CN114686297A - Method for efficiently retaining natural VE and phytosterol in walnut oil - Google Patents
Method for efficiently retaining natural VE and phytosterol in walnut oil Download PDFInfo
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
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- 239000010470 pecan oil Substances 0.000 claims abstract description 23
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- 235000014113 dietary fatty acids Nutrition 0.000 claims description 12
- 229930195729 fatty acid Natural products 0.000 claims description 12
- 239000000194 fatty acid Substances 0.000 claims description 12
- -1 fatty acid ester Chemical class 0.000 claims description 12
- 239000002994 raw material Substances 0.000 claims description 12
- 229940068065 phytosterols Drugs 0.000 claims description 9
- 238000000926 separation method Methods 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 235000019387 fatty acid methyl ester Nutrition 0.000 claims description 6
- 150000004665 fatty acids Chemical class 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 6
- 238000000199 molecular distillation Methods 0.000 claims description 6
- 238000000265 homogenisation Methods 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 abstract description 16
- 238000005057 refrigeration Methods 0.000 abstract description 9
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- 238000000605 extraction Methods 0.000 abstract description 2
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- 235000020234 walnut Nutrition 0.000 description 7
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- 241000196324 Embryophyta Species 0.000 description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
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- 238000002360 preparation method Methods 0.000 description 4
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- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
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- 238000002425 crystallisation Methods 0.000 description 3
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- WIGCFUFOHFEKBI-UHFFFAOYSA-N gamma-tocopherol Natural products CC(C)CCCC(C)CCCC(C)CCCC1CCC2C(C)C(O)C(C)C(C)C2O1 WIGCFUFOHFEKBI-UHFFFAOYSA-N 0.000 description 3
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- 206010028980 Neoplasm Diseases 0.000 description 2
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- HVYWMOMLDIMFJA-DPAQBDIFSA-N cholesterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CCCC(C)C)[C@@]1(C)CC2 HVYWMOMLDIMFJA-DPAQBDIFSA-N 0.000 description 2
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- JYGXADMDTFJGBT-VWUMJDOOSA-N hydrocortisone Chemical compound O=C1CC[C@]2(C)[C@H]3[C@@H](O)C[C@](C)([C@@](CC4)(O)C(=O)CO)[C@@H]4[C@@H]3CCC2=C1 JYGXADMDTFJGBT-VWUMJDOOSA-N 0.000 description 2
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- 235000010777 Arachis hypogaea Nutrition 0.000 description 1
- 235000018262 Arachis monticola Nutrition 0.000 description 1
- BSYNRYMUTXBXSQ-UHFFFAOYSA-N Aspirin Chemical compound CC(=O)OC1=CC=CC=C1C(O)=O BSYNRYMUTXBXSQ-UHFFFAOYSA-N 0.000 description 1
- 208000024172 Cardiovascular disease Diseases 0.000 description 1
- 244000068988 Glycine max Species 0.000 description 1
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- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000357 carcinogen Toxicity 0.000 description 1
- 239000003183 carcinogenic agent Substances 0.000 description 1
- 210000000748 cardiovascular system Anatomy 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 235000012000 cholesterol Nutrition 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 208000029078 coronary artery disease Diseases 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
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- HFHZKZSRXITVMK-UHFFFAOYSA-N oxyphenbutazone Chemical compound O=C1C(CCCC)C(=O)N(C=2C=CC=CC=2)N1C1=CC=C(O)C=C1 HFHZKZSRXITVMK-UHFFFAOYSA-N 0.000 description 1
- 229960000649 oxyphenbutazone Drugs 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/02—Pretreatment
- C11B1/04—Pretreatment of vegetable raw material
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
- A23D9/00—Other edible oils or fats, e.g. shortenings, cooking oils
- A23D9/007—Other edible oils or fats, e.g. shortenings, cooking oils characterised by ingredients other than fatty acid triglycerides
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
- A23D9/00—Other edible oils or fats, e.g. shortenings, cooking oils
- A23D9/02—Other edible oils or fats, e.g. shortenings, cooking oils characterised by the production or working-up
- A23D9/04—Working-up
-
- 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
- C11B1/06—Production of fats or fatty oils from raw materials by pressing
- C11B1/08—Production of fats or fatty oils from raw materials by pressing by hot pressing
-
- 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
-
- 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
-
- 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
- C11B3/12—Refining fats or fatty oils by distillation
-
- 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
- C11B7/00—Separation of mixtures of fats or fatty oils into their constituents, e.g. saturated oils from unsaturated oils
