CN116536099A - Preparation method of organic grape seed oil - Google Patents

Preparation method of organic grape seed oil Download PDF

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Publication number
CN116536099A
CN116536099A CN202310609257.6A CN202310609257A CN116536099A CN 116536099 A CN116536099 A CN 116536099A CN 202310609257 A CN202310609257 A CN 202310609257A CN 116536099 A CN116536099 A CN 116536099A
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grape seed
seed oil
grape
preparation
oil
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CN202310609257.6A
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Inventor
刘高维
梁旭强
卞琰
郭利斌
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Shanxi Zhongyi Biotechnology Co ltd
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Shanxi Zhongyi Biotechnology Co ltd
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Priority to CN202310609257.6A priority Critical patent/CN116536099A/en
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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
    • 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
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/92—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
    • A61K8/922—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00—Preparations for care of the skin
    • A61Q19/08—Anti-ageing preparations
    • 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
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/52—Stabilizers
    • A61K2800/522—Antioxidants; Radical scavengers

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Engineering & Computer Science (AREA)
  • General Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Veterinary Medicine (AREA)
  • Public Health (AREA)
  • Animal Behavior & Ethology (AREA)
  • Microbiology (AREA)
  • Epidemiology (AREA)
  • Birds (AREA)
  • Biochemistry (AREA)
  • Polymers & Plastics (AREA)
  • Food Science & Technology (AREA)
  • Gerontology & Geriatric Medicine (AREA)
  • Dermatology (AREA)
  • Preparation Of Compounds By Using Micro-Organisms (AREA)

Abstract

The invention provides a preparation method of organic grape seed oil, and belongs to the technical field of vegetable oil production. The grape seeds are crushed after being treated at ultralow temperature by adopting a water enzymatic method, the crushed grape seeds are mixed with water to obtain slurry, compound enzyme is added into the slurry for enzymolysis, and after enzyme deactivation and centrifugation of enzymolysis liquid, upper layer free oil is taken to obtain grape seed oil; the complex enzyme consists of cellulase: pectase: the neutral protease is composed of the components according to the mass ratio of 4-6:1-3:6-8. The method can effectively improve the extraction rate of the grape seed oil, is simple to operate, has low cost and is suitable for industrial production.

