CN114874837A - Method for preparing walnut oil by aqueous enzymatic method - Google Patents
Method for preparing walnut oil by aqueous enzymatic method Download PDFInfo
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- CN114874837A CN114874837A CN202210322677.1A CN202210322677A CN114874837A CN 114874837 A CN114874837 A CN 114874837A CN 202210322677 A CN202210322677 A CN 202210322677A CN 114874837 A CN114874837 A CN 114874837A
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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
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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
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/02—Pretreatment
- C11B1/04—Pretreatment of vegetable raw material
-
- 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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- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/74—Recovery of fats, fatty oils, fatty acids or other fatty substances, e.g. lanolin or waxes
Abstract
The invention relates to the technical field of food, in particular to a method for preparing walnut oil by an aqueous enzymatic method, which comprises the steps of crushing pretreated walnut kernels under the condition of not adding water, wherein the particle size of the crushed walnut kernels is less than or equal to 900 micrometers; adding water into the crushed walnut kernels to prepare walnut pulp; carrying out enzymolysis on the walnut pulp by using an aqueous enzymatic method; the method provided by the invention greatly improves the enzymolysis efficiency, and the final oil yield is up to more than 70%.
Description
Technical Field
The invention relates to the technical field of food, in particular to a method for preparing walnut oil by an aqueous enzymatic method.
Background
At present, the common methods in the current walnut oil production mainly comprise:
(1) and (3) squeezing: is the most common walnut oil production method at present, and is also a mature walnut oil extraction method. The method mainly utilizes a mechanical squeezing principle to extrude grease in raw materials at one time. Typically, the machines used include screw and hydraulic oil presses. The walnut protein denaturation temperature is 67.5 ℃, and the mechanical pressing can be divided into cold pressing and hot pressing according to the walnut protein denaturation degree. Generally, the hot pressing method uses a screw type oil press; the cold pressing method uses a hydraulic oil press. Cold pressing, namely pressing the oil material at the temperature of 60 ℃ by using a physical pressing method, and completely retaining the nutrient elements in the oil material. The links such as crushing, steaming and frying in the hot pressing process are reduced. The squeezed edible oil can reach the national third-level edible oil standard. Hot pressing, namely pressing the materials at a high temperature of 120-130 ℃ by using a physical pressing method, wherein the oil yield is high, the oil needs to be crushed, softened, rolled, steamed and fried, the pressed crude oil needs to be refined, and the equipment is complex. The defects that the hot pressing method requires high-temperature baking and has high energy consumption, and the hot pressing adopts a screw oil press, so that although the working efficiency is high, in order to increase the frictional resistance during pressing, walnut shells need to be introduced, which is not beneficial to the reutilization of walnut meal; the cold pressing method has no such drawbacks, but the oil yield is low.
(2) Preparing oil by a leaching method: the method is an oil preparation method which applies the extraction principle, selects a certain organic solvent capable of dissolving oil and fat, and makes the organic solvent contact with the pretreated oil to be soaked or sprayed, so that the oil and fat in the oil are dissolved. This method makes a solution of the solvent and the oil or fat dissolved therein called a mixed oil. And (3) evaporating and stripping the mixed oil by utilizing the different boiling points of the selected solvent and the grease, evaporating the solvent, and leaving the grease to obtain crude oil. The solvent vapor is condensed and recovered for recycling. Leaching is generally carried out by soaking the raw material with solvent oil (light gasoline number six) and sucking out the oil in the raw material. And then heating the mixed oil to 240-260 ℃, evaporating the light gasoline to leave crude oil, and refining the crude oil into the edible oil by six processes of degreasing, degumming, dehydrating, decoloring, deodorizing and deacidifying. The residue in the first-grade and second-grade edible oil is not more than 10 mg/kg according to national regulations; the residue of the third and fourth grade edible oil is not more than 50 mg/kg.
(3) Supercritical CO 2 An extraction method comprises the following steps: has the advantages of high extraction efficiency, no solvent residual toxicity, no easy decomposition and damage of natural active ingredients and thermosensitive ingredients, capability of maintaining the natural characteristics of the extract to the maximum extent, capability of realizing selective separation, and the like. In the extraction of edible oils, there has been much room for improvement in the extraction of vegetable oils, since the extraction by general methods may cause the dissipation and oxidation of active ingredients in plants. But the equipment has larger one-time investment and higher energy consumption.
(4) Water substitution method: is a method for obtaining grease by replacing oil with water from oil. Without pressing out, without solvent extraction, relying on the condition that water has a greater affinity for protein than oil, so that water enters the oil to displace the oil. Can be used for preparing oleum Sesami, or oil with high oil content such as semen Arachidis Hypogaeae, tea seed, and semen Helianthi.
The prior art discloses a method for efficiently processing walnut oil, which adopts the processes of pretreatment, enzymolysis, fermentation, secondary cooking, squeezing and the like. The application needs to simultaneously use enzymolysis and fermentation, and also needs to carry out secondary cooking, and finally, the walnut oil is obtained by squeezing, the process flow is complex, the operation cost is higher, the manufacturing period is longer, and the method is still a squeezing method for preparing the walnut oil in essence.
The prior art discloses a method for preparing hickory oil by an aqueous enzymatic method, wherein the water content of walnuts is 5.0-5.5 percent, the walnuts are not peeled, water is added after the walnuts are crushed to fix the volume, secondary enzymolysis is carried out, the pH is adjusted, and the highest oil yield is 71.2 percent. The application has certain requirement on the water content of the walnut kernel, and the walnut kernel is not peeled, so that the taste and the color of the walnut oil are influenced to a certain extent.
