CN107400557A - A kind of method for extracting grape-kernel oil - Google Patents
A kind of method for extracting grape-kernel oil Download PDFInfo
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- CN107400557A CN107400557A CN201710667284.3A CN201710667284A CN107400557A CN 107400557 A CN107400557 A CN 107400557A CN 201710667284 A CN201710667284 A CN 201710667284A CN 107400557 A CN107400557 A CN 107400557A
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- grape
- oil
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- enzymolysis
- kernel oil
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/02—Pretreatment
- C11B1/04—Pretreatment of vegetable raw material
Abstract
The invention belongs to plant oil extract field, discloses a kind of method for extracting grape-kernel oil, and the grape pip of crushing is acted on using biology enzyme, first use cellulase degradation, digested with alkali protease, grease can be separated after centrifugation again, reach the purpose of extraction grape-kernel oil.Compared with the technique of existing squeezing extraction, simple to operate, oil extracting rate is high, and processing safety height, mild condition, the nutritional ingredient that will not be destroyed in grease, can obtain the grape-kernel oil of the rich in nutrition content such as unrighted acid, linoleic acid, polyphenol.
Description
Technical field
The invention belongs to plant oil extract field, and in particular to a kind of method for extracting grape-kernel oil, it is especially a kind of to answer
With the method for Enzymatic Extraction Oil for Grape Seed Oil.
Background technology
Grape is one of cultivated area and the most fruit of yield in the world, and grape pip is the seed of grape, and grape pip is
The leftover bits and pieces of grape wine factory, products therefrom after Grape Skin, grape pedicel is separated after drying.Grape pip typically accounts for grape gross weight
3%~7%, as the accessory substance of wine industry, it is a kind of high-quality edible oil and fat resource.Grape pip oil content is 9%-
14%, contain abundant unrighted acid, mainly oleic acid and linoleic acid.Grape-kernel oil belongs to high linoleic acid type grease.Its
The content of Linoleic acid is up to 72%~76%.The grape-kernel oil Linoleic acid ratio of most kinds reaches total fatty acids
More than 70%, some even as high as 81% is extremely rare less than 60% kind.Linoleic acid is essential fatty acid, is easy to
It is absorbed by the body, long-term consumption grape-kernel oil can reduce human serum cholesterol, effectively adjust the vegetative nerve function of people.Grape
Seed oil is rich in vitamin E, has stronger inoxidizability, can effectively extend the shelf shelf-life, be not easy to cause due to illumination,
Heat radiation and with air contact and caused oxidative rancidity phenomenon.Because self performance is more stable, except straight as cooking oil
It is connected on dining table and eats and for making outside various food, grape-kernel oil still makes the important original of superior cosmetics and medicine
One of material.Proanthocyanidin in grape-kernel oil has protection blood vessel elasticity, protects skin afflicting with great suffering torment from ultraviolet, prevention collagen fibre
The destruction of peacekeeping elastomer, skin is kept due elasticity and tension force, avoid skin sagging and wrinkle from producing.Grape-kernel oil
In also containing mineral matter and the various fat-soluble and water soluble vitamin such as potassium needed by human, sodium, calcium, be suitable for making old man
And baby nutritive food, dietetic food and work high above the ground personnel's special food.
Existing grease processing technique has：Two kinds of techniques of squeezing and leaching, but both techniques are oily for main purpose to carry,
The condition that it is processed is very violent.And in extraction method and its supporting refining process, there is potential potential safety hazard,
And the decomposition of unrighted acid in grape-kernel oil, linoleic oxidation and the destruction of Polyphenols nutritional ingredient can be caused, with
And resource reutilization rate is relatively low and the distinct issues such as some environmental pollutions.And grape pip oil content is only 9%-14%, category
In low oil-containing crop, grease is difficult to separate.
The content of the invention
In view of this, in view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a kind of oil extracting rate higher extraction
The method of grape-kernel oil, and extract the rich in nutrition content such as obtained grape-kernel oil unrighted acid, linoleic acid, polyphenol.