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C3/00—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
- C11C3/04—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by esterification of fats or fatty oils
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C3/00—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
- C11C3/04—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by esterification of fats or fatty oils
- C11C3/08—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by esterification of fats or fatty oils with fatty acids
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Microbiology (AREA)
- General Chemical & Material Sciences (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Steroid Compounds (AREA)
- Fats And Perfumes (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention belongs to the technical field of biological extraction, and particularly relates to a method for efficiently retaining natural VE and phytosterol in walnut oil, which comprises the following steps: drying peeled pecan seeds at low temperature, hydraulically pressing oil, and collecting pecan crude oil and residue cake; adding water into the residue cake, stirring to obtain water-extracted oil of fructus Juglandis, esterifying and alcoholizing, naturally cooling, crystallizing, and filtering; adding the obtained phytosterol crystal and natural VE into the hickory crude oil; refrigerating the crude pecan oil, separating the supernatant of the crude pecan oil in a refrigerating environment, separating the supernatant again from the lower-layer solid-liquid mixture, and combining to obtain the pecan oil. On the basis of low-temperature drying, the high-quality hickory oil is efficiently prepared by adopting the processes of liquid squeezing, water extraction, refrigeration, centrifugation and the like, the natural VE and the phytosterol nutrient components in the oil are not damaged, and the natural VE and the phytosterol in the residue cake formed by squeezing can be reserved, so that the nutritional value is improved.
Description
Technical Field
The invention belongs to the technical field of biological extraction, and particularly relates to a method for efficiently retaining natural VE and phytosterol in walnut oil.
Background
The natural vitamin E is widely present in animal and plant tissues in nature, particularly in oil of seeds and pulps of plants, is a light yellow viscous transparent liquid, is colorless, tasteless, insoluble in water, and soluble in organic solvents such as ethanol, acetone, chloroform and the like and oil. The natural vitamin E is obviously different from a synthetic product in the aspects of production raw materials, optical activity, density and isomer composition, and has the functions of enhancing the immunity of the organism and resisting cancer; protecting nervous system, skeletal muscle, retina and delaying aging; maintaining normal function of the cardiovascular system, etc.; is widely used in the industries of medicine, food, cosmetics, feed and the like.
Phytosterols are widely found in plants and plant seeds, are important components of plant cells, and have very important physiological functions. The phytosterol is white powder or crystal with optical activity, is insoluble in water, acid and alkali, is slightly soluble in acetone and ethanol at normal temperature, and is dissolved in organic solvents such as diethyl ether, benzene, chloroform, ethyl acetate, petroleum ether, carbon disulfide and the like. The phytosterol can effectively reduce cholesterol in blood, and has the effect of effectively preventing and treating cardiovascular diseases such as hypertension, coronary heart disease and the like; has anti-inflammatory effect similar to that of oxyphenbutazone and hydrocortisone, and has antipyretic effect similar to that of acetylsalicylic acid; has the function of blocking carcinogen from inducing cancer cell formation; has excellent physiological effect in nourishing and protecting skin. The phytosterol is a safe natural substance and is widely used in the industries of medicine, food, cosmetics, animal growth agents, chemical industry and the like.
The walnut oil is edible vegetable oil which is prepared by squeezing walnut kernels serving as a raw material, has the oil content of 65-70 percent, and is the first of all woody oil plants and has the reputation of 'oil depots on trees'. At present, the production of the pressed walnut oil is basically the production equipment and the process technology of the bulk edible oil such as peanut, soybean and the like which are directly introduced. The basic process comprises the following steps: and (3) after the crude oil is squeezed out by an oil press, refining the crude oil through a traditional refining link to obtain refined oil. The refining link of the edible oil generally comprises 6 process steps of dephosphorization, dehydration, decolorization, deacidification, dewaxing, deodorization and the like. The treatment process can greatly lose a plurality of health-care functional components (such as phytosterol and vitamin E) in the walnut oil, so that the quality of the finished walnut oil is greatly reduced; the added chemicals may become new contaminants that affect food hygiene and safety.