The prior art discloses a method for extracting hickory oil by using water enzyme, which adopts a hydrocolloid mill, regulates the pH after constant volume, and obtains the hickory oil by performing enzymolysis once by cellulase and twice by papain and centrifuging. The enzymolysis time is 3-8 h. The application needs two times of centrifugal enzymolysis, and the enzymolysis time is as long as 8 hours.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to overcome the defects of various steps and low oil yield in the prior art, and thus, the method for preparing the walnut oil by the aqueous enzymatic method is provided.
The study shows that part of walnut oil exists between walnut cells, and the other part of walnut oil exists in the walnut cells. In order to release the walnut oil, the walnut oil needs to be crushed, so that the walnut oil can be released preliminarily; on the other hand, the particle size of the walnut is reduced, and the specific surface area is increased, so that the contact of the enzyme and the walnut is increased. According to the invention, by using an aqueous enzymatic method, enzyme and walnut slurry are uniformly mixed, then enzymolysis is carried out at a certain temperature, and the walnut oil is obtained by centrifugation.
The invention adopts the peeled walnut kernels, and the water content can be realized within 1-30 percent. By crushing the walnut kernels to a proper particle size under the condition of not adding water, the emulsification effect can be weakened, the oil yield can be improved, and the oil yield can reach more than 70 percent by adopting the method provided by the invention.
A method for preparing walnut oil by an aqueous enzymatic method specifically comprises the following steps:
crushing the pretreated walnut kernels under the condition of not adding water, wherein the particle size of the crushed walnut kernels is less than or equal to 900 microns; adding water into the crushed walnut kernels to prepare walnut pulp; carrying out enzymolysis on the walnut pulp by using an aqueous enzymatic method; and separating the walnut pulp after enzymolysis to obtain the walnut oil.
When the walnut kernel is ground, no water is added, so that the contact of the walnut kernel with water in the crushing process can be reduced, and the defatting rate of walnut milk can be improved.
Preferably, the water content of the pretreated walnut kernels is 1-30%.
Preferably, the mass ratio of the crushed walnut kernels to the water is 1: 2-1: 5.
Preferably, the enzymatic hydrolysis of the walnut pulp by using the aqueous enzymatic method specifically comprises: heating the walnut pulp to 45-55 ℃, adding protease, stirring and mixing, wherein the addition amount of the protease is 2-5 per mill of the mass of the walnut kernel by the mass of the walnut kernel, and reacting for 2-3 h to obtain the walnut pulp after enzymolysis.
Preferably, the protease includes at least one of alkaline protease, neutral protease and papain.
The invention only needs one step reaction enzymolysis, and has higher reaction efficiency and short reaction time.
Preferably, the separation specifically comprises: centrifuging the walnut pulp subjected to enzymolysis, wherein the centrifugation conditions are as follows: centrifuging for 5-15 min under the condition of 6000-10000 r/min.
Preferably, the pretreated walnut kernels comprise: selecting walnut kernels and peeling the walnut kernels:
the walnut kernel selection steps specifically comprise: selecting walnut kernels which are free from mildew, oil and rancid, insect pests and impurities and have full grains;
and/or the peeling step of the walnut kernels specifically comprises the following steps: peeling semen Juglandis by alkali cooking process, and washing with water;
the walnut raw material with certain water content is obtained by peeling.
And/or, the soda boiling process comprises: preparing an alkaline water solution with the mass concentration of 2-6 per mill, adding the walnut kernels after boiling, timing for 1-25 min, and washing the walnut kernels after alkaline boiling with water to finish the peeling process.
Preferably, the method also comprises a walnut oil refining step, and specifically comprises the following steps:
carrying out hydration degumming treatment on the walnut oil to obtain hydration degummed walnut oil; dehydrating the walnut oil after hydration and degumming to obtain dehydrated walnut oil; decolorizing the dehydrated walnut oil, and filtering to obtain decolorized walnut oil; deodorizing the decolorized walnut oil to obtain refined walnut oil.
Preferably, the hydration degumming treatment specifically comprises: heating the walnut oil to 50-70 ℃, stirring at 30-100 r/min, and standing for 2-4 hours to obtain hydrated degummed walnut oil;
the invention adopts the aqueous enzymatic method, and the walnut oil obtained after centrifugation contains water, so that the hydration degumming can be directly carried out.
And/or the dehydration treatment specifically comprises: keeping the vacuum degree above 90kPa, heating the hydration degummed walnut oil to 60-80 ℃, reducing the water content in the hydration degummed walnut oil to below 0.11 percent to obtain the dehydrated walnut oil, and the fog in the decoloring pot disappears to show that the dehydration requirement is met.
And/or the decoloring treatment specifically comprises the following steps: controlling the oil temperature of the dehydrated walnut oil at 50-70 ℃, adding a decoloring agent, wherein the addition amount of the decoloring agent is 3-5% of the weight of the dehydrated walnut oil, decoloring for 30min, quickly cooling the oil temperature to be below 40 ℃ after decoloring, and separating the decoloring agent by using a filter to obtain the decolored walnut oil.
Preferably, the decolorizing agent comprises activated clay.
The deodorization treatment specifically comprises: the oil temperature is kept at 170-180 ℃ during deodorization, the vacuum degree is kept above 90kPa, and the deodorization time is 3-5 h.
Preferably, the method further comprises the following steps: and (4) filling nitrogen after the walnut oil refining step to obtain the filled walnut oil.
The technical scheme of the invention has the following advantages:
(1) the walnut kernel is crushed under the anhydrous condition. The walnut kernel is crushed to a proper particle size, so that the walnut kernel has a better crushing effect, walnut oil existing between cells of the walnut can be released, and the walnut oil existing in the cells of the walnut can be released together. Meanwhile, because the method is carried out under the anhydrous condition, water is not introduced in the crushing process, the contact between the water and the walnut oil in the crushing process is reduced, the walnut oil is prevented from being emulsified by the water as far as possible, the specific surface area can be increased by reducing the granularity of the walnut through crushing, so that the contact between the enzyme and the walnut is increased, and the enzymolysis efficiency is improved.