The purpose of the present invention is achieved through the following technical solutions：
A kind of method for extracting grape-kernel oil, comprises the following steps：
(1) extrusion is carried out after grape pip is crushed, expanded product pulverizes and sieves；
(2) the expanded product after crushing is mixed with water, obtains mixed liquor；
(3) mixed liquor adds cellulase and carries out the first enzymolysis, obtains enzymolysis liquid I；
(4) enzymolysis liquid I adds protex-6L alkali proteases and carries out the second enzymolysis, obtains enzymolysis liquid II；
(5) pH value of enzymolysis liquid II is adjusted to after 4.5, continuing to stir 30min；
(6) free oil, emulsion, hydrolyzate and residue are centrifugally separating to obtain after enzyme deactivation；
(7) emulsion is carried out into demulsification to handle to obtain free oil, merges and collect all free oils.
The method of extraction grape-kernel oil of the present invention acts on the grape pip of crushing using biology enzyme, first uses cellulase
Enzymolysis, then is digested with alkali protease, makes grease be easier to discharge from grape pip, at the same using non-oil component to oil and
The difference and profit proportion of water affinity are different and are separated oily with non-oil component, mild condition, safe.
Wherein, it is that extrusion temperature is 130 DEG C as the extrusion expansion parameter described in preferred steps (1), screw speed is
120r/min, pitch-row 16mm, material moisture 13%.
Further, the mass ratio of the expanded product and water described in step (2) is 1:4-1:8.In some embodiments,
The mass ratio of expanded product and water described in step (2) is 1:6.
Further, the temperature of the first enzymolysis described in step (3) is 40~50 DEG C, and the time is 1.5~2h, pH 7.2-
8.6, the addition of cellulase is 2.5~3.5%.In some embodiments, the temperature of the first enzymolysis described in step (3)
For 45 DEG C, time 2h, pH 8.0, the addition of cellulase is 2.5%.
Further, the temperature of the second enzymolysis described in step (4) is 50~60 DEG C, and the time is 1.5~2h, pH 9.0-
The addition of 9.3, protex-6L alkali proteases is 2.5~3.5%.In some embodiments, described in step (4)
The temperature of two enzymolysis is 55 DEG C, time 1.5h, pH 9.0, and the addition of protex-6L alkali proteases is 3.0%.
Further, step (6) described enzyme deactivation handles 5min to be heated to 100 DEG C.
Further, step (6) centrifugation centrifuges 30min for 8000r/min.
Further, the demulsification processing described in step (7) is demulsified for freeze-thaw demulsification, high steam or pH adjusts demulsification
In one kind.In some embodiments, step (7) the demulsification processing is demulsified for freeze-thaw.
As shown from the above technical solution, the invention provides a kind of method for extracting grape-kernel oil, using biological enzyme effect
In the grape pip of crushing, first with cellulase degradation, then digested with alkali protease, grease can be separated after centrifugation,
Reach the purpose of extraction grape-kernel oil.Compared with the technique of existing squeezing extraction, simple to operate, oil extracting rate is high, and operates peace
Quan Xinggao, mild condition, the nutritional ingredient that will not be destroyed in grease, the battalion such as unrighted acid, linoleic acid, polyphenol can be obtained
Form a point abundant grape-kernel oil.
Embodiment
The invention discloses a kind of method for extracting grape-kernel oil.Those skilled in the art can use for reference present disclosure, fit
When modified technique parameter is realized.In particular, all similar replacements and change for a person skilled in the art
It is it will be apparent that they are considered as being included in the present invention.The method of the present invention is retouched by preferred embodiment
State, related personnel can substantially not depart from present invention, method described herein is being modified or fitted in spirit and scope
When change is with combining, to realize and using the technology of the present invention.
