CN108285827A - A kind of grape seed oil and preparation method thereof - Google Patents
A kind of grape seed oil and preparation method thereof Download PDFInfo
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- CN108285827A CN108285827A CN201810315870.6A CN201810315870A CN108285827A CN 108285827 A CN108285827 A CN 108285827A CN 201810315870 A CN201810315870 A CN 201810315870A CN 108285827 A CN108285827 A CN 108285827A
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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
- C11B1/02—Pretreatment
- C11B1/04—Pretreatment of vegetable raw material
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
- A23D9/00—Other edible oils or fats, e.g. shortenings, cooking oils
- A23D9/007—Other edible oils or fats, e.g. shortenings, cooking oils characterised by ingredients other than fatty acid triglycerides
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
- A23D9/00—Other edible oils or fats, e.g. shortenings, cooking oils
- A23D9/02—Other edible oils or fats, e.g. shortenings, cooking oils characterised by the production or working-up
- A23D9/04—Working-up
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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
- C11B1/02—Pretreatment
- C11B1/025—Pretreatment by enzymes or microorganisms, living or dead
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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
- C11B3/00—Refining fats or fatty oils
- C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
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- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
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- C11B3/00—Refining fats or fatty oils
- C11B3/02—Refining fats or fatty oils by chemical reaction
- C11B3/06—Refining fats or fatty oils by chemical reaction with bases
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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
- C11B3/00—Refining fats or fatty oils
- C11B3/16—Refining fats or fatty oils by mechanical means
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Abstract
The invention belongs to food processing field, a kind of grape seed oil and preparation method thereof is disclosed.The present invention extracts grape seed oil using composite plant hydrolase and acid protease fractional hydrolysis method, greatly remains the content of the active constituent especially polyphenol in grape seed oil, while taking into account grape seed oil recovery rate.Compared to squeezing or preparation grape seed oil is leached, the present invention greatly remains the active constituent in grape seed oil, and grape seed oil clear obtained can be used as high-end oil for health care.Preparation method of the present invention, the used time is short, can effectively destroy the cell wall of grape pip benevolence cell so that the grease in cell is more easy to extract, and effectively improves the recovery rate of grape seed oil.It is demulsified by using alkaline extraction, avoids dissolvent residual, while can effectively reduce acid value 0.168 (KOH)/(mg/g) of grape pip crude oil, be not necessarily to later stage alkali refining process.This method is easy to operate, at low cost, is suitable for industrialized production.
Description
Technical field
The invention belongs to food processing fields, and in particular to a kind of grape seed oil and preparation method thereof, especially a kind of work
The property high grape seed oil and preparation method thereof of ingredient especially polyphenol content.
Background technology
With the continuous improvement of society and living standards, the eating habit of people is also changed, and is eaten and drunk immoderately and is caused very
More people are suffering from " three high diseases ", i.e. hyperglycemia, hypertension and hyperlipidemia.Wherein, hyperglycemic patients are most commonly seen, need to strictly control
Diet, low sugar less salt, severe patient also need to take hypoglycemic agent.This is but also many hyperglycemic patients all select less in terms of diet
It drains the oil or even does not drain the oil.
Grape seed oil is the advanced food by making grape wine or the further processing of the by-product grape pip of juice extracting obtains
With oil.Grape seed oil is full of nutrition, and unsaturated fatty acid is up to 90% or more, predominantly linoleic acid (70% or more), oleic acid, palm fibre
Palmitic acid acid and stearic acid.Linoleic acid is essential aliphatic acid for human body, is one of the important composition for constituting human cell membrane and skin, can tie up
The blood fat balance of adult is held, cholesterol is reduced, improves angiocardiopathy.Also contain phenolic compound in grape seed oil, does not have such as
Gallate-based, catechin, epicatechin, procyanidine etc., research in recent years have reported these phenolic compounds with extensive
Bioactivity：Anti-oxidant, anticancer, radicals scavenging effect, anti-inflammatory, antiviral, hypoglycemic and other effects.In addition, grape pip
Also contain in oil phytosterol, squalene, a variety of liposoluble vitamins (A, E, D, K, P) and various trace elements (Ca, Fe, Zn,
Mn、Cu)。
Horse tinkling of pieces of jade etc. studies the antioxidation of mice organs grape seed oil, measures mouse tissue lipid peroxidation
Matter content, paddy Guang peptide peroxidase and superoxide dismutase activity.The result shows that grape seed oil experimental group small white mouse
Liver, kidney device glutathione peroxidase, superoxidase activity be higher than control group, the content of the malonaldehyde of each internal organs is bright
It is aobvious to be less than control group, it was demonstrated that grape seed oil has certain antioxidation.Lutterodt et al. has studied cold press Chardonnay, horse
Si Kadan, the free radical scavenging ability of ruby and Kang Kede grape seed oils indicate seed oil to DPPH freedom with Trolox equivalents
The removing power of base, the results showed that the DPPH free radical scavenging activities range of seed oil is from 0.07 to 2.22mmol/g.Grape seed oil nutrition
Value and medical function obtain domestic and international medical field and the abundant affirmation of nutritionist.
Currently, grape seed oil on the market mostly uses cold press and solvent extraction technology.Squeezing method oil yield is not high, solvent leaching
Going out method, there are problem of solvent residual.Aqueous enzymatic method is a kind of environment-friendly type grease extractive technique, by crushing and digesting come degrading plant
Cell wall discharges the grease in oil plant cell.Aqueous enzymatic method has the following advantages with respect to traditional handicraft：High temperature is avoided to live material
The influence of property ingredient, free oil yield is higher, lighter color, and protein denaturation degree is small, and is conducive to environmental protection and grease work
The sustainable development of industry.In recent years, lot of documents constantly carries out process optimization for aqueous enzymatic method grape seed oil recovery rate is improved.Lee
Dan Dan (2017) digests 9h using complex enzyme (cellulase, pectase, zytase, trypsase), and freeze-thaw method demulsification is fuel-displaced
Rate is 9.947%, acid value 0.52 (KOH)/(mg/g).High fine jade etc. (2009) is using enzymolysis and organic solvent extraction gained grape
Seed oil extract rate reaches 88.9%, acid value 0.43 (KOH)/(mg/g)；Hu Bin etc. (2015) first uses cellulase degradation 2h, after
Using neutral protease enzymolysis 1.5h, grape seed oil recovery rate is 77.48%；Ultrasound pretreatment 15min on this basis, extraction
Rate is up to 87.65%；Microwave demulsifying is then used, recovery rate is up to 93.83%, acid value 2.16 (KOH)/(mg/g).Lv Shanshan is adopted
With steam pre-treatment knot and cellulase/protease hydrolytic 8h, oil yield 13.26%, acid value 1.24 (KOH)/(mg/g).