If the walnut kernel is crushed by adding water, the oil yield is low; if the walnut kernel is crushed without adding water, the content of the crushed walnut kernel can reach more than 70 percent under the same process conditions.
(2) The invention adopts an aqueous enzymatic method, and has low requirement on the moisture of the walnut kernels. For example, the walnut oil prepared by a squeezing method needs the water content of walnut kernels to be lower than 5 percent; the water content of the walnut oil by the aqueous enzymatic method can be in a large range, such as 1-30 percent, even higher water content, and the aqueous enzymatic method can be adopted. The aqueous enzymatic method is maintained for two hours at the temperature of about 50 ℃ to produce oil; the squeezing method needs drying to be within 5 percent, and the energy is high.
(3) The efficiency is high: although the walnut oil is prepared by the aqueous enzymatic method at present, the method only needs to carry out one-step reaction enzymolysis by the aqueous enzymatic method, has high reaction efficiency and short reaction time, greatly improves the enzymolysis efficiency, and provides a feasible test scheme for preparing the walnut oil by the aqueous enzymatic method.
(4) The walnut oil is prepared by adopting the aqueous enzymatic method, the condition is mild, the generation of harmful substances such as aflatoxin, 3, 4 benzopyrene and the like in the original extraction technology can be prevented, and the original ecology is achieved without adding a chemical antioxidant. However, in the prior art, the oil is generally roasted at a high temperature to generate a strong fragrance, but if the roasting temperature is too high or a local scorching phenomenon is generated, harmful substances such as aflatoxin, benzopyrene and the like are likely to be generated due to the pyrolysis and incomplete combustion of organic matters.
(5) Refining walnut oil: because the walnut oil is prepared by adopting the aqueous enzymatic method, part of water still exists in the walnut oil, and the hydration degumming can be directly carried out without introducing water.
(6) The method comprises the following steps of alkali refining deacidification: because the enzymolysis temperature is carried out at 45-55 ℃, the condition is mild, and no high-temperature condition exists basically in the walnut oil preparation process, the occurrence of free fatty acid can be well inhibited. The stage of alkali refining degumming is saved, the bad taste of saponification can not be introduced, and the alkali washing is naturally not needed.
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 embodiments or the prior art descriptions will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The examples do not show the specific experimental steps or conditions, and can be performed according to the conventional experimental steps described in the literature in the field. The reagents or instruments used are not indicated by manufacturers, and are all conventional reagent products which can be obtained commercially.
The alkaline protease used in the examples of the present invention was purchased from danisc, the papain was purchased from AB enzyme preparations and novacin in germany, the enzyme activity was 80 ten thousand, and the neutral protease was purchased from novacin.
Example 1
The embodiment provides a method for preparing walnut oil by an aqueous enzymatic method, which comprises the following specific steps:
step 1: 500g of walnut kernels which are full in grains, free of mildew, oil and rancid smell, free of insect damage and free of impurities are selected.
Step 2: preparing aqueous alkali solution with the mass concentration of 4 per mill, adding walnut kernels after boiling, timing for 25min, washing the walnut kernels after boiling with water, and washing the walnut kernels clean to obtain the peeled walnut kernels with the water content of 20%.
And step 3: crushing the pretreated walnut kernels by a colloid mill under the condition of not adding water, wherein the particle size of the crushed walnut kernels is not more than 900 microns.
And 4, step 4: adding water into the crushed walnut kernels to prepare walnut slurry, wherein the mass ratio of the walnut kernels to the water is 1: 3.
And 5: heating the walnut pulp to 50 ℃, adding alkaline protease, stirring and mixing, wherein the addition amount of the alkaline protease is 3 per mill of the mass of the walnut kernel by the mass of the walnut kernel, and reacting for 2 hours to obtain the walnut pulp after enzymolysis.
Step 6: centrifuging the enzymolysis walnut slurry at 8000r/min for 10min, and collecting the upper layer to obtain walnut oil.
Example 2
The embodiment provides a method for preparing walnut oil by an aqueous enzymatic method, which comprises the following specific steps:
step 1: 500g of walnut kernels which are full in grains, free of mildew, oil and rancid smell, free of insect damage and free of impurities are selected.
Step 2: preparing aqueous alkali solution with the mass concentration of 4 per mill, adding walnut kernels after boiling, timing for 25min, washing the walnut kernels after boiling with water, and washing the walnut kernels clean to obtain the peeled walnut kernels with the water content of 20%.
And step 3: crushing the pretreated walnut kernels by a colloid mill under the condition of not adding water, wherein the particle size of the crushed walnut kernels is not more than 900 microns.
And 4, step 4: adding water into the crushed walnut kernels to prepare walnut slurry, wherein the mass ratio of the walnut kernels to the water is 1: 3.
And 5: heating the walnut pulp to 50 ℃, adding papain, stirring and mixing, wherein the addition amount of the papain is 3 per mill of the mass of the walnut kernel by the mass of the walnut kernel, and reacting for 2 hours to obtain the walnut pulp after enzymolysis.
Step 6: centrifuging the enzymolysis walnut slurry at 8000r/min for 10min, and collecting the upper layer to obtain walnut oil.
Example 3
The embodiment provides a method for preparing walnut oil by an aqueous enzymatic method, which comprises the following specific steps:
step 1: 500g of walnut kernels which are full in grains, free of mildew, oil and rancid smell, free of insect damage and free of impurities are selected.
Step 2: preparing aqueous alkali solution with the mass concentration of 4 per mill, adding walnut kernels after boiling, timing for 25min, washing the walnut kernels after boiling with water, and washing the walnut kernels clean to obtain the peeled walnut kernels with the water content of 20%.
