic acid, 1-5 parts of hydroxypropyl starch ether, microcrystalline cellulose 0.5-2
Part, 0.1-1 parts of D-sorbite, preparation method are：Hydroxypropyl starch ether is heated to 115-125 DEG C of heat preservation grinding 10min, then
Microcrystalline cellulose and D-sorbite is added, continues to grind 15min in 115-125 DEG C of heat preservation, the more polyglutamics of chitosan oligosaccharide-is then added
Acid is transferred to sealing and standing 3h in -10 DEG C of environment, micro mist finally is made to get detergent using micronizer after being sufficiently mixed.
5. the method according to claim 4 for extracting antioxidant by grape pip, it is characterised in that：The chitosan oligosaccharide-
The specific preparation method of polyglutamic acid is：Deionized water is added dropwise into chitosan oligosaccharide until being completely dissolved under grinding, stands 5min
After add food-grade polyglutamic acid, continue that deionized water is added dropwise under milling until polyglutamic acid is completely dissolved, and benefit
With microwave treater microwave reflow treatment 10min, continues microwave reflow treatment 10min after standing 5min, sesbania gum is then added
And hydrogenated palm oil, microwave reflow treatment 10min, gained mixture are ground to moisture at 70-80 DEG C again after being sufficiently mixed
It volatilizes to get chitosan oligosaccharide-polyglutamic acid.
6. the method according to claim 5 for extracting antioxidant by grape pip, it is characterised in that：The chitosan oligosaccharide,
The mass ratio of food-grade polyglutamic acid, sesbania gum and hydrogenated palm oil is 5-10:10-15:1-5:0.5-2.
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| CN109497037A (en) * | 2018-12-03 | 2019-03-22 | 蚌埠市秀之舞文化传媒有限公司 | A kind of antiseptic treating agent for ox horn |
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| CN109497037A (en) * | 2018-12-03 | 2019-03-22 | 蚌埠市秀之舞文化传媒有限公司 | A kind of antiseptic treating agent for ox horn |
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