The traditional production and preparation process of walnut oil has certain defects, and natural VE and phytosterol in a residue cake formed by squeezing cannot be reserved, so that a lot of natural VE and phytosterol functional components are lost in the prepared walnut oil. Therefore, it is necessary to optimize and improve it.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provide a method for efficiently retaining natural VE and phytosterol in walnut oil.
In order to achieve the technical purpose and achieve the technical effect, the invention is realized by the following technical scheme:
a method for efficiently retaining natural VE and phytosterol in walnut oil comprises the following steps:
1) drying peeled pecan seeds at a low temperature of 60-80 ℃ until the water content is 4-6%, putting the pecan seeds dried at the low temperature into a hydraulic oil press to prepare oil, stopping squeezing after the oil yield is 50-55%, and respectively collecting pecan crude oil and a residue cake;
2) adding deionized water into the residue cake obtained in the step 1) according to the ratio of material to liquid of 1: 6-7 w/v, stirring in a stirrer at 500-1000 rpm, standing, and removing residual shells; adjusting the pH value of the mixed solution to 3-5, placing the mixed solution into a homogenizer for homogenization for 1-3 min, centrifuging the homogenized mixed solution in a centrifuge for 15-30 min to separate an oil phase, a water phase and residues, and drying the oil phase at 70-90 ℃ for 40-60 min to dehydrate to obtain the hickory water extract oil;
3) esterifying and alcoholizing the water-extracted pecan oil obtained in the step 2), converting fatty acid and fatty acid ester contained in the water-extracted pecan oil into fatty acid methyl ester, naturally cooling and crystallizing for 5-15 h at 10-20 ℃, and filtering; adding the obtained phytosterol crystals into the hickory crude oil obtained in the step 1), separating alcohol ester and natural VE from the filtrate through molecular distillation, and adding the natural VE into the hickory crude oil obtained in the step 1);
4) adding the phytosterol crystals into the mixture obtained in the step 3), refrigerating the crude pecan oil of natural VE, separating the supernatant of the crude pecan oil in a refrigerating environment, centrifuging the lower-layer solid-liquid mixture of the crude pecan oil, separating the supernatant again, and combining the supernatants obtained by two times of separation to obtain the walnut oil.
Further, according to the method for efficiently retaining natural VE and phytosterol in walnut oil, in the step 1), a shell breaking machine is adopted to break shells of the pecan seeds, and pure seeds, pure kernels or a seed kernel mixture formed after the pecan seeds are broken shells is used as a raw material for preparing oil by a hydraulic oil press.
Further, the method for efficiently retaining the natural VE and the phytosterol in the walnut oil comprises the step 1) of drying peeled pecan seeds at a low temperature of 70 ℃ until the water content is 5%.
Further, according to the method for efficiently retaining natural VE and phytosterol in walnut oil, in the step 2), the pH value of the mixed solution is adjusted to 4, the mixed solution is placed in a homogenizer at 2000-4000 rpm for homogenizing for 1-3 min, and the homogenized mixed solution is centrifuged in a centrifuge at 7000-10000 rpm for 15-30 min.
Further, according to the method for efficiently retaining natural VE and phytosterol in walnut oil, in the step 2), the oil phase is dried at 80 ℃ for 40-60 min and dehydrated to obtain the pecan water-extracted oil.
Further, the method for efficiently retaining the natural VE and the phytosterol in the walnut oil comprises the step 3) of naturally cooling and crystallizing for 10 hours at 15 ℃.
Further, according to the method for efficiently retaining the natural VE and the phytosterol in the walnut oil, in the step 4), the refrigerating treatment temperature is 2-4 ℃, and the refrigerating time is 24-48 hours.
Further, according to the method for efficiently retaining natural VE and phytosterol in walnut oil, in the step 4), the centrifugal treatment is realized through a centrifugal machine, the rotating speed of the centrifugal machine is 2000-4000 rpm, and the centrifugal time is 5-10 min.
