Degummed tuna oil and preparation method thereof

Abstract

The invention discloses degummed tuna oil and a preparation method thereof.The preparation method of the degummed tuna oil comprises the steps that after Jinjiang crude fish oil is heated to a first preset temperature, a mixed adsorbent is added, stirring and degumming are conducted at the first preset temperature, centrifugation is conducted, and a degummed first solution is obtained, the mixed adsorbent comprises attapulgite and activated clay, the mass ratio of the attapulgite to the activated clay is 1: (3-7), the first preset temperature is 75-78 DEG C, and the mass ratio of the mixed adsorbent to the golden gun crude fish oil is (5-10): 100; heating a first solution obtained by degumming to a second preset temperature, adding a citric acid solution into the system solution, performing ultrasonic treatment, stirring at 60-65 DEG C, cooling and centrifuging to obtain the system solution; and heating the system liquid to a third preset temperature, adjusting the pH value to 5.8-6.2, adding a compound enzyme for degumming, taking an upper-layer oil sample after complete reaction, carrying out microwave treatment, removing water in the oil sample, and carrying out enzyme deactivation to obtain the degummed tuna oil.

Description

Technical Field

[0001] The invention relates to the technical field of oil processing, in particular to degummed tuna oil and a preparation method thereof. Background Art

[0002] Tuna, also known as bluefin tuna, is known as the "king of fish" and is a highly migratory fish in the upper and middle layers of the ocean. Tuna oil is a byproduct of tuna processing and is a natural health product with high nutritional value. The ω-3 unsaturated fatty acids contained in it are essential fatty acids for humans, especially eicosapentaenoic acid (EPA) and docosahexaenoic acid (DHA), which have excellent physiological activity and are an important material basis for the generation of brain cells. They have a positive effect on brain development, memory and the prevention of Alzheimer's disease. Therefore, tuna oil is a high-quality nutritional supplement suitable for a variety of people, especially those who need to nourish the brain, regulate blood lipids and improve cardiovascular health.

[0003] The degumming and refining process of oils and fats is a complex and delicate process, which aims to improve the quality of oils and fats and make them more suitable for consumption or industrial use. Phospholipids can be divided into two categories: phosphoglycerides and sphingomyelins according to the different glycerol skeletons, and the main types of phospholipids contained in animal oils include phosphatidylcholine (lecithin) and phosphatidylethanolamine (cephalin). Oil-soluble impurities not only affect the stability of oils and fats, but also affect the process effects of oil refining and deep processing. For example, in the alkali refining process, oils and fats will promote emulsification, increase the difficulty of operation, increase the consumption of refining and auxiliary agents, and reduce the quality of soap stock; in the decolorization process, the consumption of adsorbents will increase and the decolorization effect will be reduced; undegummed oils and fats cannot be physically refined and deodorized, nor can they be deeply processed. Therefore, the soluble impurities must be removed first in the crude oil refining process. There are many methods of degumming, which are specifically divided into hydration degumming, acid refining degumming, adsorption degumming, thermal degumming and chemical reagent degumming. Hydration degumming and acid refining degumming are commonly used in the oil industry. For crude oil with high phospholipid content or phospholipids to be extracted as a by-product, hydration degumming is usually carried out before deacidification. Generally, the oil residue obtained by degumming with a large amount of acid is dark in color, and some phospholipids are deteriorated, which cannot be used as a raw material for preparing edible phospholipids.

[0004] Among the numerous degumming processes, the continuously improved enzymatic degumming has attracted more and more attention due to its good economic and environmental performance. Enzymatic degumming was first developed by Rohm and Lurgi, who used a phospholipase A2 extracted from pig pancreas. This method was called the "Enzymax" process. 2Due to the limited sources, high prices and defects in the properties of the enzyme, this method has not been widely promoted. In recent years, people have discovered phospholipase A1 and phospholipase C from microbial sources that can be used for oil degumming. Microbial enzymes can be mass-produced by fermentation. However, simple enzymatic degumming still has many limitations. The degumming is not thorough and the reaction time is long. Moreover, if the degummed oil is stationary for a period of time, more phospholipids will settle, and the degumming is incomplete.

[0005] The above contents are only used to assist in understanding the technical solution of the present invention and do not constitute an admission that the above contents are prior art. Summary of the invention

[0006] The main purpose of the present invention is to provide a degummed tuna oil and a preparation method thereof, aiming to solve the above problems.

