CN115261120A - Method for preparing grape seed oil by using grape seeds and product - Google Patents
Method for preparing grape seed oil by using grape seeds and product Download PDFInfo
- Publication number
- CN115261120A CN115261120A CN202210975422.5A CN202210975422A CN115261120A CN 115261120 A CN115261120 A CN 115261120A CN 202210975422 A CN202210975422 A CN 202210975422A CN 115261120 A CN115261120 A CN 115261120A
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- China
- Prior art keywords
- oil
- grape seed
- grape
- extraction
- treatment
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Images
Classifications
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- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
- C11B1/104—Production of fats or fatty oils from raw materials by extracting using super critical gases or vapours
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- C—CHEMISTRY; METALLURGY
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- 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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- 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
- C11B3/02—Refining fats or fatty oils by chemical reaction
- C11B3/04—Refining fats or fatty oils by chemical reaction with acids
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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
- C11B3/02—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
- C11B3/10—Refining fats or fatty oils by adsorption
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention provides a method for preparing grape seed oil by utilizing grape seeds and a product, belonging to the technical field of grape seed oil preparation, and comprising the following steps: carrying out extraction treatment and separation treatment on grape seeds by using an extractor to obtain crude grape seed oil; carrying out degumming operation on the grape seed crude oil through acidification treatment and hydration treatment to obtain grape seed degummed oil; performing alkali refining treatment and water washing treatment on the grape seed degummed oil to finish deacidification operation to obtain grape seed deacidified oil; carrying out decoloring operation on the grape seed deacidified oil by using a decoloring agent to obtain grape seed decolored oil; and deodorizing the grape seed decolorized oil,obtaining a grape seed oil product; the extraction instrument adopts supercritical CO 2 A fluid extraction apparatus. The method for preparing the grape seed oil by using the grape seeds and the product can solve the problems of low extraction efficiency, low yield, low product quality and partial loss of nutritional active ingredients during refining of the grape seed oil.
Description
Technical Field
The invention relates to the technical field of grape seed oil preparation, in particular to a method for preparing grape seed oil by utilizing grape seeds and a product.
Background
The grape is a plant of genus Vitis of family Vitaceae, and is a plant of the genus Vitaceae. China has abundant grape resources, about 80% of grapes produced every year are used for brewing wine, 13% of grapes are used as fresh fruits, and 7% of grapes are used for processing fruit juice and other grape products. Grape seeds account for about 7-10% of the total weight of fresh fruits, so the grape seeds are a byproduct with a large yield in the wine industry, the utilization rate of the grape seeds in China is not high, except a small part of grape seeds serving as feed and fertilizer, a large amount of grape seeds serving as waste are discarded every year, and great resource waste and environmental stress are caused. The oil content of grape seed is 14-17%, the grape seed oil contains large amount of unsaturated fatty acid with content of more than 90%, wherein the fatty acid mainly comprises linoleic acid with content of 58-76%, and the content of linoleic acid is higher than that of common edible oil such as walnut oil and safflower oil. The grape seed oil has reasonable fatty acid composition, more nutrient components and better application value, is excellent functional edible oil and can be used for eating or health care.
The traditional pressing method and solvent extraction method are mostly adopted when the existing enterprises prepare the grape seed oil from the grape seeds. The oil yield of the squeezing method is low, the impurity content of the produced grape seed oil is high, and high temperature is easily formed in the squeezing process to destroy unsaturated fatty acid. In the products produced by the common solvent extraction method, residual solvents such as acetone, n-hexane (No. 6 solvent) and the like can not meet the requirements of international standards, the safety is low, and the high-temperature extraction environment of part of solvents can damage effective components.
At present, a new preparation method appears in the production of grape seed oil, such as supercritical CO 2 Extraction methods, aqueous enzymatic methods, and the like. The grape seed oil prepared by the aqueous enzymatic method can improve the oil yield, but the enzymolysis product can affect the original oil components, the consumption of the enzyme is high, and the cost is greatly increased. Supercritical fluid extraction with carbon dioxide (CO) 2 ) The solvent has the characteristics of low energy consumption, no pollution, safe operation, little damage to components and the like, can realize the selective separation and recovery of effective components from natural substances, and avoids the problems of low energy consumption, no pollution, low damage to the components and the likeThe defects of organic solvent residue and high-temperature extraction in the traditional method are overcome. However, the supercritical extraction method also has the problems of low extraction efficiency, low quality of the obtained grape seed oil, low yield and high production cost.
It is further found that the grape seed oil crude oil prepared by any method contains impurities which are not beneficial to human health, the physical and chemical properties are unstable, the grape seed oil crude oil can be eaten only by removing the harmful substances through a refining process, but the grape seed oil crude oil is influenced by the conditions of additives, high temperature and the like in the refining process, and the loss of part of nutritional ingredients (such as vitamins and the like) in the crude oil can also be caused.
In view of the increasing demand for green food and environmental awareness, it is imperative to research a method for preparing grape seed oil from grape seeds with high yield, good quality and less loss of active ingredients, so as to break through the restriction of grape seed oil production and have important significance for the healthy development of the grape seed oil industry.