And step 3: crushing the pretreated walnut kernels by a colloid mill under the condition of not adding water, wherein the particle size of the crushed walnut kernels is not more than 900 microns.
And 4, step 4: adding water into the crushed walnut kernels to prepare walnut slurry, wherein the mass ratio of the walnut kernels to the water is 1: 3.
And 5: heating the walnut pulp to 50 ℃, adding neutral protease, stirring and mixing, wherein the addition amount of the neutral protease is 3 per mill of the mass of the walnut kernel by the mass of the walnut kernel, and reacting for 2 hours to obtain the walnut pulp after enzymolysis.
Step 6: centrifuging the enzymolysis walnut slurry at 8000r/min for 10min, and collecting the upper layer to obtain walnut oil.
Example 4
The embodiment provides a method for preparing walnut oil by an aqueous enzymatic method, the process flow is shown in fig. 1, and the specific steps are as follows:
step 1: 500g of walnut kernels which are full in grains, free of mildew, oil and rancid smell, free of insect damage and free of impurities are selected.
Step 2: preparing aqueous alkali solution with the mass concentration of 4 per mill, adding walnut kernels after boiling, timing for 25min, washing the walnut kernels after boiling with water, and washing the walnut kernels clean to obtain the peeled walnut kernels with the water content of 20%.
And step 3: crushing the pretreated walnut kernels by a colloid mill under the condition of not adding water, wherein the particle size of the crushed walnut kernels is not more than 900 microns.
And 4, step 4: adding water into the crushed walnut kernels to prepare walnut slurry, wherein the mass ratio of the walnut kernels to the water is 1: 3.
And 5: heating the walnut pulp to 50 ℃, adding alkaline protease, stirring and mixing, wherein the addition amount of the alkaline protease is 3 per mill of the mass of the walnut kernel by the mass of the walnut kernel, and reacting for 2 hours to obtain the walnut pulp after enzymolysis.
Step 6: centrifuging the enzymolysis walnut slurry at 8000r/min for 10min, and collecting the upper layer to obtain walnut oil.
And 7: heating the walnut oil to 60 ℃, stirring at the speed of 80r/min, and standing for 3 hours to obtain the hydration degummed walnut oil.
And 8: keeping the vacuum degree above 90kpa, heating the degummed walnut oil to 70 ℃, and reducing the water content to 0.08% to obtain the dehydrated walnut oil.
And step 9: controlling the oil temperature of dehydrated walnut oil at 60 deg.C, adding activated clay 4 wt% of the oil, decolorizing for 30min, rapidly cooling to below 40 deg.C after decolorizing, and separating oil from decolorizer with filter.
Step 10: heating decolorized walnut oil to 175 deg.C, maintaining vacuum degree at above 90kPa, and performing deodorization treatment for 4 hr.
Step 11: filling nitrogen for filling, and improving the shelf life.
Example 5
The embodiment provides a method for preparing walnut oil by an aqueous enzymatic method, the process flow is shown in fig. 1, and the specific steps are as follows:
step 1: 500g of walnut kernels which are full in grains, free of mildew, oil and rancid smell, free of insect damage and free of impurities are selected.
Step 2: preparing aqueous alkali solution with the mass concentration of 4 per mill, adding walnut kernels after boiling, timing for 25min, washing the walnut kernels after boiling with water, and washing the walnut kernels clean to obtain the peeled walnut kernels with the water content of 20%.
And step 3: crushing the pretreated walnut kernels by a colloid mill under the condition of not adding water, wherein the particle size of the crushed walnut kernels is not more than 900 microns.
And 4, step 4: adding water into the crushed walnut kernels to prepare walnut slurry, wherein the mass ratio of the walnut kernels to the water is 1: 3.
And 5: heating the walnut pulp to 50 ℃, adding alkaline protease, neutral protease and papain, stirring and mixing, wherein the addition amounts of the alkaline protease, the neutral protease and the papain are respectively 1 per mill of the mass of the walnut kernel based on the mass of the walnut kernel, and reacting for 2 hours to obtain the walnut pulp after enzymolysis.
Step 6: centrifuging the enzymolysis walnut slurry at 8000r/min for 10min, and collecting the upper layer to obtain walnut oil.
And 7: heating the walnut oil to 60 ℃, stirring at the speed of 80r/min, and standing for 3 hours to obtain the hydration degummed walnut oil.
And 8: keeping the vacuum degree above 90kPa, heating the degummed walnut oil to 70 ℃, and reducing the water content to 0.08 percent to obtain the dehydrated walnut oil.
And step 9: controlling the oil temperature of dehydrated walnut oil at 60 deg.C, adding activated clay 4 wt% of the oil, decolorizing for 30min, rapidly cooling to below 40 deg.C after decolorizing, and separating oil from decolorizer with filter.
Step 10: heating decolorized walnut oil to 175 deg.C, maintaining vacuum degree at above 90kPa, and performing deodorization for 4 hr.
Step 11: filling nitrogen for filling, and improving the shelf life.
Example 6
The embodiment provides a method for preparing walnut oil by an aqueous enzymatic method, the process flow is shown in fig. 1, and the specific steps are as follows:
step 1: 500g of walnut kernels which are full in grains, free of mildew, oil and rancid smell, free of insect damage and free of impurities are selected.
Step 2: preparing aqueous alkali solution with the mass concentration of 4 per mill, adding walnut kernels after boiling, timing for 25min, washing the walnut kernels after boiling with water, and washing the walnut kernels clean to obtain the peeled walnut kernels with the water content of 20%.
And step 3: crushing the pretreated walnut kernels by a colloid mill under the condition of not adding water, wherein the particle size of the crushed walnut kernels is not more than 900 microns.