For a further understanding of the present invention, below in conjunction with the embodiment of the present invention, to the technical side in the embodiment of the present invention
Case is clearly and completely described, it is clear that and described embodiment is only part of the embodiment of the present invention, rather than all
Embodiment.Based on the embodiment in the present invention, those of ordinary skill in the art institute under the premise of creative work is not made
The every other embodiment obtained, belongs to the scope of protection of the invention.
Unless otherwise specified, reagent involved in the embodiment of the present invention is commercially available prod, can pass through business canal
Road purchase obtains.
Embodiment 1：
Grape pip crush after 130 DEG C, screw speed 120r/min, pitch-row 16mm, material moisture be 13% bar
Extrusion is carried out under part, expanded product crushed 60 mesh sieves, with 1:6 solid-liquid ratio mixes with water, 45 DEG C of water-baths, regulation pH to
7.2, add 3.0% cellulase degradation 2h, adjust the temperature to 55 DEG C of water-baths, pH to 9.0, add 3.0% protex-6L
Alkali protease digests 2h, and regulation pH value is to continuing after 4.5 to stir 30min, under conditions of boiling enzyme deactivation 5min, 8000r/min
30min is centrifuged, obtains free oil, emulsion, hydrolyzate and residue, emulsion freeze-thaw is demulsified to obtain free oil, merges and collects
All free oils produce grape-kernel oil.The oil content of grape pip is determined as 14g/100g, the trip of extraction by soxhlet extraction methods
It is about 9.4g from oil content, the oil content of the extraction after emulsion breakdown is about 2.5g, and oil extracting rate is calculated as follows：
Shown according to checkout result, oil extracting rate is up to 85%.The grape-kernel oil of extraction detects according to GB/T22478-2008,
Wherein palmitic acid content is 7.5g/100g, stearic acid content 3.9g/100g, oleic acid content 21.3g/100g, and linoleic acid contains
It is 20.5 μ g/ml to measure as 68.2g/100g, linolenic acid content 0.2g/100g, procyanidin content, and chlorophyll content is
0.94mg/kg, carotenoid content 0.83mg/kg, campesterol content are 12.92mg/100g, and stigmasterol content is
3.91mg/100g, cupreol content are 142.49mg/100g, illustrate bioactivity in the grape-kernel oil through aqueous enzymatic extraction
Content of material enriches, great nutritive value.
Embodiment 2：
Grape pip crush after 130 DEG C, screw speed 120r/min, pitch-row 16mm, material moisture be 13% bar
Extrusion is carried out under part, expanded product crushed 60 mesh sieves, with 1:6 solid-liquid ratio mixes with water, 45 DEG C of water-baths, regulation pH to
7.2, add 3.5% cellulase degradation 2h, adjust the temperature to 55 DEG C of water-baths, pH to 9.0, add 2.5% protex-6L
Alkali protease digests 2h, and regulation pH value is to continuing after 4.5 to stir 30min, under conditions of boiling enzyme deactivation 5min, 8000r/min
30min is centrifuged, obtains free oil, emulsion, hydrolyzate and residue, emulsion freeze-thaw is demulsified to obtain free oil, merges and collects
All free oils produce grape-kernel oil.The oil content of grape pip is determined as 14g/100g, the trip of extraction by soxhlet extraction methods
It is about 9.1g from oil content, the oil content of the extraction after emulsion breakdown is about 2.5g, and oil extracting rate is calculated as follows：
Shown according to checkout result, oil extracting rate is up to 82.9%.The grape-kernel oil of extraction is examined according to GB/T22478-2008
Survey, wherein palmitic acid content is 7.0g/100g, stearic acid content 3.3g/100g, oleic acid content 20.3g/100g, and Asia is oily
Acid content is 65.2g/100g, and linolenic acid content 0.2g/100g, procyanidin content is 19.5 μ g/ml, and chlorophyll content is
0.87mg/kg, carotenoid content 0.78mg/kg, campesterol content are 12.01mg/100g, and stigmasterol content is
3.91mg/100g, cupreol content are 130.12mg/100g, illustrate bioactivity in the grape-kernel oil through aqueous enzymatic extraction
Content of material enriches, great nutritive value.