Disclosure of Invention
The invention provides a method for preparing grape seed oil by utilizing grape seeds and a product, which are used for solving the problems of low extraction efficiency, low yield, low product quality and partial loss of nutritional active ingredients during refining of the grape seed oil.
In a first aspect, the present invention provides a method for preparing grape seed oil from grape seeds, comprising: extracting and separating grape seeds by using an extractor to obtain crude grape seed oil; carrying out degumming operation on the grape seed crude oil through acidification treatment and hydration treatment to obtain grape seed degummed oil; performing alkali refining treatment and water washing treatment on the grape seed degummed oil to finish deacidification operation to obtain grape seed deacidified oil; carrying out decoloring operation on the grape seed deacidified oil by using a decoloring agent to obtain grape seed decolored oil; and deodorizing the grape seed decolorized oil to obtain a grape seed oil product.
Further setting that the extraction instrument adopts supercritical CO 2 The fluid extraction instrument has the following extraction treatment conditions: the pressure of the extraction kettle is 25-35MPa, the temperature is 40-50 ℃, and CO is added 2 The flow rate is 15-20L/h, and the single extraction time is 2-3h.
The invention is beneficial toBy supercritical CO 2 The fluid extraction technology is used for extracting the grape seed oil, the oil yield is more than 15%, the extraction time is short, no solvent residue exists, the extraction efficiency and the yield of the grape seed oil are improved, the environmental pollution is low, and the problems of low extraction efficiency, low yield and low product quality in the prior art are solved; the water-soluble and fat-soluble harmful impurities in the crude oil are effectively removed through a refining process, the grape seed oil has high degumming rate, deacidification rate, decoloration rate and the like, the quality of the grape seed oil is improved, the appearance and the taste of oil are improved, the safety of the grape seed oil is ensured, and the quality guarantee period is prolonged.
The extraction treatment is further set to be carried out under the condition of constant pressure and variable temperature solvent flow circulation, and the specific operation is as follows: under the condition of constant pressure of the extraction kettle, the temperature is 40-45 ℃ and CO is added 2 Extracting at flow rate of 15-18L/h for 0.5-1h, and then extracting at 45-50 deg.C with CO 2 Extracting at flow rate of 18-20L/h for 0.5-1h, and then extracting at 40-45 deg.C with CO 2 The extraction is carried out for 0.5 to 1 hour under the condition of the flow rate of 15 to 18L/hour, and the extraction is circulated to the end of the extraction in the way.
Ordinary extraction processing adopts the mode of constant temperature and pressure and constant solvent flow to carry out, and in certain extent, the oil yield can be promoted to the increase temperature and pressure, but the nutrient substance can be harmed to the temperature is too big, and preparation cost can be showing to the pressure is too big, and the oil yield promotes not obviously. The invention adopts a constant-pressure and variable-temperature solvent flow circulation mode to extract grape seeds, and utilizes the convection mass transfer coefficient to be increased along with the temperature rise, so that the crude oil of the grape seeds is in CO 2 The characteristic that the solubility in the fluid is reduced along with the increase of the temperature continuously promotes the mass transfer and the separation of the crude oil of the grape seeds, and CO 2 The entrainment effect in the extraction kettle is increased along with the increase of the flow, and the materials and the supercritical CO in the extraction kettle can be enabled to be in circulation at the flow of the temperature-changing solvent-changing agent 2 The full contact, mixing, mass transfer and separation can improve the oil yield and extraction rate, improve the extraction efficiency, and save the production cost without increasing the pressure of an extraction kettle.
Further, the separation treatment conditions were set as follows: the treatment temperature of the separation I kettle is 60-65 ℃, and the pressure is 10-15MPa; the treatment temperature of the separation II kettle is 35-40 ℃, and the pressure is 5-10MPa.
Supercritical fluid extraction of CO 2 As a solvent, the method has the characteristics of no toxicity, no flammability, no corrosiveness, high purity and easy recycling, and compared with the common organic solvent extraction method, the supercritical fluid extract has no solvent residue, and simultaneously CO is used 2 The critical pressure and the critical temperature are mild, the extraction treatment is carried out at a lower pressure temperature, heat-sensitive substances are not affected, partial substances are not oxidized, harmful substances such as trans-fatty acid and grease polymer are not generated in the squeezing process to denature grease nutrient substances, and active substances in the squeezed oil are reserved.
The method is further set as follows: heating grape seed crude oil to 75-80 ℃, adding a citric acid solution with the mass fraction of 45-50% into the grape seed crude oil for acidification, adding a saline solution with the mass fraction of 0.5-1% into a mixed system obtained by acidification for hydration, and finally centrifuging for 15-20min under the condition of 3000-4000r/min to separate oil, colloid and water to obtain the grape seed degummed oil.
Further setting the adding amount of the citric acid solution to be 2.5-4% of the weight of the grape seed crude oil, and the adding amount of the salt water to be 5-8% of the weight of the grape seed crude oil; the acidification treatment was carried out as follows: stirring and mixing at the speed of 800-1000r/min for 5-10min, and stirring and mixing at the speed of 500-800r/min for 20-30min; the operation of the hydration treatment is as follows: stirring and mixing at 500-800r/min for 20-30min, and stirring at constant temperature and constant speed of 75-80 deg.C and 500-800r/min for 50-60min.