And 4, step 4: adding water into the crushed walnut kernels to prepare walnut slurry, wherein the mass ratio of the walnut kernels to the water is 1: 5.
And 5: heating the walnut pulp to 50 ℃, adding alkaline protease, neutral protease and papain, stirring and mixing, wherein the addition amounts of the alkaline protease, the neutral protease and the papain are respectively 1 per mill of the mass of the walnut kernel based on the mass of the walnut kernel, and reacting for 2 hours to obtain the walnut pulp after enzymolysis.
Step 6: centrifuging the enzymolysis walnut slurry at 8000r/min for 10min, and collecting the upper layer to obtain walnut oil.
And 7: heating the walnut oil to 60 ℃, stirring at the speed of 80r/min, and standing for 3 hours to obtain the hydration degummed walnut oil.
And 8: keeping the vacuum degree above 90kPa, heating the degummed walnut oil to 70 ℃, and reducing the water content to 0.08 percent to obtain the dehydrated walnut oil.
And step 9: controlling the oil temperature of dehydrated walnut oil at 60 deg.C, adding activated clay 4 wt% of the oil, decolorizing for 30min, rapidly cooling to below 40 deg.C after decolorizing, and separating oil from decolorizer with filter.
Step 10: heating decolorized walnut oil to 175 deg.C, maintaining vacuum degree at above 90kPa, and performing deodorization treatment for 4 hr.
Step 11: filling nitrogen for filling, and improving the shelf life.
Example 7
The embodiment provides a method for preparing walnut oil by an aqueous enzymatic method, the process flow is shown in fig. 1, and the specific steps are as follows:
step 1: 500g of walnut kernels which are full in grains, free of mildew, oil and rancid smell, free of insect damage and free of impurities are selected.
Step 2: preparing aqueous alkali solution with the mass concentration of 4 per mill, adding walnut kernels after boiling, timing for 25min, washing the walnut kernels after boiling with water, and washing the walnut kernels clean to obtain the peeled walnut kernels with the water content of 20%.
And step 3: crushing the pretreated walnut kernels by a colloid mill under the condition of not adding water, wherein the particle size of the crushed walnut kernels is not more than 900 microns.
And 4, step 4: adding water into the crushed walnut kernels to prepare walnut slurry, wherein the mass ratio of the walnut kernels to the water is 1: 3.
And 5: heating the walnut pulp to 50 ℃, adding alkaline protease, neutral protease and papain, stirring and mixing, wherein the addition amounts of the alkaline protease, the neutral protease and the papain are respectively 1.5 per mill of the mass of the walnut kernel based on the mass of the walnut kernel, and reacting for 2 hours to obtain the walnut pulp after enzymolysis.
Step 6: centrifuging the enzymolysis walnut slurry at 8000r/min for 10min, and collecting the upper layer to obtain walnut oil.
And 7: heating the walnut oil to 60 ℃, stirring at the speed of 80r/min, and standing for 3 hours to obtain the hydration degummed walnut oil.
And 8: keeping the vacuum degree above 90kPa, heating the degummed walnut oil to 70 ℃, and reducing the water content to 0.08 percent to obtain the dehydrated walnut oil.
And step 9: controlling the oil temperature of dehydrated walnut oil at 60 deg.C, adding activated clay 4 wt% of the oil, decolorizing for 30min, rapidly cooling to below 40 deg.C after decolorizing, and separating oil from decolorizer with filter.
Step 10: heating decolorized walnut oil to 175 deg.C, maintaining vacuum degree at above 90kPa, and performing deodorization treatment for 4 hr.
Step 11: filling nitrogen for filling, and improving the shelf life.
Example 8
The embodiment provides a method for preparing walnut oil by an aqueous enzymatic method, the process flow is shown in fig. 1, and the specific steps are as follows:
step 1: 500g of walnut kernels which are full in grains, free of mildew, oil and rancid smell, free of insect damage and free of impurities are selected.
Step 2: preparing aqueous alkali solution with the mass concentration of 4 per mill, adding walnut kernels after boiling, timing for 25min, washing the walnut kernels after boiling with water, and obtaining the peeled walnut kernels with the water content of 1 percent after washing.
And step 3: crushing the pretreated walnut kernels by a colloid mill under the condition of not adding water, wherein the particle size of the crushed walnut kernels is not more than 900 microns.
And 4, step 4: adding water into the crushed walnut kernels to prepare walnut slurry, wherein the mass ratio of the walnut kernels to the water is 1: 3.
And 5: heating the walnut pulp to 50 ℃, adding alkaline protease, neutral protease and papain, stirring and mixing, wherein the addition amounts of the alkaline protease, the neutral protease and the papain are respectively 1 per mill of the mass of the walnut kernel based on the mass of the walnut kernel, and reacting for 2 hours to obtain the walnut pulp after enzymolysis.
Step 6: centrifuging the enzymolysis walnut slurry at 8000r/min for 10min, and collecting the upper layer to obtain walnut oil.
And 7: heating the walnut oil to 60 ℃, stirring at the speed of 80r/min, and standing for 3 hours to obtain the hydration degummed walnut oil.
And 8: keeping the vacuum degree above 90kPa, heating the degummed walnut oil to 70 ℃, and reducing the water content to 0.08 percent to obtain the dehydrated walnut oil.
And step 9: controlling the oil temperature of dehydrated walnut oil at 60 deg.C, adding activated clay 4 wt% of the oil, decolorizing for 30min, rapidly cooling to below 40 deg.C after decolorizing, and separating oil from decolorizer with filter.
Step 10: heating decolorized walnut oil to 175 deg.C, maintaining vacuum degree at above 90kPa, and performing deodorization treatment for 4 hr.
Step 11: filling nitrogen for filling, and improving the shelf life.
