CN109234007B - Fish oil degumming and decoloring method - Google Patents
Fish oil degumming and decoloring method Download PDFInfo
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- CN109234007B CN109234007B CN201811200799.3A CN201811200799A CN109234007B CN 109234007 B CN109234007 B CN 109234007B CN 201811200799 A CN201811200799 A CN 201811200799A CN 109234007 B CN109234007 B CN 109234007B
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- 235000021323 fish oil Nutrition 0.000 title claims abstract description 61
- 238000000034 method Methods 0.000 title claims abstract description 37
- 102000004190 Enzymes Human genes 0.000 claims abstract description 35
- 108090000790 Enzymes Proteins 0.000 claims abstract description 35
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- 150000003839 salts Chemical class 0.000 claims abstract description 17
- 239000002904 solvent Substances 0.000 claims abstract description 12
- 230000002209 hydrophobic effect Effects 0.000 claims abstract description 9
- 239000003960 organic solvent Substances 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 25
- 108090001060 Lipase Proteins 0.000 claims description 18
- 239000004367 Lipase Substances 0.000 claims description 18
- 102000004882 Lipase Human genes 0.000 claims description 18
- 235000019421 lipase Nutrition 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 14
- 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 description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
- 102000015439 Phospholipases Human genes 0.000 claims description 13
- 108010064785 Phospholipases Proteins 0.000 claims description 13
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 9
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- IQQRAVYLUAZUGX-UHFFFAOYSA-N 1-butyl-3-methylimidazolium Chemical compound CCCCN1C=C[N+](C)=C1 IQQRAVYLUAZUGX-UHFFFAOYSA-N 0.000 claims description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 4
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 claims description 4
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 4
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 4
- 235000011152 sodium sulphate Nutrition 0.000 claims description 4
- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 claims description 4
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 3
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 3
- KYCQOKLOSUBEJK-UHFFFAOYSA-M 1-butyl-3-methylimidazol-3-ium;bromide Chemical compound [Br-].CCCCN1C=C[N+](C)=C1 KYCQOKLOSUBEJK-UHFFFAOYSA-M 0.000 claims description 2
- NJMWOUFKYKNWDW-UHFFFAOYSA-N 1-ethyl-3-methylimidazolium Chemical compound CCN1C=C[N+](C)=C1 NJMWOUFKYKNWDW-UHFFFAOYSA-N 0.000 claims description 2
- WXMVWUBWIHZLMQ-UHFFFAOYSA-N 3-methyl-1-octylimidazolium Chemical compound CCCCCCCCN1C=C[N+](C)=C1 WXMVWUBWIHZLMQ-UHFFFAOYSA-N 0.000 claims description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- 241000222175 Diutina rugosa Species 0.000 claims description 2
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- 101000968489 Rhizomucor miehei Lipase Proteins 0.000 claims description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 2
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 claims description 2
- 229910000402 monopotassium phosphate Inorganic materials 0.000 claims description 2
- 235000019796 monopotassium phosphate Nutrition 0.000 claims description 2
- 239000003208 petroleum Substances 0.000 claims description 2
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 claims description 2
- 229910000160 potassium phosphate Inorganic materials 0.000 claims description 2
- 235000011009 potassium phosphates Nutrition 0.000 claims description 2
- 238000007670 refining Methods 0.000 claims description 2
- 239000001509 sodium citrate Substances 0.000 claims description 2
- 235000011083 sodium citrates Nutrition 0.000 claims description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims 1
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 1
- 239000012071 phase Substances 0.000 abstract description 46
- 239000007791 liquid phase Substances 0.000 abstract description 21
- 235000013305 food Nutrition 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 description 10
- 239000000084 colloidal system Substances 0.000 description 8
- 239000003513 alkali Substances 0.000 description 7