But the study of active components for relating to the obtained grape seed oil of enzymolysis process is relatively fewer, and the phenol in grape seed oil
Substance is its main antioxidant, is easiest to that oxidation, degradation occurs in enzymolysis process.Therefore, urgent need is a kind of to carry
Active constituent especially polyphenol content in high grape seed oil, while taking into account the preparation side of the grape seed oil of grape seed oil recovery rate
Method.
Invention content
In view of this, the purpose of the present invention is in view of the drawbacks of the prior art, a kind of active constituent especially polyphenol is provided
The high grape seed oil and preparation method thereof of content.
It is an object of the present invention to provide a kind of grape seed oil, total phenol contents >=30mg/kg.
Further, its unsaturated fatty acid >=86.63% of the grape seed oil, total tocopherol >=253.6mg/kg, total
Sterol >=2.588mg/g, acid value are 0.168 (KOH)/(mg/g).
Another object of the present invention provides a kind of method preparing grape seed oil, includes the following steps：
(1) grape pip crushes, and sieving obtains grape pip powder；
(2) grape pip powder that step (1) obtains adds water mixing that slurries are made, and mixed enzyme, warp is added in adjusting slurry pH to acidity
The first mixed liquor is obtained after enzyme digestion reaction；
(3) pH of the first mixed liquor of step (2) is adjusted to acidity, acid protease is added and digests to obtain acid hydrolysis solution；
(4) lye pH adjustment is added to alkalinity in the acid hydrolysis solution of step (3), the second mixed liquor is obtained by the reaction；
(5) it to the second mixed liquor enzyme deactivation of step (4), centrifuges, takes upper layer free oil, obtain grape seed oil.
Step (1) of the present invention first pre-processes grape pip to obtain grape pip powder, and the pretreatment has for crushing, mistake
Sieve.
In some embodiments, the sieving in the step (1) was 20-60 mesh sieve.
In some embodiments of the present invention, grape pip powder its moisture and volatile matter content content in the step (1) is
7.0%-9.0%, oil content 14-20%, crude protein content 8-10%, fiber content 26-30%.
Step (2) of the present invention carries out mixed enzyme enzymolysis to grape pip powder.Grape pip powder adds water to be mixed to prepare slurries first, adjusts
Mixed enzyme is added to acidity in slurries pH, carries out mixed enzyme enzymolysis, the first mixed liquor is obtained after enzyme digestion reaction.
In some embodiments, the slurries in the step (2) are by water and grape pip powder by volume mass ratio 3-6
(mL)：It is prepared by 1 (g) mixing.
In certain embodiments, the slurries in the step (2) are by volume mass by water and grape pip powder than 5
(mL)：It is prepared by 1 (g) mixing.In certain embodiments, the slurries in the step (2) are by water and grape pip powder by body
Product mass ratio 6 (mL)：It is prepared by 1 (g) mixing.
In some embodiments, adjusting slurry pH to 2-6 in the step (2).In certain embodiments, the step
Suddenly adjusting slurry pH to 5 in (2).
In some embodiments, mixed enzyme described in the step (2) is cellulase, pectase, hemicellulase
(0.6-0.7) is pressed with zytase：(0.1-0.15)：(0.1-0.2)：The mass ratio of (0.1-0.15) mixes.It is specific at some
In embodiment, mixed enzyme described in the step (2) is that cellulase, pectase, hemicellulase and zytase press 0.6：
0.1：0.2：0.1 mass ratio mixing.
In some embodiments, in the step (2) mixed enzyme additive amount be slurries 1wt%-2wt%.At some
In specific embodiment, mixed enzyme additive amount is the 2wt% of slurries in the step (2).
In some embodiments, the enzyme digestion reaction is to react 1-3h at 40-60 DEG C.
Step (3) of the present invention carries out acid protease enzymolysis to the first mixed liquor.First by the first mixing in step (2)
The pH of liquid is adjusted to acidity, and acid protease is then added and digests to obtain acid hydrolysis solution.
In some embodiments, pH to 2-6 is adjusted in the step (3).In certain embodiments, the step
(3) pH to 2 is adjusted in.
In some embodiments, acid protease additive amount is 1wt%-2wt% in the step (3).In some tools
In body embodiment, acid protease additive amount is 1wt% in the step (3).
In some embodiments, enzyme digestion reaction described in the step (3) is to react 1-3h at 40-60 DEG C.At some
In specific embodiment, enzyme digestion reaction described in the step (3) is to react 3h at 50 DEG C.
Step (4) of the present invention carries out alkali carries to obtained acid hydrolysis solution and takes.Lye pH adjustment is added in acid hydrolysis solution in step (3)
To alkalinity, the second mixed liquor is obtained by the reaction.
In some embodiments, the tune pH to 8-10 in the step (4).In certain embodiments, the step
Suddenly the tune pH to 8 in (4).
In one embodiment of the present invention, the lye in the step (4) is that sodium hydroxide presses mass body with distilled water
Product is than 20-40 (g)：1 (L) is configured.
In some embodiments, reaction described in the step (4) is to react 20-40min at 40-60 DEG C.One
In a little specific embodiments, reaction is to react 30min at 50 DEG C described in the step (4).
Step (5) of the present invention extracts grape seed oil from the second mixed liquor.To the second mixed liquor enzyme deactivation in step (4), centrifugation
Separation, takes upper layer free oil, obtains grape seed oil.
In some embodiments, enzyme deactivation is that slurries are warming up to 80-90 DEG C of enzyme deactivation 10-20min in the step (5),
It is cooling.In certain embodiments, enzyme deactivation is that slurries are warming up to 85 DEG C of enzyme deactivation 15min in the step (5), cooling.
In some embodiments, centrifugal rotational speed described in the step (5) is 3000-4000r/min, centrifuges 10-
20min.In certain embodiments, centrifugal rotational speed described in the step (5) is 3500r/min, centrifuges 15min.
The present invention also provides the grape seed oils that above-mentioned method obtains.
In a specific embodiment, the hypoglycemic effect of the grape seed oil of the invention produced has been investigated, has as a result been shown
The grape seed oil that the present invention produces can effectively improve glucose tolerance in mice, significantly decrease mouse cholesterol, triglycerides, pancreas
The content of island element and HbA1c, and effect is better than corn oil.The grape seed oil (GSO) that the present invention produces organizes interleukin-6, swells
Tumor necrosis factor, c reactive protein content have reduction.The result shows that grape seed oil is made in the present invention there is apparent auxiliary to drop blood
Sugared effect.Therefore the application the present invention also provides the grape seed oil in health food.
