CN112430501A - Degumming method of cornus wisoniana raw oil - Google Patents
Degumming method of cornus wisoniana raw oil Download PDFInfo
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- 241001477876 Cornus wilsoniana Species 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 33
- 239000003921 oil Substances 0.000 claims abstract description 107
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000012535 impurity Substances 0.000 claims abstract description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000006243 chemical reaction Methods 0.000 claims abstract description 28
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 27
- 238000003756 stirring Methods 0.000 claims abstract description 23
- 238000001914 filtration Methods 0.000 claims abstract description 21
- ZIIUUSVHCHPIQD-UHFFFAOYSA-N 2,4,6-trimethyl-N-[3-(trifluoromethyl)phenyl]benzenesulfonamide Chemical compound CC1=CC(C)=CC(C)=C1S(=O)(=O)NC1=CC=CC(C(F)(F)F)=C1 ZIIUUSVHCHPIQD-UHFFFAOYSA-N 0.000 claims abstract description 19
- 102000015439 Phospholipases Human genes 0.000 claims abstract description 19
- 108010064785 Phospholipases Proteins 0.000 claims abstract description 19
- 102000004190 Enzymes Human genes 0.000 claims abstract description 16
- 108090000790 Enzymes Proteins 0.000 claims abstract description 16
- 238000006911 enzymatic reaction Methods 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 13
- 238000010907 mechanical stirring Methods 0.000 claims abstract description 12
- 239000010779 crude oil Substances 0.000 claims abstract description 10
- 230000002255 enzymatic effect Effects 0.000 claims abstract description 10
- 238000004321 preservation Methods 0.000 claims abstract description 10
- 238000010008 shearing Methods 0.000 claims abstract description 10
- 235000011121 sodium hydroxide Nutrition 0.000 claims abstract description 9
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 9
- 239000012153 distilled water Substances 0.000 claims abstract description 7
- 238000001704 evaporation Methods 0.000 claims abstract description 7
- 230000018044 dehydration Effects 0.000 claims abstract description 3
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 24
- 235000013399 edible fruits Nutrition 0.000 claims description 23
- 230000036571 hydration Effects 0.000 claims description 20
- 238000006703 hydration reaction Methods 0.000 claims description 20
- 230000008569 process Effects 0.000 claims description 11
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 8
- 239000011780 sodium chloride Substances 0.000 claims description 8
- 241000759832 Cornus walteri Species 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 238000000703 high-speed centrifugation Methods 0.000 claims description 6
- 230000000415 inactivating effect Effects 0.000 claims description 6
- 239000012267 brine Substances 0.000 claims description 3
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims description 3
- 238000002390 rotary evaporation Methods 0.000 claims description 2
- 238000007738 vacuum evaporation Methods 0.000 claims description 2
- 238000012545 processing Methods 0.000 abstract description 3
- 230000000887 hydrating effect Effects 0.000 abstract 1
- 235000019198 oils Nutrition 0.000 description 89
- 150000003904 phospholipids Chemical class 0.000 description 19
- 241000209020 Cornus Species 0.000 description 9
- 108010013563 Lipoprotein Lipase Proteins 0.000 description 6
- 102100022119 Lipoprotein lipase Human genes 0.000 description 6
- 238000001514 detection method Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- 229920000159 gelatin Polymers 0.000 description 3
- 239000008273 gelatin Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 108010093096 Immobilized Enzymes Proteins 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 238000009874 alkali refining Methods 0.000 description 2
- 229960000892 attapulgite Drugs 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 2
- 235000014113 dietary fatty acids Nutrition 0.000 description 2
- 239000000194 fatty acid Substances 0.000 description 2
- 229930195729 fatty acid Natural products 0.000 description 2
- 150000004665 fatty acids Chemical class 0.000 description 2
- 239000004519 grease Substances 0.000 description 2
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 2
- 239000004005 microsphere Substances 0.000 description 2
- 229910052625 palygorskite Inorganic materials 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
- 241001391944 Commicarpus scandens Species 0.000 description 1
- 241000142975 Cornaceae Species 0.000 description 1