- 239000007790 solid phase Substances 0.000 description 7
- 239000003921 oil Substances 0.000 description 6
- 235000019198 oils Nutrition 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 238000005119 centrifugation Methods 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 238000011049 filling Methods 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 150000003904 phospholipids Chemical class 0.000 description 3
- 229910052698 phosphorus Inorganic materials 0.000 description 3
- 239000011574 phosphorus Substances 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 238000000855 fermentation Methods 0.000 description 2
- 230000004151 fermentation Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 238000007086 side reaction Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 230000001093 anti-cancer Effects 0.000 description 1
- 230000036772 blood pressure Effects 0.000 description 1
- 230000004641 brain development Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 208000029078 coronary artery disease Diseases 0.000 description 1
- 239000003712 decolorant Substances 0.000 description 1
- 230000006806 disease prevention Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229940113115 polyethylene glycol 200 Drugs 0.000 description 1
- 229940068918 polyethylene glycol 400 Drugs 0.000 description 1
- 229940057847 polyethylene glycol 600 Drugs 0.000 description 1
- 235000020777 polyunsaturated fatty acids Nutrition 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000000108 ultra-filtration Methods 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
- C11B3/003—Refining fats or fatty oils by enzymes or microorganisms, living or dead
-
- 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
- C11B3/006—Refining fats or fatty oils by extraction
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Microbiology (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Biochemistry (AREA)
- Fats And Perfumes (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
- Edible Oils And Fats (AREA)
Abstract
本发明属于生物工程与食品技术领域，公开了一种鱼油脱胶脱色方法，包括以下步骤：(1)配置磷脂酶或/和脂肪酶浓度为1‑5000U/mL的酶液，向酶液中添加可溶性盐、亲水性溶剂和鱼油，配成三液相体系；(2)将配置好的三液相体系置于搅拌条件下反应，反应结束后，静置或离心至分四层，收集最上层的鱼油相；(3)将鱼油相加入碱液，然后加入疏水性有机溶剂，静置后取上相，回收疏水性有机溶剂，取萃取上相为精制鱼油。本发明提供了一种利用酶与多液相结合同步从粗鱼油中脱胶、脱色的方法，使工艺得以简化，处理时间短，成本降低，经济可行。The invention belongs to the technical field of bioengineering and food, and discloses a method for degumming and decolorizing fish oil. Soluble salt, hydrophilic solvent and fish oil are made into a three-phase system; (2) the prepared three-phase system is placed under stirring conditions to react, and after the reaction is completed, stand or centrifuge until it is divided into four layers, and collect the most The fish oil phase of the upper layer; (3) adding the fish oil phase to the lye, then adding the hydrophobic organic solvent, taking the upper phase after standing, recovering the hydrophobic organic solvent, and extracting the upper phase to obtain the refined fish oil. The invention provides a method for degumming and decolorizing crude fish oil synchronously by utilizing the combination of enzymes and multiple liquid phases, which simplifies the process, shortens the treatment time, reduces the cost and is economically feasible.
Description
Technical Field
The invention belongs to the technical field of bioengineering and food, relates to a separation and application technology of enzyme, and particularly relates to a method for pretreating crude fish oil by an enzyme method, degumming and decoloring.
Background
In recent years, fish oil has been the most important variety of functional oils because of its rich polyunsaturated fatty acids, and has the effects of anticancer, coronary heart disease prevention, blood pressure lowering, brain development promotion, etc., and has received wide attention at home and abroad. However, the raw material, i.e. crude fish oil, has the factors of many impurities, high chromaticity, complex components and the like, so that the raw material is difficult to decolorize and degum, the process is complex, the steps are complicated, and the loss rate is high, which has become a technical problem which troubles fish oil enterprises for many years, so that the development of simple and efficient refining technology is urgently needed.