The present invention extracts grape seed oil using composite plant hydrolase and acid protease fractional hydrolysis method, greatly retains
The content of active constituent especially polyphenol in grape seed oil, while taking into account grape seed oil recovery rate.Compared with prior art,
The present invention one of has the advantages that：
(1) compared to squeezing or leach prepare grape seed oil, the present invention greatly remain in grape seed oil activity at
Point, such as unsaturated fatty acid (86.63%), total phenol (37.46mg/kg), total tocopherol (253.6mg/kg), total sterol
(2.588mg/g), hence it is evident that higher than the active component content of grape seed oil made from existing aqueous enzymatic method.And grape seed oil obtained
Clear can be used as high-end oil for health care.
(2) preparation method of the present invention, the used time is short, can effectively destroy the cell wall of grape pip benevolence cell so that cell
In grease be more easy to extract, effectively improve the recovery rate of grape seed oil.
(3) it is demulsified by using alkaline extraction, compared with other aqueous enzymatic methods are using organic solvent oil and grease extracting, avoids solvent
Residual, while acid value 0.168 (KOH)/(mg/g) of grape pip crude oil can be effectively reduced, it is not necessarily to later stage alkali refining process.
(3) this method is easy to operate, at low cost, is suitable for industrialized production.
Specific implementation mode
The invention discloses a kind of grape seed oils and preparation method thereof.Those skilled in the art can use for reference present disclosure,
It is suitably modified technological parameter realization.In particular, it should be pointed out that all similar substitutions and modifications carry out those skilled in the art
Say it is it will be apparent that they are considered as being included in the present invention.The method and product of the present invention has passed through preferred embodiment
It is described, related personnel can obviously not depart from the content of present invention, carried out to method described herein in spirit and scope
It changes or suitably changes and combine, to realize and apply 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 embodiments are only a part of the embodiments of the present invention, rather than all
Embodiment.Based on the embodiments of the present invention, those of ordinary skill in the art institute without making creative work
The every other embodiment obtained, shall fall within the protection scope of the present invention.
Unless otherwise specified, raw materials used in the embodiment of the present invention or auxiliary material (enzyme preparation) is available on the market.Below
In embodiment, corn oil, lard are commercially available.
Grape pip oil content measures：It is measured using soxhlet extraction methods according to GB/T5009.6-2003.
The measurement of grape seed oil acid value：According to GB/T 5530-2005《Animal and plant fat acid value and acidity assaying》Using cold
Solvent method measures.
Oil yield assay method：Grape seed oil recovery rate (%)=(free oil quality/grape pip benevolence quality) × 100.
Recovery rate assay method：Grape seed oil recovery rate (%)=free oil quality/(grape pip powder quality × grape pip contains
Oil cut rate) × 100.
Grape seed oil total phenol content measures：According to GB/T 8313-2008《Tea Polyphenols in Tea and catechin content
Detection method》Using Forint phenol method spectrophotometric determination.
Total tocopherol assay method：Sample pre-treatments：1.5g (being accurate to 0.001g) oil sample is weighed, brown volumetric flask is placed in
In, appropriate n-hexane dissolution is added, 10ml is settled to after ultrasonic 5min, liquid chromatogram HPLC is carried out after crossing 0.22um miillpore filters
Analysis.
HPLC conditions：Chromatographic column isSilica (4.6mm × 250mm, 5 μm)；Ultraviolet detection wavelength 295nm, stream
Dynamic is mutually n-hexane：Isopropanol=98.5:1.5；Flow velocity 1.0ml/min；25 DEG C of column temperature；10.0 μ l of sample size.
Total sterol assay method：Sample pre-treatments：Weigh 0.2 ± 0.01g grape seed oils, addition 0.1mg/ml5 α-cholesteric
Alkanol titer makees internal standard compound, adds 3mL 2mol/L KOH-CH3CH2OH solution, ultrasonication 5min, 85 DEG C of water-bath soaps
Change 30min, 2mL water and 5mL n-hexanes, oscillation are added after cooling, 4000r/min centrifuges 5min, takes supernatant, lower layer 5mL
N-hexane extracts twice again, merges organic layer, is washed to neutrality, N2200 μ L derivatization reagents BSTFA+TMCS are added in drying
(99:1), 75 DEG C of water-bath 30min carry out GC-MS analyses after crossing 0.22 μm of miillpore filter.
GC conditions：Chromatographic column：Thermo TR-5MS (30m × 0.25mm, 0.25 μm), 1.0 μ L of sample size, into
280 DEG C, helium He, flow velocity 1.2mL/min of sample mouth temperature.Temperature programming：200 DEG C of initial temperature is warming up to 250 DEG C with 10 DEG C/min,
1min is kept, 300 DEG C is warming up to 5 DEG C/min, keeps 20min.
Mass Spectrometry Conditions:250 DEG C of interface temperature ionizes mode EI, and electron energy 70eV, 250 DEG C of ion source temperature, quality is swept
Retouch 50~550amu of range m/z.
Unsaturated fatty acid assay method：Sample pre-treatments：Oil sample 0.03 ± 0.001g grape seed oils are weighed, are added
The NaOH-CH of 0.5mol/L3OH solution 2mL, shaken well, 65 DEG C of heating water bath to oil droplets are completely dissolved, and stand cooling, are added
25% BF3-CH3OH solution 2mL is esterified 20min under 65 DEG C of water bath conditions, stands cooling, and 2mL n-hexanes, shake well is added
2mL is added afterwards and is saturated NaCl solution, centrifuges 15min, takes upper organic phase in drying sample bottle, a small amount of anhydrous Na is added2SO4
Remove micro water.
GC conditions：PEG-20M capillary columns (30m × 0.32mm, 0.25 μm)；Carrier gas：Purity is 99.999%
N2；Purge flow rate：3mL/min；Sample size：1μL；Split ratio 80:1；250 DEG C of injector temperature；250 DEG C of detector temperature；
Fid detector.Temperature program：150 DEG C of initial temperature is risen to 190 DEG C with 5 DEG C/min, keeps 2min, then risen to 5 DEG C/min
240 DEG C, keep 10min.
The assay method of color and luster：The color and luster of grape seed oil is measured using colour photometer.CIE L are used in measurement*a*b*Table color is empty
Between.Color parameter and definition：L*For lightness (black-and-white, 0-100), a*For red green phase (green-red ,-a*-+a*)、b*For champac color
Phase (blue-yellow ,-b*-+b*)。
Experimental animal：C57BL/6J mouse, SPF grades, weight (18 ± 2) g, by Shanghai Slac Experimental Animal Co., Ltd.