The invention has the beneficial effects that:
aiming at the characteristics of high oil content and high unsaturated fatty acid content of the hickory, the invention adopts the processes of liquid squeezing, water extraction, refrigeration centrifugation and the like to efficiently prepare the high-quality hickory oil on the basis of low-temperature drying, does not damage the natural VE and the phytosterol nutrient components in the oil, and can retain the natural VE and the phytosterol in the squeezed residue cake, thereby improving the nutritional value.
Of course, it is not necessary for any one product that embodies the invention to achieve all of the above advantages simultaneously.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A method for efficiently retaining natural VE and phytosterol in walnut oil comprises the following steps:
1) drying peeled pecan seeds at a low temperature of 60-80 ℃ until the water content is 4-6%, breaking the pecan seeds by using a shell breaking machine, and taking pure seeds, pure kernels or a seed kernel mixture formed by breaking the pecan seeds as a raw material for preparing oil by using a hydraulic oil press. Placing the pecan seeds dried at a low temperature into a hydraulic oil press to prepare oil, stopping squeezing after the oil yield is 50-55%, and respectively collecting pecan crude oil and residue cakes;
2) adding deionized water into the residue cake obtained in the step 1) according to the ratio of material to liquid of 1: 6-7 w/v, stirring in a stirrer at 500-1000 rpm, standing, and removing residual shells; adjusting the pH value of the mixed solution to 3-5, then placing the mixed solution into a homogenizer at 2000-4000 rpm for homogenization for 1-3 min, centrifuging the homogenized mixed solution in a centrifuge at 7000-10000 rpm for 15-30 min to separate an oil phase, a water phase and residues, and drying the oil phase at 70-90 ℃ for 40-60 min to dehydrate to obtain the water extracted oil of the pecans;
3) esterifying and alcoholizing the water-extracted pecan oil obtained in the step 2), converting fatty acid and fatty acid ester contained in the water-extracted pecan oil into fatty acid methyl ester, naturally cooling and crystallizing for 5-15 h at 10-20 ℃, and filtering; adding the obtained phytosterol crystals into the hickory crude oil obtained in the step 1), separating alcohol ester and natural VE from the filtrate through molecular distillation, and adding the natural VE into the hickory crude oil obtained in the step 1);
4) adding the phytosterol crystals into the raw material obtained in the step 3), and refrigerating the natural VE-containing pecan crude oil at the temperature of 2-4 ℃ for 24-48 hours; separating the supernatant of the walnut crude oil in a refrigeration environment, centrifuging a lower-layer solid-liquid mixture of the walnut crude oil, and separating the supernatant again, wherein the centrifugation is realized by a centrifuge, the rotation speed of the centrifuge is 2000-4000 rpm, and the centrifugation time is 5-10 min; and combining the supernatants obtained by the two times of separation to obtain the walnut oil.
The following embodiments are relevant to the present invention:
example 1
A method for efficiently retaining natural VE and phytosterol in walnut oil comprises the following steps:
1) drying peeled pecan seeds at 70 ℃ to water content of 5%, cracking the pecan seeds by using a cracker, and using pure seeds, pure kernels or a seed kernel mixture formed by cracking the pecan seeds as a raw material for preparing oil by using a hydraulic oil press. Placing the pecan seeds dried at low temperature in a hydraulic oil press to prepare oil, stopping squeezing after the oil yield is 52%, and respectively collecting pecan crude oil and residue cake;
2) adding deionized water into the residue cake obtained in the step 1) according to the ratio of material to liquid of 1:6w/v, stirring in a 800rpm stirrer, standing, and removing residual shells; adjusting pH of the mixed solution to 4, homogenizing at 3000rpm for 2min, centrifuging at 8000rpm for 20min, separating oil phase, water phase and residue, drying the oil phase at 80 deg.C for 50min, and dehydrating to obtain water-extracted oil of fructus Juglandis;
3) esterifying and alcoholizing the water-extracted pecan oil obtained in the step 2), converting fatty acid and fatty acid ester contained in the water-extracted pecan oil into fatty acid methyl ester, naturally cooling at 15 ℃ for crystallization for 40h, and filtering; adding the obtained phytosterol crystals into the hickory crude oil obtained in the step 1), separating alcohol ester and natural VE from the filtrate through molecular distillation, and adding the natural VE into the hickory crude oil obtained in the step 1);
4) adding the phytosterol crystals in the step 3), and refrigerating the natural VE-containing pecan crude oil at the temperature of 3 ℃ for 36 hours; separating the supernatant of the crude walnut oil in a refrigeration environment, centrifuging the lower layer solid-liquid mixture of the crude walnut oil, and separating the supernatant again, wherein the centrifugation is realized by a centrifuge, the rotation speed of the centrifuge is 3000rpm, and the centrifugation time is 8 min; and combining the supernatants obtained by the two times of separation to obtain the walnut oil.