Embodiment 3：
Grape pip crush after 130 DEG C, screw speed 120r/min, pitch-row 16mm, material moisture be 13% bar
Extrusion is carried out under part, expanded product crushed 80 mesh sieves, with 1:6 solid-liquid ratio mixes with water, 45 DEG C of water-baths, regulation pH to
7.2, add 3.5% cellulase degradation 2h, adjust the temperature to 55 DEG C of water-baths, pH to 9.0, add 2.5% protex-6L
Alkali protease digests 2h, and regulation pH value is to continuing after 4.5 to stir 30min, under conditions of boiling enzyme deactivation 5min, 8000r/min
30min is centrifuged, obtains free oil, emulsion, hydrolyzate and residue, emulsion freeze-thaw is demulsified to obtain free oil, merges and collects
All free oils produce grape-kernel oil.The oil content of grape pip is determined as 14g/100g, the trip of extraction by soxhlet extraction methods
It is about 9.0g from oil content, the oil content of the extraction after emulsion breakdown is about 2.3g, and oil extracting rate is calculated as follows：
Shown according to checkout result, oil extracting rate is up to 80.7%.The grape-kernel oil of extraction is examined according to GB/T22478-2008
Survey, wherein palmitic acid content is 6.8g/100g, stearic acid content 3.2g/100g, oleic acid content 18.9g/100g, and Asia is oily
Acid content is 67.6g/100g, linolenic acid content 0.17g/100g, and procyanidin content is 19.1 μ g/ml, chlorophyll content
For 0.85mg/kg, carotenoid content 0.80mg/kg, campesterol content is 12.09mg/100g, and stigmasterol content is
3.75mg/100g, cupreol content are 140.08mg/100g, illustrate bioactivity in the grape-kernel oil through aqueous enzymatic extraction
Content of material enriches, great nutritive value.
Embodiment 4：
Grape pip crush after 130 DEG C, screw speed 120r/min, pitch-row 16mm, material moisture be 13% bar
Extrusion is carried out under part, expanded product crushed 60 mesh sieves, with 1:6 solid-liquid ratio mixes with water, 45 DEG C of water-baths, regulation pH to
7.2, add 3.5% cellulase degradation 2h, adjust the temperature to 55 DEG C of water-baths, pH to 9.0, add 2.5% protex-6L
Alkali protease digests 3h, and regulation pH value is to continuing after 4.5 to stir 30min, under conditions of boiling enzyme deactivation 5min, 8000r/min
30min is centrifuged, obtains free oil, emulsion, hydrolyzate and residue, emulsion freeze-thaw is demulsified to obtain free oil, merges and collects
All free oils produce grape-kernel oil.The oil content of grape pip is determined as 14g/100g, the trip of extraction by soxhlet extraction methods
It is about 9.0g from oil content, the oil content of the extraction after emulsion breakdown is about 2.8g, and oil extracting rate is calculated as follows：
Shown according to checkout result, oil extracting rate is up to 84.3%.The grape-kernel oil of extraction is examined according to GB/T22478-2008
Survey, wherein palmitic acid content is 7.9g/100g, stearic acid content 4.0g/100g, oleic acid content 21.3g/100g, and Asia is oily
Acid content is 68.2g/100g, and linolenic acid content 0.2g/100g, procyanidin content is 20.5 μ g/ml, and chlorophyll content is
0.94mg/kg, carotenoid content 0.83mg/kg, campesterol content are 12.01mg/100g, and stigmasterol content is
3.91mg/100g, cupreol content are 140.51mg/100g, illustrate bioactivity in the grape-kernel oil through aqueous enzymatic extraction
Content of material enriches, great nutritive value.