It provides.
Key instrument：Blood glucose meter, ROCHE；Microplate reader, BioTek Cytation companies of the U.S.；Superfreeze refrigerator,
U.S. Thermo Fisher Scientific；7200 type spectrophotometers, Shanghai spectral element Instrument Ltd.；Kit, south
Bioengineering Research Institute is built up in capital.
The influence of embodiment 1, mixed enzyme type and additive amount to extraction grape seed oil
(1) grape pip pre-processes：Grape pip is crushed using universal mill, 50 mesh sieve is crossed, obtains grape pip powder raw material,
Its moisture and volatile matter content content is 8.65%, oil content 17.25%, crude protein content 9.2%, and fiber content is
30.6%.
(2) mixed enzyme digests：By distilled water and grape pip powder by volume mass than 5 (mL)：Slurries are made in 1 (g) mixing, add
Enter hydrochloric acid and slurries pH is adjusted to 5, and mixed enzyme enzymolysis is added, enzyme digestion reaction temperature 50 C, the enzyme digestion reaction time is 2h, mixed enzyme
Addition scheme it is as shown in table 1；
(3) acid protease digests：Hydrochloric acid is added in slurries, pH is adjusted to 4.5, and acid protease enzymolysis is added,
Additive amount is 0.1%, and enzyme digestion reaction temperature is 50 DEG C, and the enzyme digestion reaction time is 2h.
(4) lye extracts：Sodium hydroxide presses mass volume ratio 20~40 (g) with distilled water：1 (L) is configured, and is added in slurries
PH is adjusted to 8 by the sodium hydroxide solution of configuration, and alkali carries reaction temperature is 50 DEG C, and the alkali carries reaction time is 30min.
(5) grease is extracted：Slurries are warming up to 85 DEG C of enzyme deactivation 15min, by mixed liquor 3500r/min, 15min is centrifuged, takes
Upper layer free oil obtains light yellow grape seed oil.
The influence of 1 mixed enzyme type of table and additive amount to grape seed oil recovery rate and total phenol content
By table 1 as it can be seen that grape seed oil polyphenol content can be improved using complex enzyme, using the grape of single enzyme preparation extraction
Seed oil oil yield and polyphenol content be not high.Contain cellulase, pectase, hemicellulase and zytase in complex enzyme,
With the increase of complex enzyme content, the viscosity of slurries becomes larger, and emulsion layer increases, and grape seed oil recovery rate and total phenol content are in reduction
Trend.Complex enzyme additive amount is up to 37.46mg/kg in 1% best results, total phenol content.
The influence of 2 protease species of embodiment and additive amount to extraction grape seed oil
(1) grape pip pre-processes：Grape pip is crushed using universal mill, 50 mesh sieve is crossed, obtains grape pip powder raw material,
Its moisture and volatile matter content content is 8.65%, oil content 17.25%, crude protein content 9.2%, and fiber content is
30.6%.
(2) mixed enzyme digests：By distilled water and grape pip powder by volume mass than 5 (mL)：Slurries are made in 1 (g) mixing, add
Enter hydrochloric acid and slurries pH is adjusted to 5, and adds 1% mixed enzyme (its cellulase：Pectase：Hemicellulase：Zytase
Proportioning be 0.6:0.1:0.2:0.1), enzyme digestion reaction temperature 50 C, enzyme digestion reaction time are 2h；
(3) protease hydrolyzed：Protease hydrolyzed is added, enzyme digestion reaction temperature is 50 DEG C, and the enzyme digestion reaction time is 2h, albumen
Enzyme additive amount, pH are as shown in table 2.
(4) lye extracts：Sodium hydroxide presses mass volume ratio 20-40 (g) with distilled water：1 (L) is configured, and is added in slurries
PH is adjusted to 8 by the sodium hydroxide solution of configuration, and alkali carries reaction temperature is 50 DEG C, and the alkali carries reaction time is 30min.
(5) grease is extracted：Slurries are warming up to 85 DEG C of enzyme deactivation 15min, by mixed liquor 3500r/min, 15min is centrifuged, takes
Upper layer free oil obtains light yellow grape seed oil.
The influence of 2 protease species of table and content to grape seed oil recovery rate and total phenol content
As can be seen from Table 2, under the conditions of identical additive amount, acid protease, can be with compared with neutral proteinase, alkali protease
Improve the polyphenol content in grape seed oil.Acid protease additive amount best results at 1%, total phenol content reach 37.46mg/
kg。
The influence of 3 acid protease hydrolysis temperature of embodiment, time and pH to extraction grape seed oil
(1) grape pip pre-processes：Grape pip is crushed using universal mill, 50 mesh sieve is crossed, obtains grape pip powder raw material,
Its moisture and volatile matter content content is 8.65%, oil content 17.25%, crude protein content 9.2%, and fiber content is
30.6%.
(2) mixed enzyme digests：By distilled water and grape pip powder by volume mass than 5 (mL)：Slurries are made in 1 (g) mixing, add
Enter hydrochloric acid and slurries pH is adjusted to 5, and adds 1% mixed enzyme (its cellulase：Pectase：Hemicellulase：Zytase
Proportioning be 0.6:0.1:0.2:0.1), enzyme digestion reaction temperature 50 C, enzyme digestion reaction time are 2h.
(3) acid protease digests：Hydrochloric acid is added in slurries, and acid protease enzymolysis is added, additive amount 1%,
Influence of the hydrolysis temperature, enzymolysis time, pH of acid protease to enzymatic hydrolyzation and total phenol content has as shown in table 3.
(4) lye extracts：Sodium hydroxide presses mass volume ratio 20-40 (g) with distilled water：1 (L) is configured, and is added in slurries
PH is adjusted to 8 by the sodium hydroxide solution of configuration, and alkali carries reaction temperature is 50 DEG C, and the alkali carries reaction time is 30min.
(5) grease is extracted：Slurries are warming up to 85 DEG C of enzyme deactivation 15min, by mixed liquor 3500r/min, 15min is centrifuged, takes
Upper layer free oil obtains light yellow grape seed oil.