Example 2
A method for efficiently retaining natural VE and phytosterol in walnut oil comprises the following steps:
1) drying peeled pecan seeds at a low temperature of 60 ℃ until the water content is 6%, breaking the pecan seeds by using a shell breaking machine, and taking pure seeds, pure kernels or a seed kernel mixture formed by breaking the pecan seeds as a raw material for preparing oil by using a hydraulic oil press. Placing the pecan seeds dried at low temperature in a hydraulic oil press to prepare oil, stopping squeezing after the oil yield is 50%, and respectively collecting pecan crude oil and residue cake;
2) adding deionized water into the residue cake obtained in the step 1) according to the ratio of material to liquid of 1:7w/v, stirring in a 500rpm stirrer, standing, and removing residual shells; adjusting the pH of the mixed solution to 3, homogenizing in a homogenizer at 4000rpm for 1min, centrifuging the homogenized mixed solution in a centrifuge at 10000rpm for 15min to separate three phases of an oil phase, a water phase and residues, and drying the oil phase at 90 ℃ for 40min to dehydrate to obtain a water-extracted pecan oil;
3) esterifying and alcoholizing the water-extracted pecan oil obtained in the step 2), converting fatty acid and fatty acid ester contained in the water-extracted pecan oil into fatty acid methyl ester, naturally cooling at 10 ℃ for 15h for crystallization, and filtering; adding the obtained phytosterol crystals into the hickory crude oil obtained in the step 1), separating alcohol ester and natural VE from the filtrate through molecular distillation, and adding the natural VE into the hickory crude oil obtained in the step 1);
4) adding the phytosterol crystals in the step 3), and refrigerating the natural VE-containing pecan crude oil at the temperature of 2 ℃ for 24 hours; separating the supernatant of the crude walnut oil in a refrigeration environment, centrifuging the lower layer solid-liquid mixture of the crude walnut oil, and separating the supernatant again, wherein the centrifugation is realized by a centrifuge, the rotation speed of the centrifuge is 2000rpm, and the centrifugation time is 10 min; and mixing the supernatants obtained by the two times of separation to obtain the walnut oil.
Example 3
A method for efficiently retaining natural VE and phytosterol in walnut oil comprises the following steps:
1) drying peeled pecan seeds at a low temperature of 80 ℃ until the water content is 4%, breaking the pecan seeds by using a shell breaking machine, and taking pure seeds, pure kernels or a seed kernel mixture formed by breaking the pecan seeds as a raw material for preparing oil by using a hydraulic oil press. Placing the pecan seeds dried at low temperature in a hydraulic oil press to prepare oil, stopping squeezing after the oil yield is 55%, and respectively collecting pecan crude oil and residue cake;
2) adding deionized water into the residue cake obtained in the step 1) according to the ratio of material to liquid of 1:6w/v, stirring in a stirrer at 1000rpm, standing, and removing residual shells; adjusting pH of the mixed solution to 5, homogenizing at 2000rpm for 3min, centrifuging at 7000rpm for 30min to separate oil phase, water phase and residue, drying the oil phase at 70 deg.C for 60min, and dehydrating to obtain water-extracted oil of fructus Juglandis;
3) esterifying and alcoholizing the water-extracted pecan oil obtained in the step 2), converting fatty acid and fatty acid ester contained in the water-extracted pecan oil into fatty acid methyl ester, naturally cooling at 20 ℃ for 5 hours for crystallization, and filtering; adding the obtained phytosterol crystals into the pecan crude oil obtained in the step 1), separating alcohol ester and natural VE from the filtrate through molecular distillation, and adding the natural VE into the pecan crude oil obtained in the step 1);
4) adding the phytosterol crystals in the step 3), and refrigerating the natural VE-containing pecan crude oil at the temperature of 4 ℃ for 48 hours; separating the supernatant of the walnut crude oil in a refrigeration environment, centrifuging the lower layer solid-liquid mixture of the walnut crude oil, and separating the supernatant again, wherein the centrifugation is realized by a centrifuge, the rotation speed of the centrifuge is 4000rpm, and the centrifugation time is 5 min; and combining the supernatants obtained by the two times of separation to obtain the walnut oil.