Degumming is carried out by adding water or dilute electrolyte solution into crude oil under stirring to make the impurity absorb water, expand, coagulate and separate. In the degumming process, the substances which can be coagulated and precipitated mainly comprise phospholipid, and in addition, protein, mucus, trace metal ions and the like which are combined with the phospholipid, and the final degumming rate can reach more than 25 percent.
It is further provided that the deacidification operation comprises the following steps: heating grape seed degummed oil to 40-45 ℃, adding 20-25% of sodium hydroxide solution by mass percent into the degummed oil to perform alkali refining, stirring at constant temperature for 40-60min, centrifuging, taking an upper oil phase, adding deionized water into the upper oil phase, heating to 50-80 ℃, washing with water for 50-80min, performing centrifugal separation after washing with water, and taking the obtained oil phase to obtain grape seed deacidified oil; the addition amount of the sodium hydroxide solution is 0.3-0.5% of the weight of the grape seed degummed oil, and the addition amount of the deionized water is 8-12% of the weight of the upper oil phase.
Deacidification refers to a process of removing free fatty acid in unrefined crude oil or degummed oil, the free fatty acid is saponified by alkali liquor to generate a large amount of soapstock, the deacidification efficiency is high, the deacidification rate is up to more than 99%, the national first-grade standard of edible oil is met, the process period is short, the generated byproduct soapstock can be used for other purposes (such as being processed into soap and the like), and the full utilization of resources is realized.
The method is further set to carry out water washing treatment under the high-low temperature interaction condition, and specifically comprises the following operations: adding deionized water into the upper oil phase, heating to 50-80 deg.C, washing with water for 20-30min, cooling to 20-30 deg.C, washing with water for 10-20min to remove precipitate, heating to 50-80 deg.C, washing with water for 15-20min, cooling to 0-10 deg.C, washing with water for 5-10min to remove precipitate.
The water washing treatment is carried out under the high-low temperature interaction condition, so that soapstock and other impurities formed by deacidification can be precipitated more quickly through the change of temperature, and the impurity content in the deacidified oil is further reduced; meanwhile, the continuous high temperature can accelerate the hydration phenomenon of the degummed oil, particularly, partial saponification of neutral oil is easily caused, too much soapstock generated by saponification can hinder the saponification of residual free fatty acid, so that the deacidification rate is reduced, the saponification of the neutral oil can be slowed down through intermittent low temperature under the high-low temperature interaction condition, the loss of the neutral oil is reduced, and the deacidification rate is improved.
The method is further configured to perform the decoloring operation as follows: heating grape seed deacidified oil to 85-90 deg.C, adding 3-4wt% decolorizer, stirring at constant temperature for 30-60min, and vacuum filtering to obtain grape seed decolorized oil; the decolorizing agent is activated carbon or activated clay.
The decolorization is a process of utilizing substances (such as activated clay, activated carbon and the like) with strong selective adsorption on pigments to adsorb the pigments and other impurities in the grease, thereby achieving decolorization. The deacidified oil treated by the decolorant not only achieves the purposes of improving the oil color and removing colloid, but also can further effectively remove some trace metal ions and harmful substances in the deacidified oil, thereby providing good conditions for subsequent deodorization.
It is further provided that the deodorizing operation comprises the steps of: deodorizing grape seed decolorized oil at 225-235 deg.C under vacuum degree of 0.098MPa for 1.5-2 hr to obtain grape seed oil product.
Deodorization is a process of removing odor substances by steam distillation under the conditions of high temperature and high vacuum by utilizing the volatility difference of odor substances and fatty acid in grease. The steam is contacted with the liquid-vapor surface through the grease containing the odor component, and the steam is saturated by the volatile odor component and escapes according to the ratio of partial pressure of the volatile odor component, thereby achieving the purpose of removing the odor component.
In a second aspect, the invention provides a grape seed oil product, which is prepared by the method for preparing grape seed oil by using grape seeds; the acid value of the grape seed oil product is less than or equal to 0.66mg/g, and the vitamin E content of the grape seed oil product is 40-50mg/100g. The grape seed oil has the advantages of good quality, clear and transparent appearance, fragrant and pure smell, low impurity content, high stability, more active nutrient components, lower content of heavy metal elements such as copper, iron and the like than the national edible oil quality detection standard, and long shelf life.
The method for preparing grape seed oil by utilizing grape seeds and the product thereof provided by the invention realize the following beneficial effects by means of matching the supercritical fluid extraction and the refining process:
1) When the method is used for preparing the grape seed oil, the oil yield is over 15 percent, the extraction rate is over 95 percent, the extraction time is short, no solvent residue exists, the extraction efficiency and the yield of the grape seed oil are improved, the environmental pollution is low, and the problems of low extraction efficiency, low yield and low product quality in the prior art are solved.