In recent decades, scientists have made a series of attempts to decolorize and degum crude fish oil, but it has been a great difficulty to develop an economical and industrially feasible process. At present, the fish oil decoloring technology mainly comprises clay, active carbon and other adsorbents for adsorption decoloring, but the technological process is complex, the equipment requirement is high, and the requirements on operators are also very high. However, the development of high-quality and low-cost decolorants leads to long time consumption of the process and large production cost and time cost. In addition, the fish oil also contains mucoid impurities such as phospholipid, and the phospholipid colloid impurities are removed by treatment with water, acid, alkali or enzyme, but the fish oil usually needs multi-step washing, so that the process is complicated, the cost is high, the color of the fish oil is easily deepened, and the pretreatment difficulty is further improved. In general, the problems of complicated process, more side reactions, high energy consumption, long time and the like of the conventional fish oil pretreatment technology severely restrict the large-scale application of the fish oil.
Disclosure of Invention
The invention aims to provide a method for synchronously degumming and decoloring crude fish oil by combining enzyme and multiple liquids, aiming at the problems of complex process, more side reactions, high energy consumption, long time and the like in the existing degumming and decoloring process of the crude fish oil.
The purpose of the invention is realized by the following technical scheme:
a fish oil degumming and decoloring method comprises the following steps:
(1) preparing enzyme solution with phospholipase or/and lipase concentration of 1-5000U/mL, adding soluble salt, hydrophilic solvent and fish oil into the enzyme solution, and preparing into three-liquid-phase system; the mass ratio of the soluble salt, the hydrophilic solvent and the fish oil to the enzyme solution is 0.05-2, 0.01-0.8 and 0.01-6 respectively;
(2) reacting the prepared three-liquid phase system under stirring, standing or centrifuging to divide into four layers (the uppermost layer is a fish oil phase; the second layer is a solid phase rich in colloid, the third layer and the fourth layer are respectively an alcohol-rich phase or a salt-rich phase, and enzyme is mainly concentrated in one of the two phases), and collecting the fish oil phase at the uppermost layer;
(3) adding 0.2-8mol/L alkali solution into fish oil phase, adding 0.02-2 times volume of hydrophobic organic solvent, standing, collecting upper phase, recovering hydrophobic organic solvent, and collecting the upper phase as refined fish oil.
Preferably, the hydrophilic solvent in step (1) is one or more of polyethylene glycol (200, 400, 600), methanol, ethanol, propanol, isopropanol, tert-butanol, ethylene glycol and acetone;
preferably, the hydrophilicity in step (1)The solvent is [ BMIM]Br、[BMIM]BF4、[EMIM]ETSO4And [ OMIM]One or more of Cl.
Preferably, the soluble salt in step (1) is one or more of sodium citrate, ammonium sulfate, sodium sulfate, potassium phosphate, potassium dihydrogen phosphate and dipotassium hydrogen phosphate.
Preferably, the hydrophobic organic solvent in step (3) is n-hexane, [ BMIM]PF6One or more of petroleum ether and ethyl acetate.
Preferably, the reaction conditions of step (2) are: 100 ℃ and 1500 rpm, the reaction temperature is 10-40 ℃, and the reaction time is 0.1-24 h.
Preferably, the mass ratio of the soluble salt, the hydrophilic solvent and the fish oil to the enzyme solution is 0.1-1.0, 0.1-0.8 and 0.1-1.0 respectively.
The reaction is generally carried out at a temperature lower than the temperature at which the solvent is volatile. In order to optimize the enrichment effect as much as possible, the pH of the system can be adjusted. The pH value of the three-liquid phase system is 3-12. Preferably, the pH of the three liquid phase system is 4-9.
Preferably, the concentration of the phospholipase and the lipase in the step (1) is 5-200U/mL, the phospholipase is phospholipase ultra (lipase ultra), and the lipase is lipase AYS (Candida rugosa lipase), lipase PL20000L (Rhizomucormiehei lipase).
Preferably, the mass volume ratio of the fish oil phase to the alkali liquor in the step (3) is 0.1-1.0 g/mL.
Preferably, the alkali liquor is one or more of a sodium hydroxide solution, a potassium carbonate solution and an ammonia water solution.
In the phospholipase-catalyzed reaction, the phospholipase may be derived from natural sources or may be produced by artificial fermentation. Can be fermentation liquor, crude enzyme after simple purification, or pure enzyme after purification.