Description

Preparation method of organic grape seed oil
Technical Field
The invention belongs to the technical field of vegetable oil production, and particularly relates to a preparation method of organic grape seed oil.
Background
Grape seed oil is a high-grade edible oil obtained by further processing grape seeds, which are a by-product of the squeezing of brewed wine or juice. Grape seed oil is rich in nutrition, and unsaturated fatty acid is up to more than 90%, and mainly comprises linoleic acid (more than 70%), oleic acid, palmitic acid and stearic acid. Linoleic acid is essential fatty acid for human body, is one of important components for forming cell membrane and skin of human body, and can maintain blood lipid balance of adult, reduce cholesterol and improve cardiovascular diseases. Grape seed oil also contains phenolic compounds such as gallic acid, catechin, epicatechin, procyanidins and the like, and recent researches have reported that these phenolic compounds have a wide range of biological activities: antioxidant, anticancer, free radical scavenging, antiinflammatory, antiviral, and blood sugar lowering effects. In addition, the grape seed oil also contains phytosterol, squalene, a plurality of fat-soluble vitamins (A, E, D, K, P) and a plurality of trace elements (Ca, fe, zn, mn, cu).
At present, the main methods for extracting oil from vegetable oil materials are a squeezing method and a leaching method, wherein the oil materials need to be crushed, smashed, squeezed into embryo or baked before being squeezed or leached, and the cell structure of the oil materials is destroyed by mechanical and thermal methods, so that favorable oil extraction conditions are achieved. Although the oil yield of the method is high, the equipment is complex, more importantly, protein denaturation is caused, so that the cake after oil extraction can not be effectively utilized, protein resources are seriously wasted, and a desolventizing process is needed after solvent leaching, so that the equipment is more, the investment is large, and the pollution is heavy. Therefore, in order to overcome the defects of the traditional oil production process, the technology of extracting the vegetable oil by the aqueous enzymatic method is developed in consideration of the factors of economy, environment, safety and the like.
The hydro-enzymatic method degrades plant cell walls by using mechanical and enzymolysis as means, adopts enzyme with degradation effect on oil tissues and complexes such as lipopolysaccharide and lipoprotein on the basis of mechanical disruption to treat the oil, and increases the fluidity of oil in the oil tissues by further damaging the cell structures by the enzyme and decomposing the lipopolysaccharide by the enzyme so as to release the oil. However, the process for extracting vegetable oil by the aqueous enzymatic method has many factors, and the types of enzymes required by different oils, the enzymolysis conditions, the oil treatment modes and other process conditions are different. Therefore, how to extract grape seed oil efficiently by adopting the aqueous enzymatic method is one of the technical problems to be solved in the field.
Disclosure of Invention
Accordingly, the invention aims to provide a preparation method of organic grape seed oil, which can effectively improve the extraction rate of grape seed oil and greatly retain active ingredients in grape seed oil.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of organic grape seed oil, which comprises the following steps: grinding grape seeds after ultralow temperature treatment, mixing the crushed grape seeds with water to obtain slurry, adding complex enzyme into the slurry for enzymolysis, inactivating enzyme in the enzymolysis liquid, centrifuging, and taking upper layer free oil to obtain grape seed oil;
the complex enzyme consists of cellulase: pectase: the neutral protease is composed of the components according to the mass ratio of 4-6:1-3:6-8.
Preferably, the temperature of the ultralow temperature treatment is-80 ℃ and the time is 3-4 hours.
Preferably, the grape seeds are crushed to 60-80 meshes.
Preferably, the mass volume ratio of the grape seeds to the water is 20-30 g:100mL of the mixture was mixed well.
Preferably, the addition amount of the complex enzyme is 100-200U/g based on the mass of grape seeds.
Preferably, the enzymolysis temperature is 45-56 ℃ and the enzymolysis time is 3-6 h.
Preferably, the enzyme deactivation temperature is 85-90 ℃, and the enzyme deactivation time is 10-20 min.
Preferably, the centrifugation condition is 3000-4000 r/min, 12-15 min.
The invention also provides grape seed oil prepared by the preparation method.
The invention also provides application of the grape seed oil prepared by the preparation method in foods or cosmetics.
The invention has the beneficial effects that:
the extraction rate of the grape seed oil can be effectively improved to 11.49% by optimizing the technological conditions of the aqueous enzymatic method, the active ingredients in the grape seed oil are greatly reserved, and the total phenol content is high and reaches 41.21mg/kg. The method is simple to operate, low in cost and suitable for industrial production.
Detailed Description
The invention provides a preparation method of organic grape seed oil, which comprises the following steps: grinding grape seeds after ultralow temperature treatment, mixing the crushed grape seeds with water to obtain slurry, adding complex enzyme into the slurry for enzymolysis, inactivating enzyme in the enzymolysis liquid, centrifuging, and taking upper layer free oil to obtain grape seed oil.
The grape seeds are obtained after peeling and meat, or grape seeds which are byproducts of grape wine brewing or fruit juice squeezing are selected as raw materials for preparing grape seed oil, and preferably, the grape is an organic grape, and more preferably, an Xuegu grape.
The grape seeds are subjected to ultralow temperature treatment, wherein the temperature of the ultralow temperature treatment is-80 ℃, and the time is 3-4 hours, preferably 3.5 hours. The invention can improve the fibrosis of grape seeds, promote the pulverization and is beneficial to keeping the content of active ingredients of the extracted grape seed oil by the ultralow temperature treatment of the grape seeds.
The grape seeds treated at ultralow temperature are crushed, and the grape seeds are crushed to 60-80 meshes, preferably 70 meshes. The invention damages the cell tissue of the oil by a rolling and crushing process, is beneficial to the diffusion of water-soluble components, improves the diffusion rate of enzyme and is beneficial to improving the extraction rate of grape seed oil.
The invention mixes crushed grape seed powder with water to obtain slurry, and the mass volume ratio of grape seed to water is 20-30 g:100mL of the grape seeds are uniformly mixed, and the mass volume ratio of the grape seeds to the water is preferably 22-27 g:100mL, more preferably 24 to 26g:100mL.