2) According to the invention, water-soluble and fat-soluble harmful impurities in the crude oil are effectively removed through a refining process, the grape seed oil has high degumming rate, deacidification rate, decoloration rate and the like, active nutritional ingredients in the grape seed oil are retained to the maximum extent, the problem of loss of part of nutritional active ingredients in the refining process in the prior art is solved, the quality of the grape seed oil is improved, the quality and taste of oil are improved, the safety of the grape seed oil is ensured, and the quality guarantee period is prolonged.
3) The grape seed oil prepared by the invention has good quality, is clear and transparent, has fragrant and pure smell, low impurity content and high stability, the heavy metal elements such as copper, iron and the like are lower than the national edible oil quality detection standard, the quality guarantee period is long, the grape seed oil can be directly eaten as high-end health care oil, and nutrient substances with the effects of oxidation resistance, aging resistance, inflammation resistance and the like which are rich in the grape seed oil can be used as cosmetic additives in other fields such as the cosmetic industry and the like.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and those skilled in the art can also obtain other drawings according to the drawings without creative efforts.
FIG. 1 shows the measurement results of the influence of different methods on the oil yield, extraction rate and deacidification rate of grape seeds;
fig. 2 shows the results of measurements of the effect of different methods on the oxidative stability of the grapeseed oil product.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are a part of the embodiments of the present invention, but not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art based on the embodiments of the present invention without any inventive step, also belong to the scope of protection of the present invention.
In a specific embodiment, the method for preparing grape seed oil by using grape seeds comprises the following steps:
1) And (3) extraction: crushing grape seeds by a crusher to 60-80 meshes, and then sending the obtained grape seed powder into an extraction instrument for extraction treatment and separation treatment to obtain crude grape seed oil. The extraction conditions were as follows: the pressure of the extraction kettle is 25-35MPa, the temperature is 40-50 ℃, and CO is added 2 The flow rate is 15-20L/h, and the single extraction time is 2-3h. The separation treatment conditions were as follows: the treatment temperature of the separation I kettle is 60-65 ℃, and the pressure is 10-15MPa; the treatment temperature of the separation II kettle is 35-40 ℃, and the pressure is 5-10MPa.
In the specific embodiment, the extraction apparatus adopts HA220-35-200 type supercritical CO 2 A fluid extraction apparatus.
In a specific embodiment, the extraction treatment is performed under the condition of constant-pressure and variable-temperature solvent flow circulation, and the specific operations are as follows: under the condition of constant pressure of the extraction kettle, the temperature is 40-45 ℃ and CO is added 2 Extracting at flow rate of 15-18L/h for 0.5-1h, and then extracting at 45-50 deg.C with CO 2 Extracting at flow rate of 18-20L/h for 0.5-1h, and extracting at 40-45 deg.C with CO 2 The extraction is carried out for 0.5 to 1 hour under the condition of the flow rate of 15 to 18L/hour, and the extraction is circulated to the end of the extraction in the way.
2) Degumming: heating grape seed crude oil to 75-80 ℃, adding citric acid solution with the weight percentage of 45-50% and the weight percentage of 2.5-4% of the grape seed crude oil, stirring and mixing for 5-10min at the speed of 800-1000r/min, stirring and mixing for 20-30min at the speed of 500-800r/min for acidification, adding table salt water with the weight percentage of 5-8% of the grape seed crude oil and the weight percentage of 0.5-1% into a mixed system obtained by acidification, stirring and mixing for 20-30min at the speed of 500-800r/min, stirring for 50-60min at constant temperature and constant speed of 500-800r/min at the temperature of 75-80 ℃ for hydration treatment, and finally centrifuging for 15-20min at the speed of 3000-4000r/min for separating oil, colloid and water to obtain the grape seed degummed oil.
3) Deacidifying: heating grape seed degummed oil to 40-45 ℃, adding sodium hydroxide solution with the weight of 0.3-0.5% of the grape seed degummed oil and the mass fraction of 20-25% into the degummed oil for alkali refining, stirring the mixture at constant temperature for 40-60min, centrifuging the mixture, taking an upper oil phase, adding deionized water with the weight of 8-12% of the upper oil phase into the upper oil phase, heating the mixture to 50-80 ℃, washing the mixture for 50-80min, performing centrifugal separation after washing the mixture, and taking the obtained oil phase to obtain the grape seed deacidified oil.
In a specific embodiment, the water washing treatment is performed under the high-low temperature interaction condition, and the specific operations are as follows: adding deionized water into the upper oil phase, heating to 50-80 deg.C, washing with water for 20-30min, cooling to 20-30 deg.C, washing with water for 10-20min to remove precipitate, heating to 50-80 deg.C, washing with water for 15-20min, cooling to 0-10 deg.C, washing with water for 5-10min to remove precipitate.
4) And (3) decoloring: heating grape seed deacidified oil to 85-90 deg.C, adding 3-4wt% decolorizer, stirring at constant temperature for 30-60min, and vacuum filtering to obtain grape seed decolorized oil. The decolorizing agent is activated carbon or activated clay.