- OYHQOLUKZRVURQ-HZJYTTRNSA-N Linoleic acid Chemical compound CCCCC\C=C/C\C=C/CCCCCCCC(O)=O OYHQOLUKZRVURQ-HZJYTTRNSA-N 0.000 description 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
- 235000021314 Palmitic acid Nutrition 0.000 description 1
- 235000019483 Peanut oil Nutrition 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 230000003044 adaptive effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000010495 camellia oil Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000001877 deodorizing effect Effects 0.000 description 1
- 239000008157 edible vegetable oil Substances 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- 235000020778 linoleic acid Nutrition 0.000 description 1
- OYHQOLUKZRVURQ-IXWMQOLASA-N linoleic acid Natural products CCCCC\C=C/C\C=C\CCCCCCCC(O)=O OYHQOLUKZRVURQ-IXWMQOLASA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 239000004006 olive oil Substances 0.000 description 1
- 235000008390 olive oil Nutrition 0.000 description 1
- 239000000312 peanut oil Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000003549 soybean oil Substances 0.000 description 1
- 235000012424 soybean oil Nutrition 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 1
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
- 239000008158 vegetable oil Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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
- 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
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Microbiology (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention provides a degumming method of cornus wisoniana crude oil, which comprises the steps of filtering and removing impurities, hydrating and degumming, and degumming and layering and dehydrating by an ultrasonic-assisted enzyme method. The ultrasonic-assisted enzymatic degumming comprises the following steps: heating the hydrated and degummed oil to 60-90 ℃, adding an oxalic acid solution, carrying out heat preservation and stirring reaction for 20-30min, then reducing the temperature to 47-52 ℃, adding a caustic soda solution to adjust the pH value to 4.5-6.0, then adding 1-3% of distilled water and immobilized phospholipase, carrying out high-speed shearing and stirring for 30-60s, quickly transferring an enzyme reaction system to an ultrasonic reactor with a mechanical stirring device and capable of controlling the water bath temperature, and continuously reacting for 1-2.5h under the heat preservation condition by adopting ultrasonic treatment with the power of 100 and 150W in combination with mechanical stirring. And the layered dehydration comprises heating to inactivate enzyme, shearing at high speed, stirring, centrifuging, collecting the upper oil layer, and vacuum evaporating to remove water to obtain the degummed oil. The method can improve the degumming rate of cornus wisoniana crude oil, shorten the processing time of the crude oil and improve the phase of finished oil.
Description
Technical Field
The invention relates to the technical field of vegetable oil processing, in particular to a degumming method of cornus wisoniana raw oil.
Background
Cornus walteri fruit oil is prepared from Cornus walteri fruit of Cornus of Cornaceae by squeezing, filtering, decolorizing, deodorizing, etc. The fatty acid composition (based on the total fatty acid content) contains linoleic acid (C18: 2) not less than 38%, oleic acid (C18: 1) not less than 20%, and palmitic acid (C16: 0) not less than 15%.
Cornus wisoniana fruit oil is a high-quality woody edible vegetable oil newly discovered in China, is rich in unsaturated fatty acid and beneficial trace components, has higher edible value than soybean oil and peanut oil, and can be compared favorably with tea oil and olive oil after being refined. In 2013, cornus wisoniana oil is approved by the national health committee as a new food raw material, and a foundation is laid for industrialization and marketization of cornus wisoniana oil. The cornus wisoniana fruit contains a large amount of pigment and resin, and the cornus wisoniana fruit oil can enter oil in the squeezing process of the cornus wisoniana fruit oil, so that the cornus wisoniana fruit crude oil contains a large amount of colloid. The existence of colloid not only reduces the quality of the grease, but also can promote the excessive emulsification between the grease and the alkali liquor in the alkali refining deacidification process, increase the separation difficulty of the alkali refining nigre and aggravate the loss of neutral oil. At the same time, it is not beneficial to the operation of other refining processes. Therefore, it must be removed cleanly.