Comparative example 1
Grape pip crosses 60 mesh sieves after crushing, with 1:6 solid-liquid ratio mixes with water, 45 DEG C of water-baths, adjusts pH to 7.2, adds
3.5% cellulase degradation 2h, adjusts the temperature to 55 DEG C of water-baths, pH to 9.0, adds 2.5% protex-6L basic proteins
Enzyme digests 3h, and regulation pH value is boiled and centrifuged under conditions of enzyme deactivation 5min, 8000r/min to continuing after 4.5 to stir 30min
30min, obtains free oil, emulsion, hydrolyzate and residue, and emulsion freeze-thaw is demulsified to obtain free oil, merge collect it is all
Free oil produce grape-kernel oil.The oil content of grape pip is determined as 14g/100g, the free oil of extraction by soxhlet extraction methods
Content is about 7.9g, and the oil content of the extraction after emulsion breakdown is about 1.2g, and oil extracting rate is calculated as follows：
Shown according to checkout result, oil extracting rate is up to 65%.The grape-kernel oil of extraction detects according to GB/T22478-2008,
Wherein palmitic acid content is 5.5g/100g, stearic acid content 2.1g/100g, oleic acid content 15.7g/100g, and linoleic acid contains
It is 16.5 μ g/ml to measure as 57.2g/100g, linolenic acid content 0.11g/100g, procyanidin content, and chlorophyll content is
0.67mg/kg, carotenoid content 0.56mg/kg, campesterol content are 9.14mg/100g, and stigmasterol content is
2.17mg/100g, cupreol content are 113.12mg/100g.This technique extract grape-kernel oil bioactive substance content compared with
Linoleic acid content low, that linoleic acid content requires in being formed already below national standard GB/T22478-2008 aliphatic acid.
Comparative example 2
Grape pip crush after 130 DEG C, screw speed 120r/min, pitch-row 16mm, material moisture be 13% bar
Extrusion is carried out under part, expanded product crushed 60 mesh sieves, with 1:6 solid-liquid ratio mixes with water, 37 DEG C of water-baths, regulation pH to
5.0, add 3.0% complex enzyme (cellulase and hemicellulase 1:1 ratio) enzymolysis 1h, 55 DEG C of water-baths are adjusted the temperature to,
PH to 7.5,4.0% As1398 neutral protease enzymolysis 2h are added, continue to stir 30min after regulation pH value to 4.0, boil and go out
Enzyme 5min,
30min is centrifuged under conditions of 8000r/min, obtains free oil, emulsion, hydrolyzate and residue, emulsion freezing
Defrosting is demulsified to obtain free oil, merges and collects all free oils and produce grape-kernel oil.The oil content of grape pip passes through soxhlet type
Method is determined as 14g/100g, and the free oil content of extraction is about 7.4g, and the oil content of the extraction after emulsion breakdown is about 1.1g,
Oil extracting rate is calculated as follows：
Shown according to checkout result, oil extracting rate is up to 60.7%.The grape-kernel oil of extraction is examined according to GB/T22478-2008
Survey, wherein palmitic acid content is 5.1g/100g, stearic acid content 2.9g/100g, oleic acid content 11.3g/100g, and Asia is oily
Acid content is 55.2g/100g, linolenic acid content 0.09g/100g, and procyanidin content is 10.5 μ g/ml, chlorophyll content
For 0.54mg/kg, carotenoid content 0.51mg/kg, campesterol content is 9.94mg/100g, and stigmasterol content is
2.65mg/100g, cupreol content are 108.21mg/100g.The grape-kernel oil content items bioactivity of this technique extraction
Content is relatively low, and aliphatic acid forms the requirement for being unable to reach GB/T22478-2008.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (9)
- A kind of 1. method for extracting grape-kernel oil, it is characterised in that comprise the following steps：(1) extrusion is carried out after grape pip is crushed, expanded product pulverizes and sieves；(2) the expanded product after crushing is mixed with water, obtains mixed liquor；(3) mixed liquor adds cellulase and carries out the first enzymolysis, obtains enzymolysis liquid I；(4) enzymolysis liquid I adds protex-6L alkali proteases and carries out the second enzymolysis, obtains enzymolysis liquid II；(5) pH value of enzymolysis liquid II is adjusted to after 4.5, continuing to stir 30min；(6) free oil, emulsion, hydrolyzate and residue are centrifugally separating to obtain after enzyme deactivation；(7) emulsion is carried out into demulsification to handle to obtain free oil, merges and collect all free oils.