As a preferred embodiment, the decolorizing agent is activated carbon. In the method, the activated carbon is preferably used as the decoloring agent, because the selling price of the activated carbon is lower than that of activated clay, the activated carbon can be recycled after being cleaned, the production cost is favorably reduced, and the integral decoloring effect of the activated carbon on the chlorophyll a and the chlorophyll b is better than that of the activated clay, so that the activated carbon is selected as the decoloring agent, and the decoloring rate of the activated carbon can reach over 74 percent by taking the removal rate of the chlorophyll b as a detection index.
As a further improvement to the previous implementation, the grape seed deacidified oil is added with 1wt% of vitamin protective agent before being heated, and the vitamin protective agent is a mixture of alpha-terpineol and ethyl maltol in a weight ratio of 1.
The vitamin protective agent is added before the decolorant, bonding can be formed between the active group of the vitamin protective agent and fat-soluble vitamins by synergistically utilizing the active group of the vitamin protective agent and the fat-soluble vitamins, so that the active site where the vitamins and the decolorant are combined is occupied by the protective agent, the adsorption of the decolorant on the vitamins is reduced, the unique flavors of various fat-soluble nutrient components such as VE and VK in oil are retained to the maximum extent, the loss of the vitamins in the decoloring process is reduced, the oxidation stability and the quality of the grape seed oil are further improved by utilizing the oxidation resistance of the vitamins, the quality guarantee period of the grape seed oil is prolonged, the protective agent can volatilize without residue in a high-temperature deodorization link, and the flavor of the grape seed oil and the like cannot be negatively influenced.
5) Deodorizing: deodorizing grape seed decolorized oil at 225-235 deg.C under vacuum degree of 0.098MPa for 1.5-2 hr to obtain grape seed oil product.
The present invention will be described in further detail with reference to examples.
Example 1:
a method for preparing grape seed oil by using grape seeds comprises the following steps:
1) And (3) extraction: pulverizing grape seed with pulverizer, sieving with 60 mesh sieve, and feeding the obtained grape seed powder into HA220-35-200 type supercritical CO 2 And carrying out extraction treatment and separation treatment in a fluid extraction instrument to obtain the crude grape seed oil. The separation treatment conditions were as follows: the treatment temperature of the separation I kettle is 62 ℃, and the pressure is 12MPa; the treatment temperature of the separation II kettle is 36 ℃, and the pressure is 6MPa.
The extraction treatment is carried out under the condition of constant pressure and variable temperature and variable solvent flow circulation, and the specific operation is as follows: under the condition of constant pressure of 30MPa in the extraction kettle, the temperature is 42 ℃ and CO is added 2 Extracting at 16L/h for 1h, and then extracting at 48 deg.C with CO 2 Extracting at flow rate of 20L/h for 1 hr, and extracting with CO at 42 deg.C 2 The extraction is carried out for 1h under the condition of the flow rate of 16L/h, and the circulation is carried out until the extraction is finished in this way, and the single extraction time is 3h.
2) Degumming: heating grape seed crude oil to 80 ℃, adding a citric acid solution with 3% of the weight of the grape seed crude oil and 50% of the mass fraction into the grape seed crude oil, stirring and mixing the grape seed crude oil for 5min at the speed of 1000r/min, then stirring and mixing the grape seed crude oil for 20min at the speed of 500r/min for acidification, then adding a salt water with 7% of the weight of the grape seed crude oil and 0.5% of the mass fraction into a mixed system obtained by acidification, stirring and mixing the grape seed crude oil for 20min at the speed of 600r/min, then stirring the grape seed crude oil for 50min at constant temperature and constant speed at the temperature of 80 ℃ and the speed of 600r/min for hydration, and finally centrifuging the grape seed degummed oil for 15min at the speed of 4000r/min to separate grease, colloid and water, thus obtaining the grape seed degummed oil.
3) Deacidifying: heating grape seed degummed oil to 40 ℃, adding a sodium hydroxide solution with the mass fraction of 24 percent and the weight of 0.3 percent of that of the grape seed degummed oil into the grape seed degummed oil for alkali refining, stirring the mixture for 45min at constant temperature, centrifuging the mixture, taking an upper oil phase, adding deionized water with the weight of 10 percent of that of the upper oil phase into the upper oil phase, washing the mixture for 60min, performing centrifugal separation after washing, and taking the obtained oil phase to obtain the grape seed deacidified oil.
The washing treatment is carried out under the condition of high-temperature and low-temperature interaction, and the specific operations are as follows: adding deionized water into the upper oil phase, heating to 60 deg.C, washing with water for 20min, cooling to 20 deg.C, washing with water for 10min to remove precipitate, heating to 60 deg.C, washing with water for 20min, cooling to 5 deg.C, washing with water for 10min to remove precipitate.
4) And (3) decoloring: heating grape seed deacidified oil to 90 deg.C, adding 3wt% decolorizer, stirring at constant temperature for 50min, and vacuum filtering to obtain grape seed decolorized oil. The decolorizing agent is activated carbon.
5) Deodorizing: deodorizing grape seed decolorized oil at 230 deg.C and vacuum degree of 0.098MPa for 2 hr to obtain grape seed oil product.
The physical and chemical properties of the grape seed crude oil and the grape seed oil obtained in example 1 were measured according to the specifications of GB/T22478-2008, and the results are shown in table 1 below.