3 acid protease hydrolysis temperature of table, the influence of time and pH to grape seed oil recovery rate and total phenol content
| Hydrolysis temperature (DEG C) | Enzymolysis time (h) | pH | Oil yield (%) | Recovery rate (%) | Total phenol content (mg/kg) |
| 40 | 2 | 4.5 | 9.23 | 53.51 | 34.27 |
| 50 | 2 | 4.5 | 10.29 | 59.65 | 37.46 |
| 60 | 2 | 4.5 | 10.34 | 59.94 | 35.13 |
| 50 | 1 | 4.5 | 6.78 | 39.30 | 32.11 |
| 50 | 3 | 4.5 | 11.26 | 65.28 | 40.12 |
| 50 | 2 | 2 | 9.45 | 54.78 | 42.34 |
| 50 | 2 | 6 | 10.67 | 61.86 | 30.12 |
By table 3 as it can be seen that grape seed oil total phenol content when 50 DEG C of acid protease hydrolysis temperature, enzymolysis time 2h, pH=2
Highest, up to 42.34mg/kg.
The influence of 4 lye Extracting temperature of embodiment and time to extraction grape seed oil
A kind of preparation method of auxiliary hyperglycemic grape seed oil, key step are as follows
(1) grape pip pre-processes：Grape pip is crushed using universal mill, 50 mesh sieve is crossed, obtains grape pip powder raw material,
Its moisture and volatile matter content content is 8.65%, oil content 17.25%, crude protein content 9.2%, and fiber content is
30.6%.
(2) mixed enzyme digests：By distilled water and grape pip powder by volume mass than 5 (mL)：Slurries are made in 1 (g) mixing, add
Enter hydrochloric acid and slurries pH is adjusted to 5, and adds 1% mixed enzyme (its cellulase：Pectase：Hemicellulase：Zytase
Proportioning be 0.6:0.1:0.2:0.1), enzyme digestion reaction temperature 50 C, enzyme digestion reaction time are 2h；
(3) acid protease digests：Hydrochloric acid is added in slurries, pH is adjusted to 4.5, and acid protease enzymolysis is added,
Additive amount is 1%, and enzyme digestion reaction temperature is 50 DEG C, and the enzyme digestion reaction time is 2h,.
(4) lye extracts：Sodium hydroxide presses mass volume ratio 20-40 (g) with distilled water：1 (L) is configured, and is added in slurries
PH is adjusted to 8 by the sodium hydroxide solution of configuration, and the alkali reaction temperature time is as shown in table 4.
(5) grease is extracted：Slurries are warming up to 85 DEG C of enzyme deactivation 15min, by mixed liquor 3500r/min, 15min is centrifuged, takes
Upper layer free oil obtains light yellow grape seed oil.
4 alkali carries of table take influence of the temperature and time to grape seed oil recovery rate and total phenol content
By table 4 as it can be seen that grape seed oil total phenol content highest when alkali carries temperature 50 C, alkali carries time 30min, is
37.46mg/kg.During alkali carries, temperature is excessively high or extraction time is longer, can all reduce the total phenol content in grape seed oil.
Embodiment 5 does not use alkali carries to take the influence to extracting grape seed oil
(1) grape pip pre-processes：Grape pip is crushed using universal mill, 50 mesh sieve is crossed, obtains grape pip powder raw material,
Its moisture and volatile matter content content is 8.65%, oil content 17.25%, crude protein content 9.2%, and fiber content is
30.6%.
(2) mixed enzyme digests：By distilled water and grape pip powder by volume mass than 5 (mL)：Slurries are made in 1 (g) mixing, add
Enter hydrochloric acid and slurries pH is adjusted to 5, and adds 1% mixed enzyme (its cellulase：Pectase：Hemicellulase：Zytase
Proportioning be 0.6:0.1:0.2:0.1), enzyme digestion reaction temperature 50 C, enzyme digestion reaction time are 2h；
(3) acid protease digests：Hydrochloric acid is added in slurries, pH is adjusted to 4.5, and acid protease enzymolysis is added,
Additive amount is 1%, and enzyme digestion reaction temperature is 50 DEG C, and the enzyme digestion reaction time is 2h..
(4) grease is extracted：Slurries are warming up to 85 DEG C of enzyme deactivation 15min, by mixed liquor 3500r/min, 15min is centrifuged, takes
Upper layer free oil obtains light yellow grape seed oil.
At this point, grape seed oil oil yield is 3.61%, and recovery rate 20.93%, total phenol content 40.14mg/kg.
Influence of the embodiment 6 using other breaking methods to extraction grape seed oil
(1) grape pip pre-processes：Grape pip is crushed using universal mill, 50 mesh sieve is crossed, obtains grape pip powder raw material,
Its moisture and volatile matter content content is 8.65%, oil content 17.25%, crude protein content 9.2%, and fiber content is
30.6%.
(2) mixed enzyme digests：By distilled water and grape pip powder by volume mass than 5 (mL)：Slurries are made in 1 (g) mixing, add
Enter hydrochloric acid and slurries pH is adjusted to 5, and adds 1% mixed enzyme (its cellulase：Pectase：Hemicellulase：Zytase
Proportioning be 0.6:0.1:0.2:0.1), enzyme digestion reaction temperature 50 C, enzyme digestion reaction time are 2h；
(3) acid protease digests：Hydrochloric acid is added in slurries, pH is adjusted to 4.5, and acid protease enzymolysis is added,
Additive amount is 1%, and enzyme digestion reaction temperature is 50 DEG C, and the enzyme digestion reaction time is 2h.
(4) enzyme deactivation：Slurries are warming up to 85 DEG C of enzyme deactivation 15min.
(5) it extracts：100ml n-hexanes, the ultrasound 30min in ultrasonic cleaning machine is added.
(6) grease is extracted：By mixed liquor 3500r/min, 15min is centrifuged, upper organic phase, 40 DEG C of rotary evaporations is taken to obtain
To light yellow grape seed oil.
At this point, grape seed oil oil yield is 6.01%, and recovery rate 34.84%, total phenol content 32.14mg/kg.
Influence of 7 solid-liquid ratio of embodiment to extraction grape seed oil
(1) grape pip pre-processes：Grape pip is crushed using universal mill, 50 mesh sieve is crossed, obtains grape pip powder raw material,
Its moisture and volatile matter content content is 8.65%, oil content 17.25%, crude protein content 9.2%, and fiber content is
30.6%.
(2) mixed enzyme digests：Slurries are made in distilled water and grape pip powder mixing, hydrochloric acid is added, slurries pH is adjusted to 5, and
Mixed enzyme (its cellulase of addition 1%：Pectase：Hemicellulase：The proportioning of zytase is 0.6:0.1:0.2:
0.1), enzyme digestion reaction temperature 50 C, enzyme digestion reaction time are 2h；
(3) acid protease digests：Hydrochloric acid is added in slurries, pH is adjusted to 4.5, and acid protease enzymolysis is added,
Additive amount is 1%, and enzyme digestion reaction temperature is 50 DEG C, and the enzyme digestion reaction time is 2h.