Example 9
The embodiment provides a method for preparing walnut oil by an aqueous enzymatic method, the process flow is shown in fig. 1, and the specific steps are as follows:
step 1: 500g of walnut kernels which are full in grains, free of mildew, oil and rancid smell, free of insect damage and free of impurities are selected.
And 2, step: preparing aqueous alkali solution with the mass concentration of 4 per mill, adding walnut kernels after boiling, timing for 25min, washing the walnut kernels after boiling with water, and obtaining the peeled walnut kernels with the water content of 1 percent after washing.
And step 3: crushing the pretreated walnut kernels by a colloid mill under the condition of not adding water, wherein the particle size of the crushed walnut kernels is not more than 900 microns.
And 4, step 4: adding water into the crushed walnut kernels to prepare walnut slurry, wherein the mass ratio of the walnut kernels to the water is 1: 5.
And 5: heating the walnut pulp to 50 ℃, adding alkaline protease, neutral protease and papain, stirring and mixing, wherein the addition amounts of the alkaline protease, the neutral protease and the papain are respectively 1 per mill of the mass of the walnut kernel based on the mass of the walnut kernel, and reacting for 2 hours to obtain the walnut pulp after enzymolysis.
Step 6: centrifuging the enzymolysis walnut slurry at 8000r/min for 10min, and collecting the upper layer to obtain walnut oil.
And 7: heating the walnut oil to 60 ℃, stirring at the speed of 80r/min, and standing for 3 hours to obtain the hydration degummed walnut oil.
And 8: keeping the vacuum degree above 90kPa, heating the degummed walnut oil to 70 ℃, and reducing the water content to 0.08 percent to obtain the dehydrated walnut oil.
And step 9: controlling the oil temperature of dehydrated walnut oil at 60 deg.C, adding activated clay 4 wt% of the oil, decolorizing for 30min, rapidly cooling to below 40 deg.C after decolorizing, and separating oil from decolorizer with filter.
Step 10: heating decolorized walnut oil to 175 deg.C, maintaining vacuum degree at above 90kPa, and performing deodorization treatment for 4 hr.
Step 11: filling nitrogen for filling, and improving the shelf life.
Example 10
The embodiment provides a method for preparing walnut oil by an aqueous enzymatic method, which comprises the following specific steps:
step 1: 500g of walnut kernels which are full in grains, free of mildew, oil and rancid smell, free of insect damage and free of impurities are selected.
Step 2: preparing aqueous alkali solution with the mass concentration of 2 per mill, adding walnut kernels after boiling, timing for 25min, washing the walnut kernels after boiling with water, and obtaining the peeled walnut kernels with the water content of 30 percent after washing.
And step 3: crushing the pretreated walnut kernels by a colloid mill under the condition of not adding water, wherein the particle size of the crushed walnut kernels is not more than 900 microns.
And 4, step 4: adding water into the crushed walnut kernels to prepare walnut slurry, wherein the mass ratio of the walnut kernels to the water is 1: 5.
And 5: heating the walnut pulp to 45 ℃, adding alkaline protease, neutral protease and papain, stirring and mixing, wherein the addition amounts of the alkaline protease, the neutral protease and the papain are respectively 1 per mill of the mass of the walnut kernel based on the mass of the walnut kernel, and reacting for 2 hours to obtain the walnut pulp after enzymolysis.
Step 6: centrifuging the enzymolysis walnut slurry at 6000r/min for 5min, and collecting the upper layer to obtain walnut oil.
And 7: heating walnut oil to 50 ℃, stirring at a speed of 100r/min, and standing for 4 hours to obtain the hydration degummed walnut oil.
And 8: keeping the vacuum degree above 90kPa, heating the degummed walnut oil to 80 ℃, and reducing the water content to 0.08 percent to obtain the dehydrated walnut oil.
And step 9: controlling the oil temperature of dehydrated walnut oil at 50 deg.C, adding activated clay 5 wt% of the oil, decolorizing for 20min, rapidly cooling to below 40 deg.C after decolorizing, and separating oil from decolorizer with filter.
Step 10: heating decolorized walnut oil to 180 deg.C, maintaining vacuum degree at above 90kPa, and deodorizing for 5 hr.
Step 11: filling nitrogen for filling, and improving the shelf life.
Example 11
The embodiment provides a method for preparing walnut oil by an aqueous enzymatic method, which comprises the following specific steps:
step 1: 500g of walnut kernels which are full in grains, free of mildew, oil and rancid smell, free of insect damage and free of impurities are selected.
Step 2: preparing aqueous alkali solution with mass concentration of 6 per mill, boiling, adding semen Juglandis, timing for 1min, washing semen Juglandis with water, and cleaning to obtain semen Persicae with water content of 1%.
And step 3: crushing the pretreated walnut kernels by a colloid mill under the condition of not adding water, wherein the particle size of the crushed walnut kernels is not more than 900 microns.
And 4, step 4: adding water into the crushed walnut kernels to prepare walnut slurry, wherein the mass ratio of the walnut kernels to the water is 1: 2.
And 5: heating the walnut pulp to 55 ℃, adding alkaline protease, neutral protease and papain, stirring and mixing, wherein the addition amounts of the alkaline protease, the neutral protease and the papain are respectively 1.5 per mill of the mass of the walnut kernel based on the mass of the walnut kernel, and reacting for 3 hours to obtain the walnut pulp after enzymolysis.
Step 6: centrifuging the enzymolysis walnut slurry at 10000r/min for 15min, and taking the upper layer to obtain walnut oil.
And 7: heating the walnut oil to 70 ℃, stirring at 30r/min, and standing for 2 hours to obtain the hydration degummed walnut oil.
And 8: keeping the vacuum degree above 90kPa, heating the degummed walnut oil to 80 ℃, and reducing the water content to 0.08 percent to obtain the dehydrated walnut oil.