TABLE 1 measurement results of physical and chemical properties of crude and seed oil products of grape seeds
The fatty acid contents of the crude grape seed oil and the grape seed oil obtained in example 1 were measured by the normalization method in GB/T5009.168-2016, and the results are shown in Table 2 below.
TABLE 2 determination of fatty acid content of crude and seed oil products from grape seeds
The results show that the fatty acids in the grapeseed oil product are mainly linoleic acid, oleic acid and palmitic acid, and the content of various fatty acids after refining has not been changed significantly.
The mineral element contents of the grape seed crude oil and the grape seed oil obtained in example 1 were measured with reference to GB/T5009.91-2017 for potassium and sodium, GB/T5009.90-2016 for iron, GB/T5009.241-2017 for magnesium, GB/T5009.242-2017 for manganese, GB/T5009.13-2017 for copper, GB/T5009.14-2017 for zinc, and GB/T5009.92-2016 for calcium, and the results are shown in table 3 below.
TABLE 3 determination of mineral content of crude and seed oil products from grape seeds
| Mineral elements | Grape seed crude oil mg/100g | Grape seed oil product mg/100g |
| Copper (Cu) | 1.44 | Undetected |
| Zinc | 0.382 | 0.37 |
| Iron | 0.63 | 0.49 |
| Magnesium alloy | 0.18 | 0.17 |
| Manganese oxide | 0.071 | Not detected out |
| Potassium salt | 6.33 | 6.34 |
| Sodium salt | 0.26 | 0.58 |
| Calcium carbonate | 0.15 | 0.14 |
The result shows that the grape seed oil product contains various trace elements, the refining has no significant influence on the content of each trace element, the refining can obviously reduce the content of heavy metal elements such as manganese and copper, and the heavy metal elements cannot be detected in the refined grape seed oil product, so that the grape seed oil product has high nutritional value and safety.
Example 2:
a method of preparing grape seed oil from grape seeds, repeating the steps of example 1, except that:
in the extraction of the step 1), the extraction treatment is carried out under the condition of constant pressure, constant temperature and constant solvent flow circulation, and the specific operation is as follows: under the condition that the pressure of the extraction kettle is constant at 30MPa, the temperature is 42 ℃ and CO is generated 2 Flow rateThe extraction is carried out for 3h under the condition of 20L/h.
In the step 3), during deacidification, washing treatment is carried out under a constant temperature condition, and the specific operation is as follows: adding deionized water into the upper oil phase, heating to 60 deg.C, washing with water for 60min, removing precipitate, centrifuging, and collecting the oil phase to obtain grape seed deacidified oil.
Example 3:
a method of preparing grape seed oil from grape seeds, repeating the steps of example 1, except that:
the specific steps of the decolorization in the step 4) are as follows: taking deacidified grape seed oil, adding 1wt% of vitamin protective agent, mixing well, heating to 90 deg.C, adding 3wt% of decolorizing agent, stirring at constant temperature for 50min, and vacuum filtering to obtain grape seed decolorized oil. The decolorant is activated carbon, and the vitamin protective agent is a mixture of alpha-terpineol and ethyl maltol in a weight ratio of 1-2.
Example 4:
a method of preparing grape seed oil from grape seeds, repeating the steps of example 1, except that:
the specific steps of the decolorization in the step 4) are as follows: taking deacidified grape seed oil, adding 1wt% of vitamin protective agent, mixing well, heating to 90 deg.C, adding 3wt% of decolorizing agent, stirring at constant temperature for 50min, and vacuum filtering to obtain grape seed decolorized oil. The decolorizing agent is activated carbon, and the vitamin protective agent is alpha-terpineol.
Example 5:
a process for preparing grape seed oil from grape seeds, the procedure of example 1 was repeated except that:
the specific steps of the decolorization in the step 4) are as follows: taking deacidified grape seed oil, adding 1wt% of vitamin protective agent, mixing well, heating to 90 deg.C, adding 3wt% of decolorizing agent, stirring at constant temperature for 50min, and vacuum filtering to obtain grape seed decolorized oil. The decolorizing agent is activated carbon, and the vitamin protective agent is ethyl maltol.
Test example 1:
influence of different methods on oil yield, extraction rate and deacidification rate of grape seeds
The test method comprises the following steps: the same batch of grape seeds, 100g, was treated according to the methods of example 1 and example 2, respectively, and the oil content, oil yield and extraction rate of the grape seeds were measured, and the deacidification rate was measured after the deacidification step was performed. The oil content determination method comprises the following steps: according to GB/T5009.6-2003, a Soxhlet extraction method is adopted. The oil yield calculation method comprises the following steps: grape seed oil yield (%) = grape seed crude oil quality/grape seed quality × 100. The extraction rate calculation method comprises the following steps: grape seed oil extraction rate (%) = grape seed crude oil mass/(grape seed mass × grape seed oil content) × 100. The deacidification rate calculation method comprises the following steps: deacidification rate (%) = (grape seed crude oleic acid value-deacidification oleic acid value)/grape seed crude oleic acid value x 100, and the acid value determination is referred to GB5009.229-2016. Each example was provided with 3 replicates and averaged. The results are shown in FIG. 1.