(4) lye extracts：Sodium hydroxide presses mass volume ratio 20-40 (g) with distilled water：1 (L) is configured, and is added in slurries
PH is adjusted to 8 by the sodium hydroxide solution of configuration, and alkali carries reaction temperature is 50 DEG C, and the alkali carries reaction time is 30min.
(5) grease is extracted：Slurries are warming up to 85 DEG C of enzyme deactivation 15min, by mixed liquor 3500r/min, 15min is centrifuged, takes
Upper layer free oil obtains light yellow grape seed oil.
Influence of 5 solid-liquid ratio of table to grape seed oil recovery rate and total phenol content
| Distilled water (mL)：Grape pip powder mixes (g) | Oil yield (%) | Recovery rate (%) | Total phenol content (mg/kg) |
| 3:1 | 9.67 | 56.06 | 35.68 |
| 4:1 | 9.90 | 57.39 | 36.52 |
| 5:1 | 10.29 | 59.65 | 37.46 |
| 6:1 | 10.12 | 58.67 | 38.68 |
Table 5 is as it can be seen that distilled water presses volume mass than 6 (mL) with grape pip powder:Total phenol when 1 (g) extracts grape seed oil contains
Amount is higher, up to 38.68mg/kg.
The measurement of embodiment 8 grape seed oil beneficiating ingredient and acid value
(1) grape pip pre-processes：Grape pip is crushed using universal mill, 50 mesh sieve is crossed, obtains grape pip powder raw material,
Its moisture and volatile matter content content is 8.65%, oil content 17.25%, crude protein content 9.2%, and fiber content is
30.6%.
(2) mixed enzyme digests：By distilled water and grape pip powder by volume mass than 5 (mL)：Slurries are made in 1 (g) mixing, add
Enter hydrochloric acid and slurries pH is adjusted to 5, and adds 1% mixed enzyme (its cellulase：Pectase：Hemicellulase：Zytase
Proportioning be 0.6:0.1:0.2:0.1), enzyme digestion reaction temperature 50 C, enzyme digestion reaction time are 2h；
(3) acid protease digests：Hydrochloric acid is added in slurries, pH is adjusted to 4.5, and acid protease enzymolysis is added,
Additive amount is 1%, and enzyme digestion reaction temperature is 50 DEG C, and the enzyme digestion reaction time is 2h.
(4) lye extracts：Sodium hydroxide presses mass volume ratio 20-40 (g) with distilled water：1 (L) is configured, and is added in slurries
PH is adjusted to 8 by the sodium hydroxide solution of configuration, and alkali carries reaction temperature is 50 DEG C, and the alkali carries reaction time is 30min.
(5) grease is extracted：Slurries are warming up to 85 DEG C of enzyme deactivation 15min, by mixed liquor 3500r/min, 15min is centrifuged, takes
Upper layer free oil obtains light yellow grape seed oil.
The content of benefit materials in grape seed oil：Unsaturated fatty acid (86.63%), total phenol (37.46mg/kg), total life
Educate phenol (253.6mg/kg), total sterol (2.588mg/g).Gained grape seed oil acid value is 0.168 (KOH)/(mg/g).
The polyphenol of 9 other methods of reference examples compares
Grape pip crushes, and crosses 40 mesh, solid-liquid ratio 1:9, it is 6.5 to adjust pH, adds 1% complex enzyme (cellulase, pectin
Enzyme, zytase, trypsase mass ratio 2:1:2:1), 45 DEG C of enzymolysis 9h, enzyme deactivation 5min postcoolings to room temperature, with 3900r/
The rotating speed of min centrifuges, and draws upper layer edible vegetable oil and freezes enzymolysis liquid repeatedly with freeze-thaw method breaking emulsion, thaws, centrifuged,
Until upper layer does not have oil reservoir, oil quality (Li Dandan, 2017) is weighed.Grape seed oil total phenol content is obtained by experiment
12.79mg/kg, acid value are 0.52 (KOH)/(mg/g).Grape pip oil sample total phenol content is more compared with reference examples 9, in embodiment 8
Height, acid value are lower.The enzymolysis time of reference examples 9 is long, is unfavorable for active constituent in crude oil, promotes Oxidation of Fat and Oils.
The polyphenol of 10 other methods of reference examples compares
Grape pip crushes, and 40 mesh is crossed, with 1:Citric acid-sodium citrate buffer, pH5.5,50 DEG C of water-baths are added in 3 ratios
5min is added the stirring of enzyme dosage 1% (V/W) cellulase, petroleum ether is added after digesting 1.5h, continues to act on 30min, 8000r/
Min centrifuges 30min, oil phase rotary evaporation, and gained crude oil is weighed (Gao Lu, 2009).Grape seed oil total phenol content is obtained by experiment
20.14mg/kg, acid value are 0.43 (KOH)/(mg/g).Compared with reference examples 10, grape pip oil sample total phenol content in embodiment 8
Higher, acid value are lower.
The polyphenol of 11 other methods of reference examples compares
Grape pip crushed 40 mesh, solid-liquid ratio 1:6, the citric acid solution that pH value is 4.18 is added, atmospheric steam is pre-
20min is handled, cellulase is added in the additive amount that 1.0% (V/W) is pressed after cooling, and 45 DEG C of waters bath with thermostatic control digest 1h, are warming up to 55
DEG C, continue to be warming up to 85 DEG C after digesting 8h, keeps 10min enzyme deactivations, be cooled to room temperature, 10min, nothing are centrifuged at 4500r/min
Water ether oil and grease extracting, it is dry, solvent remaining in oil removing is removed, grape seed oil (Lv Shanshan, 2010) is obtained.Experiment gained grape
Seed oil total phenol content is 10.28mg/kg, and acid value is 1.24 (KOH)/(mg/g).
Compared with reference examples 11, grape pip oil sample total phenol content higher, acid value are lower in embodiment 8.The enzyme of reference examples 11
Overlong time is solved, active constituent in crude oil is unfavorable for, promotes Oxidation of Fat and Oils.