Comparative example 1
A preparation method of walnut oil comprises the following steps:
1) drying peeled pecan seeds at 70 ℃ to water content of 5%, cracking the pecan seeds by using a cracker, and using pure seeds, pure kernels or a seed kernel mixture formed by cracking the pecan seeds as a raw material for preparing oil by using a hydraulic oil press. Placing the pecan seeds dried at low temperature into a hydraulic oil press to prepare oil, stopping squeezing after the oil yield is 52%, and collecting pecan crude oil;
2) refrigerating the hickory crude oil at 3 deg.C for 36 h; separating the supernatant of the crude walnut oil in a refrigeration environment, centrifuging the lower layer solid-liquid mixture of the crude walnut oil, and separating the supernatant again, wherein the centrifugation is realized by a centrifuge, the rotation speed of the centrifuge is 3000rpm, and the centrifugation time is 8 min; and combining the supernatants obtained by the two times of separation to obtain the walnut oil.
Comparative example 2
A preparation method of walnut oil comprises the following steps:
1) drying peeled pecan seeds at a low temperature of 60 ℃ until the water content is 6%, breaking the pecan seeds by using a shell breaking machine, and taking pure seeds, pure kernels or a seed kernel mixture formed by breaking the pecan seeds as a raw material for preparing oil by using a hydraulic oil press. Placing the pecan seeds dried at low temperature in a hydraulic oil press to prepare oil, stopping squeezing after the oil yield is 50%, and collecting pecan crude oil;
2) refrigerating the hickory crude oil at 2 deg.C for 24 hr; separating the supernatant of the crude walnut oil in a refrigeration environment, centrifuging the lower layer solid-liquid mixture of the crude walnut oil, and separating the supernatant again, wherein the centrifugation is realized by a centrifuge, the rotation speed of the centrifuge is 2000rpm, and the centrifugation time is 10 min; and mixing the supernatants obtained by the two times of separation to obtain the walnut oil.
Comparative example 3
A preparation method of walnut oil comprises the following steps:
1) drying peeled pecan seeds at a low temperature of 80 ℃ until the water content is 4%, breaking the pecan seeds by using a shell breaking machine, and taking pure seeds, pure kernels or a seed kernel mixture formed by breaking the pecan seeds as a raw material for preparing oil by using a hydraulic oil press. Placing the pecan seeds dried at low temperature in a hydraulic oil press to prepare oil, stopping squeezing after the oil yield is 55%, and collecting pecan crude oil;
2) refrigerating the hickory crude oil at 4 deg.C for 48 h; separating the supernatant of the walnut crude oil in a refrigeration environment, centrifuging the lower layer solid-liquid mixture of the walnut crude oil, and separating the supernatant again, wherein the centrifugation is realized by a centrifuge, the rotation speed of the centrifuge is 4000rpm, and the centrifugation time is 5 min; and mixing the supernatants obtained by the two times of separation to obtain the walnut oil.