FIG. 1 shows the measurement results of the influence of different methods on the oil yield, extraction rate and deacidification rate of grape seeds. As shown in the figure, in example 1, the oil content of grape seeds was 16.59%, the oil yield was 15.78%, the extraction rate was 95.12%, and the deacidification rate was 99.8%, and in example 2, the oil content of grape seeds was 16.42%, the oil yield was 14.31%, the extraction rate was 87.15%, and the deacidification rate was 98.2%. The comparison shows that the oil yield, the extraction rate and the deacidification rate obtained by the method in the embodiment 1 are all significantly higher than those of the method in the embodiment 2, which illustrates that the extraction treatment of the grape seeds in the embodiment 1 by adopting a constant-pressure variable-temperature variable-solvent flow circulation mode can significantly improve the oil yield and the extraction rate of the grape seeds, improve the extraction efficiency and facilitate the improvement of the resource utilization rate, and meanwhile, the water washing treatment in the embodiment 1 under the high-low temperature interaction condition can further reduce the impurity content in the deacidification oil, slow down the saponification of the neutral oil through the intermittent low temperature, reduce the loss of the neutral oil and improve the deacidification rate.
Test example 2:
effect of different methods on grape seed oil nutrient composition and oxidative stability
The test method comprises the following steps: the same batch of grape seeds was treated by 100g according to the methods of example 1 and examples 3 to 5, respectively, and the deacidified grape seed oil and the decolorized grape seed oil before and after the decolorization step were sampled, and the vitamin contents thereof were measured, respectively, and the oxidation stability of the grape seed oil products obtained in the examples was measured. The method for measuring the vitamin content comprises the following steps: accurately weighing 0.2g of grape seed oil product, dissolving with diethyl ether (removing aldehyde), diluting to a constant volume of 10mL, performing ultrasonic treatment for 5min, filtering with 0.22 μm filter membrane, analyzing vitamin composition and content with Agilent Technologies 1200 high performance liquid chromatograph, and quantifying by external standard method. The oxidation stability determination method comprises the following steps: respectively containing the grape seed oil products in beakers by a Schaal oven method, placing the beakers in a constant-temperature drying box at 63 ℃ with an opening for accelerating oxidation, and measuring the peroxide value of a sample by taking 1d as a unit and taking 20d as 1 period. Each example was provided with 3 replicates and averaged. The results are shown in Table 4 and FIG. 2.
TABLE 4 determination of vitamin content in grape seed oil by various methods (unit: mg/100 g)
| Before decolorization | Example 1 | Example 3 | Example 4 | Example 5 | |
| VA | 8.621 | 8.641 | 8.643 | 8.634 | 8.637 |
| VD | 4.562 | 4.368 | 4.479 | 4.512 | 4.365 |
| VE | 66.183 | 43.152 | 48.654 | 43.654 | 43.059 |
| VK | 57.544 | 29.514 | 33.641 | 29.547 | 30.657 |
The results show that the content of vitamin A and D in the grape seed oil before and after the decolorization step is not obviously changed, and the content of vitamin E and K is obviously reduced. The loss of the vitamin E and K content before and after the decoloring step in the example 3 is minimum, the loss of the vitamin E and K content in the example 1 is maximum, and the difference between the example 4 and the example 5 and the example 1 is smaller, which shows that the vitamin protective agent added in the example 3 can play a synergistic effect, so that the decoloring agent reduces the adsorption of the vitamin, the unique flavors of various fat-soluble nutrient components such as VE and VK in the grease are retained to the maximum extent, and the loss of the vitamin in the decoloring process is reduced.
Fig. 2 shows the results of measurements of the effect of different methods on the oxidative stability of the grapeseed oil product. The results show that the peroxide value of the grape seed crude oil is increased most rapidly in the accelerated oxidation process, and the peroxide value of the grape seed crude oil is increased at a speed which is obviously lower than that of the grape seed crude oil in examples 1 and 3-5, which shows that the oxidation stability and the quality of the grape seed oil can be obviously improved by the refining process. The change trend of the peroxide values of the comparative example 1, the example 3 and the example 5 is found to be the slowest in the increase trend of the peroxide value of the example 3, which is significantly lower than the increase trend of the peroxide values of the example 1, the example 4 and the example 5, and the results of the table 4 show that the vitamin protective agent added in the example 3 can exert a synergistic effect, so that the loss of the vitamins in the decoloring process is reduced, and further the oxidation stability and the quality of the grape seed oil are improved by utilizing the oxidation resistance of the vitamins, and the shelf life of the grape seed oil is prolonged.
It should be noted that, in the present invention, concentrations, ratios, and the like which are not specifically described are weight concentrations, weight ratios, and the like, which belong to the common writing habits of those skilled in the art, and therefore, are not described in detail herein.