The polyphenol of 12 other methods of reference examples compares
After grape pip freeze-day with constant temperature, 80 mesh sieve is crushed, distilled water (1 is added:6.6) it, is placed in ultrasound reactor,
Ultrasonic power 225W, ultrasonic 15min, temperature 50 C.PH5.0 is adjusted later, cellulase 2.0% is first added, and digests 2.0h,
PH7.0 is adjusted again, adds 1.0% neutral protease enzymolysis 1.5h.After enzymolysis, the enzyme deactivation 10min in boiling water bath, in 4000r/
20min is centrifuged under min, collects upper layer free oil and lotion.Emulsion is put into beaker and is placed in microwave reactor, microwave power
500W, microwave time 7min.Emulsion after microwave action is being centrifuged into 15min at 4000r/min, is detaching free oil, it will
Gained free oil weighs (Hu Bin, 2015) after merging twice.Experiment gained grape seed oil total phenol content is 18.56mg/kg, acid value
For 2.16 (KOH)/(mg/g).
Compared with reference examples 12, grape pip oil sample total phenol content higher, acid value are lower in embodiment 8.
13 conventional press method of embodiment and the method for the invention extract the influence to grape seed oil coloration
Conventional press method is measured respectively and embodiment 8 extracts grape seed oil coloration.
6 conventional press method of table and embodiment 8 extract the coloration of grape seed oil
| Extracting mode | L* | a* | b* | ΔE* |
| Conventional press method | 83.05±2.96 | -4.10±0.65 | 47.31±1.66 | 47.82±2.02 |
| Embodiment 8 | 84.99±1.00 | -4.07±0.09 | 38.70±0.97 | 39.02±1.13 |
By table 6 as it can be seen that the total color difference Δ E of 8 gained grape seed oil of embodiment*It is 39.02 ± 1.13, which is less than tradition
Squeezing method extracts the Δ E of grape seed oil*The aberration of value 47.82,8 gained grape seed oil of embodiment is small, and color is more uniform.The Portugals Liang Zhong
The brightness value L of grape seed oil*：Conventional press method (83.05)<8 method of embodiment (84.99) illustrates grape seed oil obtained by 8 method of embodiment
Brightness value L*Closer to white, color and luster is bright, and the grape seed oil obtained by conventional press method is more muddy.The a of two kinds of grape seed oils*
It is negative value, b*It is positive value, it is green and yellow illustrates that the color and luster of grape seed oil is partial to.Meanwhile grape seed oil obtained by 8 method of embodiment
Red value of green a*With champac value b*It is more biased towards in neutrality than conventional press method.
14 auxiliary hyperglycemic grape seed oil of embodiment has the effect experiment of function of blood sugar reduction
(1) raising of rat
Rat feeding is in Experimental Animal Center SPF grades of barrier animal laboratory of Southern Yangtze University.Animal daily nursing and experiment
Condition meets《Ministry of Health of the People's Republic of China's experimental animal environment and facility standard》.
Healthy male C 57 BL/6 J mouse (20 ± 2g) is bought, normal diet (AIN93G) adaptability is raised 5 days, fasting 16
Hour, mouse tail blood is taken, mouse is randomly divided by normal group (ND), corn oil group (CO), pig according to mouse fasting blood glucose level
Grape seed oil group (GSO) obtained by 8 method of oily model control group (Lard) and embodiment, every group 12.
3.2 grouping feed formula administrations
It is grouped feed formula administration：Normal group feed formula is according to research diet companies with reference to U.S.'s nutrition
The AIN-93G experimental animal feed formulas that association is recommended are formulated, model control group feed formula prepare with reference to D12492 and
At every group of feeding time is morning 8:30-9:00, free diet continuously gives the feed of different formulations 3 months.
The feed formula of 7 different experiments group of table
(2) sample collection and index determining
Fasting blood-glucose and sugar tolerance (blood sample)：After forage feed 3 months, mouse is deprived of food but not water 16h, and determination limit is on an empty stomach
The glucose solution of 1g/kg weight is injected intraperitoneally in fasting blood-glucose when blood glucose is as 0min, and measure mouse with blood glucose meter notes in abdominal cavity
Tail vein blood glucose when 30min, 60min, 90min, 120min after glucose solution is penetrated, for measuring sugar tolerance.
Insulin, cholesterol, triglycerides, HbA1c are horizontal (blood sample)：After the test, each group animal fasting 12 hours,
Mouse is injected intraperitoneally using 1% Nembutal sodium solution, eyeball is taken a blood sample after anesthesia, stands 1h or so, 3000g centrifugations
Serum is taken to be preserved in -80 DEG C of refrigerators after 10min for use.
Inflammatory factor IL-6, TNF-α, CRP (tissue):Post mortem at mouse takes liver, kidney, spleen, pancreas, small
Intestines.By each internal organs be stored in -80 DEG C it is spare.
It measures each group biochemical indicator respectively using kit, is as a result indicated with mean ± SD, using SPSS statistical softwares
(23.0) it analyzes, ANOVA analyses is carried out to result.
After experiment, each group mouse biochemical marker level changes as shown in table 8-10.
The different group glucose tolerance in mice of table 8 compare
Note：The different letter of same row indicates there is significant difference in table.
Table 8 the experimental results showed that compared with Lard model group groups, obviously more stablize, and illustrates GSO by the blood glucose trend of GSO groups
Group has better tolerance to glucose injection, and the blood glucose at 60min and 90min is significantly lower than Lard groups (p<0.05).
Compared to 60% high lipid food group mouse, the insulin sensitivity of ND group mouse is best.Region area (AUC) is lower under broken line,
The insulin sensitivity of this group of mouse is better.ND group mouse area under the curve (AUC) is minimum, 60% high lipid food group mouse AUC
It is compared with normal group mouse, significant increase (p<0.01) it is compared with Lard groups, region area under GSO group mouse broken lines
Significantly reduce (p<0.01), illustrate that the grape seed oil that the present invention produces can effectively improve glucose tolerance in mice.
The different group mouse cholesterol of table 9, triglycerides, insulin, HbA1c compare
Table 9 is the results show that lard model (Lard) group mouse cholesterol, triglycerides, insulin, HbA1c and blank group
Compare and all has significant differences (P<0.01), prompt modeling success.
Grape seed oil (GSO) organizes cholesterol, triglycerides, insulin, HbA1c and lard (Lard) the model group phase of mouse
Than each index improves significantly.Meanwhile the insulin and HbA1c contents and corn of grape seed oil (GSO) group mouse
Oily (CO) group compares, also significant reduction (p<0.05) grape seed oil that, the prompt present invention produces can significantly decrease
The content of mouse cholesterol, triglycerides, insulin and HbA1c, and effect is better than corn oil.
The different group mouse liver IL-6 of table 10, TNF-α, CRP compare
Note：The different letter of same row indicates significant difference in table.