At present, the degumming method is most widely applied to hydration degumming, but the hydration degumming effect is not ideal due to the high content of phospholipids in the raw oil of cornus wisoniana. Therefore, the method aims at the characteristics of cornus wisoniana oil, researches and improves the degumming process of the cornus wisoniana oil, and is urgent to solve the problems of incomplete degumming, low efficiency and the like of the cornus wisoniana oil.
Disclosure of Invention
Technical problem to be solved
In view of the above disadvantages and shortcomings of the prior art, the present invention provides a method for degumming raw cornus wisonii fruit oil, so as to improve the degumming rate of raw cornus wisonii fruit oil, shorten the processing time of raw oil, and improve the product phase of the finished oil.
(II) technical scheme
In order to achieve the purpose, the invention adopts the main technical scheme that:
a degumming method of cornus wisoniana raw oil comprises the following steps:
s1, filtering and removing impurities: carrying out high-speed centrifugation and impurity removal on the squeezed cornus wisoniana crude oil, and then filtering and impurity removal to obtain the cornus wisoniana crude oil subjected to preliminary impurity removal;
s2, hydration degumming: heating crude Cornus walteri fruit oil subjected to preliminary impurity removal to 60-90 ℃, adding saline water with the temperature of +/-3 ℃ of the crude Cornus walteri fruit oil, preserving heat, stirring for 15-30min (preferably 20-30 min), carrying out hydration degumming treatment, then centrifuging, and filtering to remove peptized impurities to obtain hydrated degummed oil;
s3, ultrasonic-assisted enzymatic degumming: heating the hydrated degummed oil to 60-90 ℃, adding an oxalic acid solution with the temperature of +/-3 ℃ of the temperature of the hydrated degummed oil, preserving heat, stirring, reacting for 20-30min, then cooling to 47-52 ℃, adding a caustic soda solution, adjusting the pH of a reaction system to 4.5-6.0, adding 1-3% of distilled water and immobilized phospholipase, wherein the addition amount of the immobilized phospholipase is 25-35mg/Kg of the hydrated degummed oil; after shearing and stirring at a high speed for 30-60s, quickly moving an enzyme reaction system into an ultrasonic reactor which is provided with a mechanical stirring device and can control the temperature of water bath, and continuously reacting for 1-2.5h (preferably 90-120 min) under the condition of heat preservation by adopting ultrasonic treatment with the power of 100-;
s4, layered dehydration: after the enzyme reaction is finished, raising the temperature of the reaction system to 95 ℃, inactivating the enzyme for 5-15min (preferably sterilizing for 10 min), then centrifuging for 20-60min (preferably 30 min) under the condition of high-speed shearing and stirring, collecting the upper oil layer, and evaporating in vacuum to remove water to obtain the degummed oil.
In S2, the temperature of the added salt water is the same as the temperature of cornus wisoniana raw oil.
According to a preferred embodiment of the present invention, in S2, the mass volume fraction of the added brine is 0.18 to 0.22%, preferably 0.2%.
According to the preferred embodiment of the present invention, the amount of the saline water used in S2 is 4.5 to 5.5mL/100g cornus wisoniana raw oil, preferably 5mL/100g cornus wisoniana raw oil.
In S3, the temperature of the oxalic acid solution is the same as the temperature of the hydrated degummed oil.
According to the preferred embodiment of the present invention, in S3, the concentration of oxalic acid solution is 18-22% by mass, preferably 20% by mass.
According to the preferred embodiment of the present invention, in S3, the oxalic acid solution is added in an amount of 0.48 to 0.55%, preferably 0.5% by weight of the degummed oil hydrate.
According to a preferred embodiment of the present invention, the concentration of the caustic soda solution in S3 is 3.5 to 4.5% by mass, preferably 4% by mass.
According to the preferred embodiment of the invention, in S3, the addition amount of the immobilized phospholipase is 30mg/Kg of hydrated degummed oil; the high-speed shear stirring is 8000-11000 rpm.