After the reaction in the step (2) is finished, the salt-rich phase or the alcohol-rich phase enriched by the phospholipase can be directly used for the next reaction, and a pure enzyme product can be obtained by an ultrafiltration or adsorption method.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides a method for synchronously degumming and decoloring crude fish oil by combining enzyme and multiple liquids. The process is simplified, the treatment time is short, the cost is reduced, and the method is economical and feasible. The concrete points are as follows: the fish oil can be distributed on the upper phase by utilizing the characteristics of synchronously and efficiently removing impurities and improving the enzyme catalysis efficiency of a multi-liquid-phase system, phospholipid is converted into more hydrophilic colloid to be enriched in a second-layer solid phase by utilizing phospholipase, pigment is converted into more hydrophilic substances to enter an alcohol-rich phase or a salt-rich phase, and then more impurities and pigment are separated from the fish oil by combining alkali washing and hydrophobic solvent extraction. The process is beneficial to greatly improving the degumming and decoloring efficiency, and can enrich the enzyme in one phase, so that the purification and recovery are convenient, and the related cost is greatly reduced. The method has the advantages of low energy consumption, high utilization rate of raw materials, simple process and the like.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the embodiments of the present invention are not limited thereto, and may be carried out with reference to conventional techniques for process parameters not particularly noted.
The phospholipase Ultra, PL20000L used in this example was purchased from Novozyme, and AYS was purchased from Amano.
Example 1
Taking 8g of phosphorus lipase Ultra-containing crude enzyme liquid (100U/mL), adding 4g of trisodium citrate dihydrate, uniformly mixing, adding 4g of polyethylene glycol 400 and 4g of tuna oil, filling into a triangular flask with a plug, and uniformly mixing to prepare a multi-liquid-phase system; the reaction was carried out with stirring at 1000rpm and controlled at 37 ℃ for 12 h. After the reaction is finished, setting the rotation speed of 5000rpm for centrifugation for 10min, dividing the mixture into four phases, wherein the upper liquid phase product is a fish oil phase, the second layer is a solid phase rich in colloid, the third layer and the fourth layer are respectively an alcohol-rich phase or a salt-rich phase, and the enzyme is mainly concentrated in the third layer. Then adding 7.5ml of 5mol/L sodium hydroxide solution, adding equal volume of normal hexane, standing, extracting, and distilling the extracted upper phase to obtain the refined fish oil. The degumming and decoloring rates of the fish oil are respectively 99.3 percent and 64.0 percent, while the degumming and decoloring rates of the single alkali washing method are only 56.9 percent and 36.9 percent, and the degumming and decoloring rates of the fish oil treated by a multi-liquid-phase system prepared by replacing a crude enzyme liquid with pure water are only 83.9 percent and 63.7 percent.
Example 2
Taking 9g of crude enzyme liquid (100U/mL) containing lipase PL20000L, adding 3g of sodium sulfate, mixing uniformly, adding 4g of polyethylene glycol 600 and 4g of tuna oil, filling into a triangular flask with a plug, and mixing uniformly to prepare a multi-liquid-phase system; the reaction was carried out with stirring at 1000rpm and controlled at 37 ℃ for 1 h. After the reaction is finished, setting the rotation speed of 5000rpm for centrifugation for 10min, dividing the mixture into four phases, wherein the upper liquid phase product is a fish oil phase, the second layer is a solid phase rich in colloid, the third layer and the fourth layer are respectively an alcohol-rich phase or a salt-rich phase, and the enzyme is mainly concentrated in the third layer. Then adding 7.5ml of 5mol/L sodium hydroxide solution, adding equal volume of normal hexane, standing, extracting, and distilling the extracted upper phase to obtain the refined fish oil. The degumming and decoloring rates of the fish oil are respectively 89.6 percent and 60 percent, while the degumming and decoloring rates of the single alkali washing method are only 56.9 percent and 36.9 percent, and the degumming and decoloring rates of the fish oil treated by a multi-liquid-phase system prepared by replacing a crude enzyme liquid with pure water are only 56.9 percent and 44.7 percent.