And step 9: controlling the oil temperature of dehydrated walnut oil at 70 deg.C, adding activated clay 3 wt% of the oil, decolorizing for 20min, rapidly cooling to below 40 deg.C after decolorizing, and separating oil from decolorizer with filter.
Step 10: heating decolorized walnut oil to 170 deg.C, maintaining vacuum degree at above 90kPa, and deodorizing for 3 hr.
Step 11: filling nitrogen for filling, and improving the shelf life.
Comparative example 1
The comparative example provides a method for preparing walnut oil by an aqueous enzymatic method for crushing pretreated walnut kernels by using a colloid mill under the condition of adding water, and the method comprises the following specific steps:
step 1: 500g of walnut kernels which are full in grains, free of mildew, oil and rancid smell, free of insect damage and free of impurities are selected.
Step 2: preparing aqueous alkali solution with the mass concentration of 4 per mill, adding walnut kernels after boiling, timing for 25min, washing the walnut kernels after boiling with water, and washing the walnut kernels clean to obtain the peeled walnut kernels with the water content of 20%.
And 3, step 3: adding water into the peeled walnut kernels, wherein the mass ratio of the walnut kernels to the water is 1: 3.
And 4, step 4: crushing with colloid mill to obtain walnut kernel with particle size not greater than 900 μm.
And 5: heating the walnut pulp to 50 ℃, adding alkaline protease, stirring and mixing, wherein the addition amount of the alkaline protease is 3 per mill of the mass of the walnut kernel by the mass of the walnut kernel, and reacting for 2 hours to obtain the walnut pulp after enzymolysis.
Step 6: centrifuging the enzymolysis walnut slurry at 8000r/min for 10min, and collecting the upper layer to obtain walnut oil.
And 7: heating the walnut oil to 50 ℃, stirring at 30r/min, and standing for 4 hours to obtain the hydration degummed walnut oil.
And 8: dehydrating the walnut oil: maintaining the vacuum degree above 90kPa, heating degummed walnut oil to 60 deg.C, and reducing water content to below 0.11% to obtain dehydrated walnut oil.
And step 9: controlling the oil temperature of dehydrated walnut oil at 50 deg.C, adding activated clay 5 wt% of the oil, decolorizing for 40min, rapidly cooling to below 40 deg.C after decolorizing, and separating oil from decolorizer with filter.
Step 10: heating decolorized walnut oil to 170 deg.C, maintaining vacuum degree at above 90kPa, and deodorizing for 3 hr.
Step 11: filling nitrogen for filling, and improving the shelf life.
Comparative example 2
The comparative example provides a method for preparing walnut oil by an aqueous enzymatic method after crushing, which comprises the following specific steps:
step 1: 500g of walnut kernels which are full in grains, free of mildew, oil and rancid smell, free of insect damage and free of impurities are selected.
Step 2: preparing aqueous alkali solution with the mass concentration of 4 per mill, adding walnut kernels after boiling, timing for 25min, washing the walnut kernels after boiling with water, and washing the walnut kernels clean to obtain the peeled walnut kernels with the water content of 20%.
And step 3: crushing the pretreated walnut kernels, wherein the average particle size of the crushed walnut kernels is 1500 mu m.
And 4, step 4: adding water into the crushed walnut kernels to prepare walnut slurry, wherein the mass ratio of the walnut kernels to the water is 1: 3.
and 5: heating the walnut pulp to 50 ℃, adding alkaline protease, stirring and mixing, wherein the addition amount of the alkaline protease is 3 per mill of the mass of the walnut kernel by the mass of the walnut kernel, and reacting for 2 hours to obtain the walnut pulp after enzymolysis.
Step 6: centrifuging the enzymolysis walnut slurry at 8000r/min for 10min, and collecting the upper layer to obtain walnut oil.
And 7: heating the walnut oil to 50 ℃, stirring at 30r/min, and standing for 4 hours to obtain the hydration degummed walnut oil.
And 8: keeping the vacuum degree above 90kPa, heating the degummed walnut oil to 60 ℃, and reducing the water content to 0.08 percent to obtain the dehydrated walnut oil.
And step 9: controlling the oil temperature of dehydrated walnut oil at 50 deg.C, adding activated clay 5 wt% of the oil, decolorizing for 20min, rapidly cooling to below 40 deg.C after decolorizing, and separating oil from decolorizer with filter.
Step 10: heating decolorized walnut oil to 170 deg.C, maintaining vacuum degree at above 90kPa, and deodorizing for 3 hr.
Step 11: filling nitrogen for filling, and improving the shelf life.
Comparative example 3
The comparative example provides a method for homogenizing after crushing by a colloid mill and adding water, which comprises the following specific steps:
step 1: 500g of walnut kernels which are full in grains, free of mildew, oil and rancid taste, free of insect pests and free of impurities are selected.
Step 2: preparing aqueous alkali solution with the mass concentration of 4 per mill, adding walnut kernels after boiling, timing for 25min, washing the walnut kernels after boiling with water, and washing the walnut kernels clean to obtain the peeled walnut kernels with the water content of 20%.
And step 3: crushing the pretreated walnut kernels by a colloid mill under the condition of not adding water, wherein the particle size of the crushed walnut kernels is not more than 900 microns.
And 4, step 4: adding water into the crushed walnut kernels to prepare walnut slurry, wherein the mass ratio of the walnut kernels to the water is 1:3, heating the walnut slurry to 55 ℃ for homogenization, wherein the homogenization pressure is as follows: 20 MPa.
And 5: heating the walnut pulp to 50 ℃, adding alkaline protease, stirring and mixing, wherein the addition amount of the alkaline protease is 3 per mill of the mass of the walnut kernel by the mass of the walnut kernel, and reacting for 2 hours to obtain the walnut pulp after enzymolysis.