- 2. according to the method for claim 1, it is characterised in that the extrusion expansion parameter described in step (1) is extrusion temperature For 130 DEG C, screw speed 120r/min, pitch-row 16mm, material moisture 13%.
- 3. according to the method for claim 1, it is characterised in that step (1) sieving was 60~100 mesh sieves.
- 4. according to the method for claim 1, it is characterised in that the mass ratio of expanded product and water described in step (2) is 1:4-1:8。
- 5. according to the method for claim 1, it is characterised in that the temperature of the first enzymolysis described in step (3) is 40~50 DEG C, the time is 1.5~2h, pH 7.2-8.6, and the addition of cellulase is calculated as 2.5~3.5% by g/ml.
- 6. according to the method for claim 1, it is characterised in that the temperature of the second enzymolysis described in step (4) is 50~60 DEG C, the time is 1.5~2h, and the addition of pH 9.0-9.3, protex-6L alkali proteases is calculated as 2.5~3.5% by g/ml.
- 7. according to the method for claim 1, it is characterised in that step (6) described enzyme deactivation is handled to be heated to 100 DEG C 5min。
- 8. according to the method for claim 1, it is characterised in that step (6) centrifugation centrifuges 30min for 8000r/min.
- 9. according to the method for claim 1, it is characterised in that demulsification described in step (7) processing is freeze-thaw demulsification, One kind during high steam is demulsified or pH regulations are demulsified.
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Cited By (4)
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| CN108285827A (en) * | 2018-04-10 | 2018-07-17 | 无限极（中国）有限公司 | A kind of grape seed oil and preparation method thereof |
| CN109467545A (en) * | 2018-09-26 | 2019-03-15 | 春归保健科技有限公司 | A method of extracting procyanidine from Rosa roxburghii Tratt skin |
| CN113046170A (en) * | 2021-03-26 | 2021-06-29 | 大连奥川生物科技有限公司 | Preparation method and application of avocado oil rich in furan lipid unsaponifiable matter |
| CN113416599A (en) * | 2021-06-29 | 2021-09-21 | 广西壮族自治区亚热带作物研究所（广西亚热带农产品加工研究所） | Passion fruit seed oil and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108285827A (en) * | 2018-04-10 | 2018-07-17 | 无限极（中国）有限公司 | A kind of grape seed oil and preparation method thereof |
| CN108285827B (en) * | 2018-04-10 | 2021-10-08 | 无限极（中国）有限公司 | Grape seed oil and preparation method thereof |
| CN109467545A (en) * | 2018-09-26 | 2019-03-15 | 春归保健科技有限公司 | A method of extracting procyanidine from Rosa roxburghii Tratt skin |
| CN109467545B (en) * | 2018-09-26 | 2022-05-20 | 春归保健科技有限公司 | Method for extracting procyanidine from roxburgh rose peel |
| CN113046170A (en) * | 2021-03-26 | 2021-06-29 | 大连奥川生物科技有限公司 | Preparation method and application of avocado oil rich in furan lipid unsaponifiable matter |
| CN113046170B (en) * | 2021-03-26 | 2022-03-11 | 大连奥川生物科技有限公司 | Preparation method and application of avocado oil rich in furan lipid unsaponifiable matter |
| CN113416599A (en) * | 2021-06-29 | 2021-09-21 | 广西壮族自治区亚热带作物研究所（广西亚热带农产品加工研究所） | Passion fruit seed oil and preparation method thereof |
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