Example 3
Taking 8g of phosphorus lipase Ultra-containing crude enzyme liquid (100U/mL), adding 4g of trisodium citrate dihydrate, uniformly mixing, adding 4g of [ BMIM ] BF4 and 4g of tuna oil, filling into a triangular flask with a plug, and uniformly mixing to prepare a multi-liquid-phase system; the reaction was carried out with stirring at 1000rpm and controlled at 37 ℃ for 12 h. After the reaction is finished, setting the rotation speed of 5000rpm for centrifugation for 10min, dividing the mixture into four phases, wherein the upper liquid phase product is a fish oil phase, the second layer is a solid phase rich in colloid, the third layer and the fourth layer are respectively an alcohol-rich phase or a salt-rich phase, and the enzyme is mainly concentrated in the third layer. Then adding 7.5ml of 5mol/L sodium hydroxide solution, adding equal volume of normal hexane, standing, extracting, and distilling the extracted upper phase to obtain the refined fish oil. The degumming and decoloration rates of the fish oil are respectively 99.26 percent and 58.20 percent, while the degumming and decoloration rates of the fish oil processed by a multi-liquid phase system prepared by replacing a crude enzyme liquid with pure water are only 90.27 percent and 57.10 percent.
Example 4
Taking 8g of crude enzyme liquid (100U/mL respectively) containing phospholipase Ultra and lipase TL100L, adding 4g of ammonium sulfate, uniformly mixing, adding 4g of polyethylene glycol 200 and 4g of tuna oil, putting into a triangular flask with a plug, and uniformly mixing to prepare a multi-liquid-phase system; the reaction was carried out with stirring at 1000rpm and controlled at 37 ℃ for 6 h. After the reaction is finished, setting the rotation speed of 5000rpm for centrifugation for 10min, dividing the mixture into four phases, wherein the upper liquid phase product is a fish oil phase, the second layer is a solid phase rich in colloid, the third layer and the fourth layer are respectively an alcohol-rich phase or a salt-rich phase, and the enzyme is mainly concentrated in the third layer. Then, 10ml of sodium hydroxide solution with the concentration of 4mol/L is added, then equal volume of normal hexane is added, extraction is carried out after standing, and the extracted upper phase is distilled to obtain the refined fish oil. The degumming and decoloration rates of the fish oil respectively reach 88.19 percent and 46.27 percent, while the degumming and decoloration rates of the fish oil processed by a multi-liquid phase system prepared by replacing a crude enzyme liquid with pure water are only 56.93 percent and 44.72 percent.
Example 5
Taking 9g of phosphorus lipase Ultra-containing crude enzyme liquid (100U/mL), adding 3g of sodium sulfate, uniformly mixing, adding 4g of methanol and 4g of tuna oil, filling into a triangular flask with a plug, and uniformly mixing to prepare a multi-liquid-phase system; the reaction was carried out with stirring at 1000rpm and controlled at 37 ℃ for 6 h. After the reaction is finished, setting the rotation speed of 5000rpm for centrifugation for 10min, dividing the mixture into four phases, wherein the upper liquid phase product is a fish oil phase, the second layer is a solid phase rich in colloid, the third layer and the fourth layer are respectively an alcohol-rich phase or a salt-rich phase, and the enzyme is mainly concentrated in the third layer. Then, 10ml of sodium hydroxide solution with the concentration of 4mol/L is added, then equal volume of normal hexane is added, extraction is carried out after standing, and the extracted upper phase is distilled to obtain the refined fish oil. The degumming and decoloration rates of the fish oil respectively reach 84.00 percent and 77.05 percent, while the degumming and decoloration rates of the fish oil treated by a multi-liquid phase system prepared by replacing a crude enzyme liquid with pure water are only 60.78 percent and 48.54 percent.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811200799.3A CN109234007B (en) | 2018-10-16 | 2018-10-16 | Fish oil degumming and decoloring method |
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