The invention directly adds complex enzyme into slurry (grape seed powder-water) for enzymolysis. The complex enzyme consists of cellulase: pectase: the neutral protease consists of the following components in mass ratio of 4-6:1-3:6-8: pectase: the mass ratio of neutral protease is preferably 5:2:7. Based on the mass of grape seeds, the addition amount of the complex enzyme is 100-200U/g, preferably 140-180U/g, and more preferably 170U/g. The enzymolysis temperature is 45-56 ℃, preferably 48-53 ℃, more preferably 50-52 ℃; the enzymolysis time is 3-6 hours, preferably 4-5 hours. The specific sources of cellulase, pectinase and neutral protease are not limited in the present invention.
The enzymatic hydrolysate after enzymatic hydrolysis is subjected to enzyme deactivation treatment, wherein the enzyme deactivation temperature is 85-90 ℃, preferably 86 ℃, and the enzyme deactivation time is 10-20 min, preferably 15-18 min. Naturally cooling the enzyme-deactivated enzymolysis liquid to room temperature, and then performing centrifugal treatment, wherein the centrifugal condition is 3000-4000 r/min, 12-15 min, preferably 3500r/min, and 13-14 min. After centrifugal treatment, the invention takes the upper layer free oil, namely grape seed oil.
The invention also provides grape seed oil prepared by the preparation method, and the grape seed oil can be used in the food industry or added into cosmetics.
In the following examples, conventional methods are used unless otherwise specified.
Materials, reagents and the like used in the examples described below are commercially available unless otherwise specified.
Example 1
A preparation method of organic grape seed oil comprises the following steps:
(1) Peeling organic grape (Xugrape) to obtain grape seed;
(2) Carrying out ultralow temperature treatment on grape seeds, wherein the temperature of the ultralow temperature treatment is-80 ℃ and the time is 3.5h;
(3) Grinding grape seeds to 70 meshes; the mass volume ratio of the crushed grape seeds to water is 26g:100mL of the mixture is uniformly mixed to obtain slurry;
(4) And (3) directly adding complex enzyme into the slurry for enzymolysis. The complex enzyme consists of cellulase: pectase: the neutral protease is obtained by mixing according to the mass ratio of 5:2:7; the addition amount of the complex enzyme is 170U/g; the enzymolysis temperature is 52 ℃, and the enzymolysis time is 5 hours.
(5) And (3) carrying out enzyme deactivation treatment on the enzymatic hydrolysate after enzymatic hydrolysis, wherein the enzyme deactivation temperature is 90 ℃, and the enzyme deactivation time is 15min. Naturally cooling the enzyme-deactivated enzymolysis liquid to room temperature, and then carrying out centrifugal treatment, wherein the centrifugal condition is 3500r/min for 15min, and taking the upper free oil after centrifugation, namely the grape seed oil.
Example 2
This embodiment differs from embodiment 1 only in that: the ultralow temperature treatment time in the step (2) is 3 hours.
Example 3
This embodiment differs from embodiment 1 only in that: the ultralow temperature treatment time in the step (2) is 4 hours.
Example 4
This embodiment differs from embodiment 1 only in that: in the step (3), the mass volume ratio of grape seeds to water is 20g:100mL of the mixture was mixed well.
Example 5
This embodiment differs from embodiment 1 only in that: cellulase in step (4): pectase: neutral protease is composed of the following components in a mass ratio of 4:1:6.
Example 6
This embodiment differs from embodiment 1 only in that: cellulase in step (4): pectase: neutral protease is composed of the following components in mass ratio of 6:3:8.
Example 7
This embodiment differs from embodiment 1 only in that: the addition amount of the complex enzyme in the step (4) is 100U/g.
Example 8
This embodiment differs from embodiment 1 only in that: the addition amount of the complex enzyme in the step (4) is 200U/g.
Example 9
This embodiment differs from embodiment 1 only in that: the enzymolysis temperature in the step (4) is 48 ℃; the enzymolysis time is 6 hours.
Comparative example 1
The difference between this comparative example and example 1 is that: discarding the ultralow temperature treatment process in the step (2).
Comparative example 2
The difference between this comparative example and example 1 is that: cellulase in step (4): pectase: neutral protease is composed of the following components in mass ratio of 5:0:7.
Comparative example 3
The difference between this comparative example and example 1 is that: cellulase in step (4): pectase: neutral protease is composed of the following components in mass ratio of 0:2:7.
Comparative example 4
The difference between this comparative example and example 1 is that: cellulase in step (4): pectase: neutral protease is composed of the following components in mass ratio of 5:2:0.
Comparative example 5
The difference between this comparative example and example 1 is that: in the step (4), the complex enzyme consists of cellulase: hemicellulase: pectase: neutral protease is composed of the following components in a mass ratio of 5:2:2:7.
Comparative example 6
The difference between this comparative example and example 1 is that: in the step (4), the complex enzyme consists of cellulase: hemicellulase: pectase: xylanase is composed of the following components in a mass ratio of 5:2:2:7.
Comparative example 7
The difference between this comparative example and example 1 is that: in the step (4), the complex enzyme consists of cellulase: pectase: xylanase is composed of the following components in mass ratio of 5:2:7.
Grape seed oil extraction was performed by the methods of example 1 and comparative examples 1 to 7, respectively, and the oil yield, extraction rate and total phenol amount were counted. The results are shown in Table 1.
The oil yield measuring method comprises the following steps: grape seed oil yield (%) = (free oil mass/grape seed mass) ×100.
The extraction rate measuring method comprises the following steps: grape seed oil extraction (%) =free oil mass/(grape seed meal mass×grape seed oil content) ×100.
Measuring the total phenol content of grape seed oil: the method is characterized in that the method is determined by using a Fulin phenol method spectrophotometer according to GB/T8313-2008 method for detecting the content of tea polyphenol and catechin in tea.
TABLE 1 oil yield, extraction yield and total phenol content for the different methods
As shown in Table 1, the present invention can effectively increase the oil yield to 11.49% and the total phenol content of the obtained grape seed oil to 41.21mg/kg by extracting grape seed oil by aqueous enzymatic method using complex enzyme (cellulase: pectase: neutral protease).
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.