According to the preferred embodiment of the present invention, in S4, the vacuum evaporation condition is rotary evaporation at 80 ℃ and 0.09 MPa.
The immobilized phospholipase is an immobilized enzyme which is obtained by binding water-soluble free enzyme molecules in a certain interval (on a water-insoluble carrier) through physical and/or chemical action and recycling the enzyme by a simple separation method (such as centrifugal sedimentation) after use for multiple times.
In the present invention, sodium alginate-gelatin immobilized phospholipase (phospholipase a1) microspheres are preferably used. The microsphere has regular pits on the surface, has strong strength and toughness, is not easy to break when being used repeatedly for degumming, has light specific gravity, is homogenized in a reaction system by stirring and ultrasonic waves, and is not easy to concentrate at the bottom of the reaction system. In addition, the immobilized phospholipase A1 modified by the silane coupling agent and immobilized by attapulgite can be used, and the immobilized enzyme has widely adaptive reaction conditions, strong thermal stability and can adapt to a wider pH range.
(III) advantageous effects
The invention discloses a degumming method of cornus wisoniana raw oil, which comprises the steps of firstly carrying out hydration degumming to remove hydrated phospholipid, then further degumming the cornus wisoniana raw oil by adopting immobilized phospholipase, and carrying out stirring and ultrasonic treatment in the degumming process by using the immobilized phospholipase, thereby achieving the purpose of thorough degumming. The degumming of the immobilized phospholipase not only can improve the activity and stability of the enzyme in a reaction system, realize the separation and the repeated use of the enzyme, and greatly reduce the application cost of the enzyme.
Ultrasonic treatment with specific power is applied in the enzymatic degumming process, wherein the application of ultrasonic can cause the micro-change of enzyme molecular conformation, so that the ultramicro structure of enzyme molecules is more reasonable, and active functional groups (breaking through steric hindrance under the action of ultrasonic) of the enzyme molecules are more easily combined with reactants, thereby showing higher catalytic activity. In addition, the ultrasonic wave increases the homogenization degree of a reaction system, increases the mass transfer speed of the enzymolysis reaction and improves the degumming efficiency. Cavitation bubbles generated by the ultrasonic cavitation effect increase the interfacial area of the enzyme-catalyzed reaction when the immiscible multiphase boundary is broken. In conclusion, the degumming rate of the hydrated degumming oil is enhanced, the oil quality phase is improved, the phospholipid content is reduced, and the degumming time is shortened by adopting the ultrasonic-assisted enzymatic degumming.
The degumming process can obviously shorten the enzymatic degumming reaction time of cornus wisoniana raw oil, improve the degumming effect, meet the requirement of subsequent physical refining, reduce the generation amount of degumming wastewater, play a positive role in protecting the surrounding environment, and have potential advantages in the aspects of environmental protection and quality.
Detailed Description
For the purpose of better explaining the present invention and to facilitate understanding, the present invention will be described in detail below with reference to specific embodiments.
To further illustrate the degumming process according to the invention, reference is made to the following examples.
Example 1
The embodiment provides a degumming method of cornus wisoniana raw oil, which comprises the following steps:
(1) and (3) filtering and removing impurities: placing squeezed cornus wisoniana raw oil (the initial phospholipid content is 19.692 mg/g) in a centrifugal filter, and removing impurities after high-speed centrifugation to obtain the cornus wisoniana raw oil after filtration and impurity removal.
(2) Hydration degumming: heating the raw oil of cornus wisoniana after impurity removal to 80 ℃, adding 82 ℃ saline water (the mass volume concentration is 0.2%) according to the dosage ratio of 5mL/100g of raw oil, keeping the temperature at 80 ℃, stirring for 30min for hydration degumming treatment, and after the reaction is finished, centrifuging again and filtering to remove peptizing impurities to obtain the hydration degummed oil.