It should be noted that, in the present invention, the detailed steps of some operations are not detailed, but belong to the prior art known to those skilled in the art, and therefore, are not described herein again.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the same; while the invention has been described in detail and with reference to the foregoing embodiments, those skilled in the art will appreciate that; the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. A method for preparing grape seed oil by using grape seeds is characterized by comprising the following steps:
carrying out extraction treatment and separation treatment on grape seeds by using an extractor to obtain crude grape seed oil;
carrying out degumming operation on the grape seed crude oil through acidification treatment and hydration treatment to obtain grape seed degummed oil;
performing alkali refining treatment and water washing treatment on the grape seed degummed oil to complete deacidification operation to obtain grape seed deacidified oil;
carrying out decoloring operation on the grape seed deacidified oil by using a decoloring agent to obtain grape seed decolored oil; and the number of the first and second groups,
deodorizing the grape seed decolorized oil to obtain a grape seed oil product;
the extraction instrument adopts supercritical CO 2 The fluid extractor, the extraction processing conditions are as follows: the pressure of the extraction kettle is 25-35MPa, the temperature is 40-50 ℃, and CO is added 2 The flow rate is 15-20L/h, and the single extraction time is 2-3h.
2. The method for preparing grape seed oil from grape seeds as claimed in claim 1, wherein the extraction treatment is performed under the condition of constant pressure and temperature variable solvent flow circulation, and the specific operations are as follows: under the condition of constant pressure of the extraction kettle, the temperature is 40-45 ℃ and CO is added 2 Extracting at flow rate of 15-18L/h for 0.5-1h, and extracting at 45-50 deg.C with CO 2 Extracting at flow rate of 18-20L/h for 0.5-1h, and then extracting at 40-45 deg.C with CO 2 The extraction is carried out for 0.5 to 1 hour at a flow rate of 15 to 18L/hour, and the extraction is circulated to the end of the extraction in the way.
3. The method for preparing grape seed oil from grape seeds as claimed in claim 1, wherein the separation process conditions are as follows: the treatment temperature of the separation I kettle is 60-65 ℃, and the pressure is 10-15MPa; the treatment temperature of the separation II kettle is 35-40 ℃, and the pressure is 5-10MPa.
4. The method for preparing grape seed oil from grape seeds as claimed in claim 1, wherein the degumming operation comprises the following steps: heating grape seed crude oil to 75-80 ℃, adding a citric acid solution with the mass fraction of 45-50% into the grape seed crude oil for acidification, adding a saline solution with the mass fraction of 0.5-1% into a mixed system obtained by acidification for hydration, and finally centrifuging for 15-20min under the condition of 3000-4000r/min to separate oil, colloid and water to obtain the grape seed degummed oil.
5. The method for preparing grape seed oil from grape seeds according to claim 4, wherein the citric acid solution is added in an amount of 2.5-4% of the weight of the grape seed crude oil, and the saline solution is added in an amount of 5-8% of the weight of the grape seed crude oil;
the acidification treatment is carried out as follows: stirring and mixing at 800-1000r/min for 5-10min, and stirring and mixing at 500-800r/min for 20-30min;
the operation of the hydration treatment is as follows: stirring and mixing at 500-800r/min for 20-30min, and stirring at constant temperature and constant speed of 75-80 deg.C and 500-800r/min for 50-60min.
6. The method for preparing grape seed oil from grape seeds as claimed in claim 1, wherein the deacidification operation comprises the following steps: heating grape seed degummed oil to 40-45 ℃, adding 20-25% by mass of sodium hydroxide solution into the degummed oil to perform alkali refining, stirring at constant temperature for 40-60min, centrifuging, taking an upper oil phase, adding deionized water into the upper oil phase, heating to 50-80 ℃, washing for 50-80min, washing, performing centrifugal separation, taking the obtained oil phase, and thus obtaining grape seed deacidified oil;
the addition amount of the sodium hydroxide solution is 0.3-0.5% of the weight of the grape seed degummed oil, and the addition amount of the deionized water is 8-12% of the weight of the upper oil phase.
7. The method for preparing grape seed oil from grape seeds according to claim 1 or 6, wherein the water washing treatment is performed under the high-low temperature interaction condition, and the specific operations are as follows: adding deionized water into the upper oil phase, heating to 50-80 deg.C, washing with water for 20-30min, cooling to 20-30 deg.C, washing with water for 10-20min to remove precipitate, heating to 50-80 deg.C, washing with water for 15-20min, cooling to 0-10 deg.C, washing with water for 5-10min to remove precipitate.
8. The method for preparing grape seed oil from grape seeds as claimed in claim 1, wherein the decolorization operation comprises the following steps: heating grape seed deacidified oil to 85-90 deg.C, adding 3-4wt% decolorizer, stirring at constant temperature for 30-60min, and vacuum filtering to obtain grape seed decolorized oil; the decolorant is active carbon or active clay.
9. The method for preparing grape seed oil from grape seeds of claim 1, wherein the deodorization operation comprises the following steps: deodorizing grape seed decolorized oil at 225-235 deg.C under vacuum degree of 0.098MPa for 1.5-2 hr to obtain grape seed oil product.
10. A grape seed oil product, which is prepared by the method for preparing the grape seed oil by using the grape seeds as claimed in any one of claims 1 to 9; the acid value of the grape seed oil product is less than or equal to 0.66mg/g, and the vitamin E content of the grape seed oil product is 40-50mg/100g.
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