Step 6: centrifuging the enzymolysis walnut slurry at 8000r/min for 10min, and collecting the upper layer to obtain walnut oil.
And 7: heating the walnut oil to 50 ℃, stirring at 30r/min, and standing for 4 hours to obtain the hydration degummed walnut oil.
And step 8: keeping the vacuum degree above 90kPa, heating the degummed walnut oil to 60 ℃, and reducing the water content to 0.08 percent to obtain the dehydrated walnut oil.
And step 9: controlling the oil temperature of dehydrated walnut oil at 50 deg.C, adding activated clay 5 wt% of the oil, decolorizing for 30min, rapidly cooling to 40 deg.C after decolorizing, and separating oil from decolorizer with filter.
Step 10: heating decolorized walnut oil to 170 deg.C, maintaining vacuum degree at above 90kPa, and deodorizing for 3 hr.
Step 11: filling nitrogen for filling, and improving the shelf life.
Experimental example 1
The fat contents of the walnut kernels in examples 1 to 11, the walnut oil obtained by separating in examples 1 to 11, the walnut kernels in comparative examples 1 to 3 and the walnut oil obtained by separating in comparative examples 1 to 3 are respectively measured by a second acid hydrolysis method in GB 5009.6-2016 national food safety standard food determination, and the oil yield is defined as the calculation method: separating the walnut slurry after enzymolysis to obtain the percentage of walnut oil in the prokaryotic peach kernels.
The results of oil yield are calculated as shown in table 1:
TABLE 1 oil yield results
Experimental example 2
No harmful substances were detected by using a headspace gas chromatograph.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (10)
1. The method for preparing walnut oil by using the aqueous enzymatic method is characterized by comprising the following steps:
crushing the pretreated walnut kernels under the condition of not adding water, wherein the particle size of the crushed walnut kernels is less than or equal to 900 microns; adding water into the crushed walnut kernels to prepare walnut pulp; carrying out enzymolysis on the walnut pulp by using an aqueous enzymatic method; and separating the walnut pulp after enzymolysis to obtain the walnut oil.
2. The method for preparing walnut oil by using the aqueous enzymatic method as claimed in claim 1, wherein the water content of the pretreated walnut kernels is 1-30%.
3. The method for preparing walnut oil by the aqueous enzymatic method according to any one of claims 1 to 2, wherein the mass ratio of the crushed walnut kernels to water is 1:2 to 1: 5.
4. The method for preparing walnut oil by using the aqueous enzymatic method according to any one of claims 1 to 3, wherein the step of performing enzymatic hydrolysis on walnut slurry by using the aqueous enzymatic method specifically comprises: heating the walnut pulp to 45-55 ℃, adding protease, stirring and mixing, wherein the addition amount of the protease is 2-5 per mill of the mass of the walnut kernel by the mass of the walnut kernel, and reacting for 2-3 h to obtain the walnut pulp after enzymolysis.
5. The method for preparing walnut oil by using the aqueous enzymatic method of claim 4, wherein the protease comprises at least one of alkaline protease, neutral protease and papain.
6. The method for preparing walnut oil by using the aqueous enzymatic method according to any one of claims 1 to 5, wherein the separation specifically comprises: centrifuging the walnut pulp subjected to enzymolysis, wherein the centrifugation conditions are as follows: centrifuging for 5-15 min under the condition of 6000-10000 r/min.
7. The method for preparing walnut oil by using the aqueous enzymatic method according to any one of claims 1 to 6, wherein the pretreated walnut kernels comprise: selecting walnut kernels and peeling the walnut kernels:
the walnut kernel selection steps specifically comprise: selecting walnut kernels which are free from mildew, oil and rancid, insect pests and impurities and have full grains;
and/or the peeling step of the walnut kernels specifically comprises the following steps: peeling semen Juglandis by alkali cooking process, and washing with water;
and/or, the soda boiling process comprises: preparing an alkaline water solution with the mass concentration of 2-6 per mill, adding the walnut kernels after boiling, timing for 1-25 min, and washing the walnut kernels after alkaline boiling with water to finish the peeling process.
8. The method for preparing walnut oil by the aqueous enzymatic method according to any one of claims 1 to 7, further comprising a step of refining walnut oil;
optionally, the refining step comprises hydration degumming, dehydration, decolorization or deodorization treatment.
9. The method for preparing walnut oil by using the aqueous enzymatic method according to claim 8, wherein the hydration degumming treatment specifically comprises: heating the walnut oil to 50-70 ℃, stirring at 30-100 r/min, and standing for 2-4 h to obtain hydrated degummed walnut oil;
and/or the dehydration treatment specifically comprises: keeping the vacuum degree above 90kPa, heating the hydration degummed walnut oil to 60-80 ℃ to reduce the water content in the hydration degummed walnut oil to below 0.11 percent, and obtaining dehydrated walnut oil;
and/or the decoloring treatment specifically comprises the following steps: controlling the oil temperature of the dehydrated walnut oil at 50-70 ℃, adding a decoloring agent, wherein the adding amount of the decoloring agent is 3-5% of the weight of the dehydrated walnut oil, decoloring for 20-40 min, quickly cooling the oil temperature to be below 40 ℃ after decoloring, and separating the decoloring agent by using a filter to obtain the decolored walnut oil;
the deodorization treatment specifically comprises: the oil temperature is kept at 170-180 ℃ during deodorization, the vacuum degree is kept above 90kPa, and the deodorization time is 3-5 h.
10. The method for preparing walnut oil by using the aqueous enzymatic method according to any one of claims 8 to 9, further comprising: and (4) filling nitrogen after the walnut oil refining step to obtain the filled walnut oil.
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