(3) Ultrasonic-assisted enzymatic degumming: heating the hydrated degummed oil to 80 ℃, adding an oxalic acid solution (the concentration is 20 wt%) at 82 ℃, the addition amount of which is 0.5 percent of the weight of the oil, carrying out heat preservation and stirring reaction for 30min, then cooling to 50 ℃, adding an NaOH solution with the mass concentration of 4 percent, adjusting the pH value of a reaction system to 5.0, adding distilled water and immobilized phospholipase (sodium alginate-gelatin immobilized phospholipase A1) with the weight of 2.5 percent of the oil, carrying out high-speed shearing at 10000 r/min for 60s, quickly transferring the enzyme reaction system to an ultrasonic reactor with a mechanical stirring device and capable of controlling the water bath temperature, and continuously carrying out reaction for 2h by adopting ultrasonic treatment with the power of 150W and mechanical stirring under the heat preservation condition.
(4) Layering and dehydrating: and after the enzyme reaction is finished, raising the temperature of the reaction system to 95 ℃, inactivating the enzyme for 10min, centrifuging for 30min under the condition of 10000 r/min, collecting an upper oil layer, and rotationally evaporating at the temperature of 80 ℃ under the condition of 0.09Mpa to remove water to finally obtain the degummed cornus wisonii fruit oil.
Analysis and detection prove that the content of phospholipid in the degummed cornus wisonii fruit oil is 0.288mg/g, and the phospholipid removal rate reaches 98.54%.
Example 2
The embodiment provides a degumming method of cornus wisoniana raw oil, which comprises the following steps:
(1) and (3) filtering and removing impurities: placing squeezed cornus wisoniana raw oil (the initial phospholipid content is 19.692 mg/g) in a centrifugal filter, and removing impurities after high-speed centrifugation to obtain the cornus wisoniana raw oil after filtration and impurity removal.
(2) Hydration degumming: heating the raw oil of cornus wisoniana after impurity removal to 80 ℃, adding 80 ℃ saline water (the mass volume concentration is 0.21%) according to the dosage ratio of 5.5mL/100g of the raw oil, keeping the temperature at 80 ℃, stirring for 30min for hydration degumming, and after the reaction is finished, centrifuging again and filtering to remove peptizing impurities to obtain the hydration degummed oil.
(3) Ultrasonic-assisted enzymatic degumming: heating the hydrated degummed oil to 85 ℃, adding oxalic acid solution (the concentration is 19.5 wt%) with the temperature of 85 ℃ and the addition amount of 0.48 percent of the weight of the oil, keeping the temperature and stirring for reaction for 30min, then cooling the temperature to 50 ℃, adding NaOH solution with the mass concentration of 4.2 percent, adjusting the pH value of a reaction system to 4.5, adding distilled water with the weight of 3 percent of the weight of the oil and immobilized phospholipase (sodium alginate-gelatin immobilized phospholipase A1), adding 32mg/Kg of the oil into the immobilized phospholipase, shearing the immobilized phospholipase at a high speed of 10000 r/min for 60s, quickly transferring the enzyme reaction system into an ultrasonic reactor with a mechanical stirring device and capable of controlling the water bath temperature, and continuously reacting for 150min by adopting ultrasonic treatment with the power of 100W and mechanical stirring under the condition of keeping the temperature.
(4) Layering and dehydrating: and after the enzyme reaction is finished, raising the temperature of the reaction system to 95 ℃, inactivating the enzyme for 10min, centrifuging for 60min at 8000 r/min, collecting an upper oil layer, and rotationally evaporating at 0.09Mpa and 80 ℃ to remove water to finally obtain the degummed cornus wisonii fruit oil.
Analysis and detection prove that the content of phospholipid in the degummed cornus wisoniana fruit oil is 0.266mg/g, and the phospholipid removal rate reaches 98.65%.
Example 3
The embodiment provides a degumming method of cornus wisoniana raw oil, which comprises the following steps:
(1) and (3) filtering and removing impurities: placing squeezed cornus wisoniana raw oil (the initial phospholipid content is 19.692 mg/g) in a centrifugal filter, and removing impurities after high-speed centrifugation to obtain the cornus wisoniana raw oil after filtration and impurity removal.