Table 10 is the results show that lard model (Lard) group mouse interleukin -6 (IL-6), tumor necrosis factor (TNF-
α), c reactive protein (CRP) relatively all has significant differences (P with blank group<0.01), prompt modeling success.
It is equal that the grape seed oil (GSO) that the present invention produces organizes interleukin-6, tumor necrosis factor, c reactive protein content
There is reduction, the significant difference (P compared with lard model group<0.01).C in the grape seed oil group that the present invention produces reacts egg
Bai Hanliang compares significant reduction (P with corn oil group<0.05).
Conclusion：The result shows that grape seed oil, which is made, in the present invention has apparent auxiliary hyperglycemic effect.
The foregoing is merely the preferred embodiment of the present invention, scheme, feature, original described in every inventional idea of the present invention
Reason and its equivalent or simple change done, are included in the scope of protection of the invention patent.The technical field of the invention
Technical staff described specific embodiment can be modified or be supplemented, or substitute by a similar method, only
The protection model of the present invention should all be belonged to without departing from the structure or beyond the scope defined by this claim of the present invention
It encloses.
Claims (10)
1. a kind of grape seed oil, which is characterized in that its total phenol content >=30mg/kg.
2. grape seed oil according to claim 1, which is characterized in that its unsaturated fatty acid >=86.63%, total tocopherol >=
253.6mg/kg, total sterol >=2.588mg/g, acid value are 0.168 (KOH)/(mg/g).
3. the preparation method of grape seed oil described in claims 1 or 2, includes the following steps：
(1) grape pip crushes, and sieving obtains grape pip powder；
(2) grape pip powder that step (1) obtains adds water mixing that slurries are made, and mixed enzyme is added in adjusting slurry pH to acidity, through enzymolysis
The first mixed liquor is obtained after reaction；
(3) pH of the first mixed liquor of step (2) is adjusted to acidity, acid protease is added and digests to obtain acid hydrolysis solution；
(4) lye pH adjustment is added to alkalinity in the acid hydrolysis solution of step (3), the second mixed liquor is obtained by the reaction；
(5) it to (4) second mixed liquor enzyme deactivation of step, centrifuges, takes upper layer free oil, obtain grape seed oil.
4. preparation method according to claim 3, which is characterized in that the sieving in the step (1) was 20~60 mesh
Sieve.
5. preparation method according to claim 3, which is characterized in that the slurries in the step (2) are by water and grape
Seed powder presses volume mass ratio 3-6 (mL)：It is prepared by 1 (g) mixing；Adjusting slurry pH to 2-6；The mixed enzyme is cellulase, pectin
Enzyme, hemicellulase and zytase press (0.6-0.7)：(0.1-0.15)：(0.1-0.2)：The mass ratio of (0.1-0.15) is mixed
It closes, mixed enzyme additive amount is the 1wt%-2wt% of slurries；The enzyme digestion reaction is to react 1-3h at 40-60 DEG C.
6. preparation method according to claim 3, which is characterized in that adjust pH to 2-6 in the step (3)；Acidic protein
Enzyme additive amount is 1wt%-2wt%；The enzyme digestion reaction is to react 1-3h at 40-60 DEG C.
7. preparation method according to claim 3, which is characterized in that the tune pH to 8-10 in the step (4)；It is described anti-
Should react 20-40min at 40-60 DEG C.
8. preparation method according to claim 3, which is characterized in that enzyme deactivation is to be warming up to slurries in the step (5)
80-90 DEG C of enzyme deactivation 10-20min, it is cooling；The centrifugal rotational speed is 3000-4000r/min, centrifuges 10-20min.
9. the grape seed oil that claim 1-8 any one of them preparation methods obtain.
10. application of the grape seed oil described in claim 1-2 or 9 in health food.
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| CN112004935A (en) * | 2018-03-30 | 2020-11-27 | 帝斯曼知识产权资产管理有限公司 | Method for obtaining microbial oils and method for reducing emulsions by maintaining low carbohydrate concentrations |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102746938A (en) * | 2012-07-14 | 2012-10-24 | 中国农业科学院油料作物研究所 | Method for preparing grease and protein from oil seed kernels by aqueous enzymatic method |
| CN103351944A (en) * | 2013-04-11 | 2013-10-16 | 石河子市天成油脂有限公司 | Method for extracting grape seed oil by cold pressing |
| CN103509642A (en) * | 2013-05-24 | 2014-01-15 | 天津国纳科技发展有限公司 | Production technology of resveratrol riched grape seed oil |
| CN107400557A (en) * | 2017-08-07 | 2017-11-28 | 无限极（中国）有限公司 | A kind of method for extracting grape-kernel oil |
-
2018
- 2018-04-10 CN CN201810315870.6A patent/CN108285827B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102746938A (en) * | 2012-07-14 | 2012-10-24 | 中国农业科学院油料作物研究所 | Method for preparing grease and protein from oil seed kernels by aqueous enzymatic method |
| CN103351944A (en) * | 2013-04-11 | 2013-10-16 | 石河子市天成油脂有限公司 | Method for extracting grape seed oil by cold pressing |
| CN103509642A (en) * | 2013-05-24 | 2014-01-15 | 天津国纳科技发展有限公司 | Production technology of resveratrol riched grape seed oil |
| CN107400557A (en) * | 2017-08-07 | 2017-11-28 | 无限极（中国）有限公司 | A kind of method for extracting grape-kernel oil |
Non-Patent Citations (6)
| Title |
|---|
| 吕姗姗等: "水酶法提取葡萄籽油的工艺研究 ", 《粮油加工》 * |
| 周玲仙: "《云南特有食物图鉴》", 31 March 2012, 云南科技出版社 * |
| 李曌 等: "溶剂类型对葡萄籽多酚提取及抗氧化活性的影响", 《食品工业》 * |
| 杨晋等: "超临界CO_2流体提取含原花青素的葡萄籽油 ", 《食品科技》 * |
| 翟岳明: "关于植物油碱处理的工艺改进", 《涂料工业》 * |
| 郑亚蕾等: "4个葡萄品种葡萄籽冷榨油的性质与体外抗氧化活性", 《食品科学》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112004935A (en) * | 2018-03-30 | 2020-11-27 | 帝斯曼知识产权资产管理有限公司 | Method for obtaining microbial oils and method for reducing emulsions by maintaining low carbohydrate concentrations |
| CN112004935B (en) * | 2018-03-30 | 2024-05-14 | 帝斯曼知识产权资产管理有限公司 | Method for obtaining microbial oil and method for reducing emulsion by maintaining low carbohydrate concentration |
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