Taking 60kg of peeled pecan seeds, dividing the peeled pecan seeds into 6 parts, treating each part according to the examples 1-3 and the comparative examples 1-3, and taking the comparative examples as reference objects to research the income condition brought by natural VE and phytosterol in the absorbed slag cakes. The results are as follows:
compared with the comparative example 1, the content of natural VE in the example 1 is increased by 18 percent, and the content of phytosterol is increased by 15 percent;
compared with the comparative example 2, the content of natural VE in the example 2 is increased by 17 percent, and the content of phytosterol is increased by 14 percent;
example 3 compared to comparative example 3, the content of natural VE was increased by 18% and the content of phytosterols by 14%.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (8)
1. A method for efficiently retaining natural VE and phytosterol in walnut oil is characterized by comprising the following steps:
1) drying peeled pecan seeds at a low temperature of 60-80 ℃ until the water content is 4-6%, putting the pecan seeds dried at the low temperature into a hydraulic oil press to prepare oil, stopping squeezing after the oil yield is 50-55%, and respectively collecting pecan crude oil and a residue cake;
2) adding deionized water into the residue cake obtained in the step 1) according to the material-liquid ratio of 1: 6-7 w/v, stirring in a stirrer at 500-1000 rpm, standing, and removing residual shells; adjusting the pH value of the mixed solution to 3-5, placing the mixed solution into a homogenizer for homogenization for 1-3 min, centrifuging the homogenized mixed solution in a centrifuge for 15-30 min to separate an oil phase, a water phase and residues, and drying the oil phase at 70-90 ℃ for 40-60 min to dehydrate to obtain the hickory water extract oil;
3) esterifying and alcoholizing the water-extracted pecan oil obtained in the step 2), converting fatty acid and fatty acid ester contained in the water-extracted pecan oil into fatty acid methyl ester, naturally cooling and crystallizing for 5-15 h at 10-20 ℃, and filtering; adding the obtained phytosterol crystals into the hickory crude oil obtained in the step 1), separating alcohol ester and natural VE from the filtrate through molecular distillation, and adding the natural VE into the hickory crude oil obtained in the step 1);
4) adding the phytosterol crystals into the mixture obtained in the step 3), refrigerating the crude pecan oil of natural VE, separating the supernatant of the crude pecan oil in a refrigerating environment, centrifuging the lower-layer solid-liquid mixture of the crude pecan oil, separating the supernatant again, and combining the supernatants obtained by two times of separation to obtain the walnut oil.
2. The method for efficiently retaining natural VE and phytosterols in walnut oil according to claim 1, wherein the method comprises the following steps: in the step 1), a shell breaking machine is adopted to break the shells of the hickory seeds, and pure seeds, pure kernels or a seed kernel mixture formed after the hickory seeds are broken is used as a raw material for preparing oil by a hydraulic oil press.
3. The method for efficiently retaining natural VE and phytosterols in walnut oil according to claim 1, wherein the method comprises the following steps: in the step 1), peeled pecan seeds are dried at a low temperature of 70 ℃ until the water content is 5 percent.
4. The method for efficiently retaining natural VE and phytosterols in walnut oil according to claim 1, wherein the method comprises the following steps: in the step 2), the pH value of the mixed solution is adjusted to be 4, the mixed solution is placed in a homogenizer at 2000-4000 rpm for homogenization for 1-3 min, and the homogenized mixed solution is centrifuged in a centrifuge at 7000-10000 rpm for 15-30 min.
5. The method for efficiently retaining natural VE and phytosterols in walnut oil according to claim 1, wherein the method comprises the following steps: in the step 2), drying the oil phase at 80 ℃ for 40-60 min, and dehydrating to obtain the water-extracted pecan oil.
6. The method for efficiently retaining natural VE and phytosterols in walnut oil according to claim 1, wherein the method comprises the following steps: in the step 3), naturally cooling and crystallizing for 10 hours at 15 ℃.
7. The method for efficiently retaining natural VE and phytosterols in walnut oil according to claim 1, wherein the method comprises the following steps: in the step 4), the temperature of the cold storage treatment is 2-4 ℃, and the cold storage time is 24-48 h.
8. The method for efficiently retaining natural VE and phytosterols in walnut oil according to claim 1, wherein the method comprises the following steps: in the step 4), the centrifugal treatment is realized by a centrifugal machine, the rotating speed of the centrifugal machine is 2000-4000 rpm, and the centrifugal time is 5-10 min.
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