(2) Hydration degumming: heating the crude oil of cornus wisoniana after impurity removal to 70 ℃, adding 75 ℃ saline (the mass volume concentration is 0.22%) according to the dosage ratio of 4.5mL/100g of crude oil, keeping the temperature at 70 ℃, stirring for 30min for hydration degumming, and after the reaction is finished, centrifuging again and filtering to remove peptizing impurities to obtain the hydration degummed oil.
(3) Ultrasonic-assisted enzymatic degumming: heating the hydrated degummed oil to 75 ℃, adding oxalic acid solution (the concentration is 20 wt%) at 75 ℃ and the addition amount is 0.48 percent of the weight of the oil, carrying out heat preservation and stirring reaction for 30min, then cooling to 52 ℃, adding NaOH solution with the mass concentration of 4%, adjusting the pH value of a reaction system to 6, adding distilled water and immobilized phospholipase (attapulgite-immobilized phospholipase A1) with the addition amount of 2 percent of the weight of the oil, carrying out 10000 r/min high-speed shearing for 60s, quickly transferring an enzyme reaction system to an ultrasonic reactor with a mechanical stirring device and capable of controlling the water bath temperature, and continuously reacting for 2h by adopting ultrasonic treatment with the power of 150W and mechanical stirring under the heat preservation condition.
(4) Layering and dehydrating: and after the enzyme reaction is finished, raising the temperature of the reaction system to 95 ℃, inactivating the enzyme for 10min, centrifuging for 30min under the condition of 10000 r/min, collecting an upper oil layer, and rotationally evaporating at the temperature of 80 ℃ under the condition of 0.09Mpa to remove water to finally obtain the degummed cornus wisonii fruit oil.
Analysis and detection prove that the content of phospholipid in the degummed cornus wisonii fruit oil is 0.274mg/g, and the phospholipid removal rate reaches 98.61%.
Example 4
The embodiment provides a degumming method of cornus wisoniana raw oil, which comprises the following steps:
(1) and (3) filtering and removing impurities: placing squeezed cornus wisoniana raw oil (the initial phospholipid content is 19.692 mg/g) in a centrifugal filter, and removing impurities after high-speed centrifugation to obtain the cornus wisoniana raw oil after filtration and impurity removal.
(2) Hydration degumming: heating the raw oil of cornus wisoniana after impurity removal to 90 ℃, adding 90 ℃ saline water (the mass volume concentration is 0.2%) according to the dosage ratio of 5mL/100g of raw oil, keeping the temperature at 90 ℃, stirring for 30min for hydration degumming treatment, and after the reaction is finished, centrifuging again and filtering to remove peptizing impurities to obtain hydration degummed oil.
(3) Ultrasonic-assisted enzymatic degumming: heating the hydrated degummed oil to 85 ℃, adding oxalic acid solution (the concentration is 20 wt%) with the temperature of 85 ℃ and the addition amount of 0.5 percent of the weight of the oil, carrying out heat preservation and stirring reaction for 30min, then cooling to 51 ℃, adding NaOH solution with the mass concentration of 4 percent, adjusting the pH value of a reaction system to 6, adding distilled water with the weight of 2 percent of the weight of the oil and immobilized phospholipase (phospholipase A1 immobilized by attapulgite), wherein the addition amount of the immobilized phospholipase is 32mg/Kg of the oil, rapidly transferring an enzyme reaction system into an ultrasonic reactor with a mechanical stirring device and capable of controlling the water bath temperature after 10000 r/min high-speed shearing for 60s, and continuously reacting for 2h by adopting ultrasonic treatment with the power of 150W and mechanical stirring under the heat preservation condition.
(4) Layering and dehydrating: and after the enzyme reaction is finished, raising the temperature of the reaction system to 95 ℃, inactivating the enzyme for 10min, centrifuging for 30min under the condition of 10000 r/min, collecting an upper oil layer, and rotationally evaporating at the temperature of 80 ℃ under the condition of 0.09Mpa to remove water to finally obtain the degummed cornus wisonii fruit oil.