Claims (10)

1. A method for preparing organic grape seed oil, which is characterized by comprising the following steps: grinding grape seeds after ultralow temperature treatment, mixing the crushed grape seeds with water to obtain slurry, adding complex enzyme into the slurry for enzymolysis, inactivating enzyme in the enzymolysis liquid, centrifuging, and taking upper layer free oil to obtain grape seed oil;
the complex enzyme consists of cellulase: pectase: the neutral protease is composed of the components according to the mass ratio of 4-6:1-3:6-8.
2. The method according to claim 1, wherein the ultra-low temperature treatment is carried out at-80 ℃ for 3 to 4 hours.
3. The method according to claim 1, wherein the grape seeds are crushed to 60 to 80 mesh.
4. The preparation method according to claim 1, wherein the mass volume ratio of grape seeds to water is 20-30 g:100mL of the mixture was mixed well.
5. The method according to claim 1, wherein the amount of the complex enzyme to be added is 100 to 200U/g based on the mass of grape seed.
6. The preparation method according to claim 1, wherein the enzymolysis temperature is 45-56 ℃ and the enzymolysis time is 3-6 h.
7. The preparation method according to claim 1, wherein the enzyme deactivation temperature is 85-90 ℃ and the enzyme deactivation time is 10-20 min.
8. The method according to claim 1, wherein the centrifugation conditions are 3000 to 4000r/min,12 to 15min.
9. The grape seed oil prepared by the preparation method of any one of claims 1 to 8.
10. Use of the grape seed oil prepared by the preparation method of any one of claims 1 to 8 in food or cosmetics.
CN202310609257.6A 2023-05-29 2023-05-29 Preparation method of organic grape seed oil Pending CN116536099A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202310609257.6A CN116536099A (en) 2023-05-29 2023-05-29 Preparation method of organic grape seed oil

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202310609257.6A CN116536099A (en) 2023-05-29 2023-05-29 Preparation method of organic grape seed oil

Publications (1)

Publication Number Publication Date
CN116536099A true CN116536099A (en) 2023-08-04

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