Analysis and detection prove that the content of phospholipid in the degummed cornus wisoniana fruit oil is 0.270mg/g, and the phospholipid removal rate reaches 98.63%.
Comparative example 1
In the comparative example, on the basis of the example 1, the step of hydration degumming is removed, and the raw oil of cornus wisoniana after filtration and impurity removal is directly processed in the step (3).
Analysis and detection prove that the content of phospholipid in the degummed cornus wisoniana fruit oil is 6.593mg/g, and the phospholipid removal rate reaches 66.5%.
Comparative example 2
This comparative example was based on example 1 and the enzyme reaction temperature was lowered to 42 ℃. Analysis and detection prove that the phospholipid content in the degummed cornus wisoniana fruit oil is 1.886mg/g, and the phospholipid removal rate reaches 90.42%.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. A degumming method of cornus wisoniana raw oil is characterized by comprising the following steps:
s1, filtering and removing impurities: carrying out high-speed centrifugation and impurity removal on the squeezed cornus wisoniana crude oil, and then filtering and impurity removal to obtain the cornus wisoniana crude oil subjected to preliminary impurity removal;
s2, hydration degumming: heating crude Cornus walteri fruit oil subjected to preliminary impurity removal to 60-90 ℃, adding saline water with the temperature of the crude Cornus walteri fruit oil being +/-3 ℃, preserving heat, stirring for 15-30min, carrying out hydration degumming treatment, then centrifuging, and filtering to remove peptized impurities to obtain hydrated degummed oil;
s3, ultrasonic-assisted enzymatic degumming: heating the hydrated degummed oil to 60-90 ℃, adding an oxalic acid solution with the temperature of +/-3 ℃ of the temperature of the hydrated degummed oil, preserving heat, stirring, reacting for 20-30min, then cooling to 47-52 ℃, adding a caustic soda solution, adjusting the pH of a reaction system to 4.5-6.0, adding 1-3% of distilled water and immobilized phospholipase, wherein the addition amount of the immobilized phospholipase is 25-35mg/Kg of the hydrated degummed oil; after shearing and stirring at a high speed for 30-60s, quickly transferring an enzyme reaction system to an ultrasonic reactor which is provided with a mechanical stirring device and can control the temperature of water bath, and continuously reacting for 1-2.5h under the condition of heat preservation by adopting ultrasonic treatment with the power of 100-;
s4, layered dehydration: and after the enzyme reaction is finished, raising the temperature of the reaction system to 95 ℃, inactivating the enzyme for 5-15min, centrifuging for 20-60min under the condition of high-speed shearing and stirring, collecting an upper oil layer, and evaporating in vacuum to remove water to obtain the degummed oil.
2. The degumming process according to claim 1, wherein in S2 the temperature of the added brine is the same as the temperature of cornus wisoniana raw oil.
3. The degumming process according to claim 1, wherein the S2, the saline water is added in a mass volume fraction of 0.18-0.22%.
4. The degumming method according to claim 1, wherein in S2 the amount of brine is 4.5-5.5mL/100g cornus wisoniana raw oil.
5. The degumming method according to claim 1, wherein in S3, the temperature of the oxalic acid solution is the same as the temperature of the hydrated degummed oil.
6. The degumming method according to claim 1, wherein in S3, the mass percentage concentration of the oxalic acid solution is 18-22%.
7. The degumming method according to claim 1, wherein in S3, the oxalic acid solution is added in an amount of 0.48-0.55% by weight of the hydrated degummed oil.
8. The degumming method according to claim 1, wherein the concentration of the caustic soda solution in S3 is 3.5-4.5% by weight.
9. The degumming method according to claim 1, wherein in S3, the addition amount of the immobilized phospholipase is 30mg/Kg of hydrated degummed oil; the high-speed shear stirring is 8000-11000 rpm.
10. The degumming process according to claim 1, wherein in S4, the vacuum evaporation conditions are rotary evaporation at 80 ℃ and 0.09 Mpa.
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