[0007] In order to achieve the above object, the present invention provides a method for preparing degummed tuna oil, the method for preparing degummed tuna oil comprising:

[0008] After heating the crude tuna oil to a first preset temperature, adding a mixed adsorbent, stirring and degumming at the first preset temperature, and centrifuging to obtain a first degummed solution, wherein the mixed adsorbent comprises attapulgite and activated clay, the mass ratio of the attapulgite to the activated clay is 1:(3-7), the first preset temperature is 75°C-78°C, and the mass ratio of the mixed adsorbent to the crude tuna oil is (5-10):100;

[0009] The first solution obtained by degumming is heated to a second preset temperature, a citric acid solution is added to the system liquid, ultrasonic treatment is performed, and the system liquid is stirred at 60° C.-65° C., cooled and centrifuged to obtain a system liquid, wherein the second preset temperature is 62° C.-68° C.;

[0010] The system liquid is heated to a third preset temperature, the pH is adjusted to 5.8-6.2, and then a composite enzyme is added for degumming. After the reaction is complete, an upper layer oil sample is taken, microwave treatment is performed, the oil sample water is removed, and the enzyme is inactivated to obtain degummed tuna oil. The third preset temperature is 45° C.-50° C., the amount of composite enzyme added is 1.0%-1.3%, and the composite phospholipase degumming ratio is PLA 1 :PLC=1:3(v / v), the composite phospholipase includes phospholipase A 1 and phospholipase C.

[0011] Preferably, in the method for preparing degummed tuna oil, after the crude tuna oil is heated to a first preset temperature, a mixed adsorbent is added, and degumming is carried out by stirring at the first preset temperature, and the first solution after degumming is obtained by centrifugation, the stirring speed is 400r / min-450r / min, the reaction time is 25min-30min, and the centrifugal speed is 5000r / min-6000r / min.

[0012] Preferably, in the method for preparing degummed tuna oil, the first solution obtained by degumming is heated to a second preset temperature, a citric acid solution is added to the system liquid, ultrasonic treatment is performed, and stirring is performed at 60° C.-65° C., cooling and centrifugation are performed to obtain the system liquid, comprising:

[0013] The first solution obtained by degumming is heated to a second preset temperature of 62°C-68°C, a citric acid solution is added to the system liquid, 2%-5% deionized water is added, ultrasonic treatment is performed for 5 minutes, and stirring is performed at 60°C-65°C for 25 minutes-30 minutes, and cooling and centrifugation is performed at 4600r / min-4800r / min to obtain a system liquid.

[0014] Preferably, in the method for preparing degummed tuna oil, the ratio of the citric acid solution to the crude tuna oil is (1.0 ml-1.5 ml): 100 g.

[0015] Preferably, in the method for preparing degummed tuna oil, the system liquid is heated to a third preset temperature, the pH is adjusted to 5.8-6.2, and then a composite enzyme is added for degumming. After the reaction is complete, an upper layer oil sample is taken, microwave-treated, the moisture in the oil sample is removed, and the enzyme is inactivated to obtain a degummed tuna oil in which the amount of the composite enzyme added is 1.2% or 1.3%.

[0016] Preferably, in the method for preparing degummed tuna oil, the system liquid is heated to a third preset temperature, the pH is adjusted to 5.8-6.2, a composite enzyme is added for degumming, an upper oil sample is taken after the reaction is complete, microwave treatment is performed, water in the oil sample is removed and the enzyme is inactivated to obtain degummed tuna oil, the third preset temperature is 45° C.-48° C., the stirring rate is 350 r / min, and the reaction time is 2h-4h.

[0017] Preferably, in the method for preparing degummed tuna oil, the system liquid is heated to a third preset temperature, the pH is adjusted to 5.8-6.2, and then a composite enzyme is added for degumming. After the reaction is complete, an upper oil sample is taken, microwave treatment is performed, water in the oil sample is removed, and the enzyme is inactivated to obtain degummed tuna oil. The power of the microwave treatment is 600w-800w, and the treatment time is 4-5min.

[0018] Preferably, in the method for preparing degummed tuna oil, the system liquid is heated to a third preset temperature, the pH is adjusted to 5.8-6.2, and then a composite enzyme is added for degumming. After the reaction is complete, an upper oil sample is taken, microwave treatment is performed, water in the oil sample is removed, and the enzyme is inactivated to obtain degummed tuna oil, the pH is adjusted to 6, the microwave treatment power is 700w, and the treatment time is 4min.

[0019] Preferably, in the method for preparing degummed tuna oil, after heating the crude tuna oil to a first preset temperature, adding a mixed adsorbent, stirring and degumming at the first preset temperature, and before centrifuging to obtain a first degummed solution, the preparation method further comprises:

[0020] The crude tuna oil was obtained by ultrasonic-assisted n-hexane method, and the impurities in the crude oil were removed by vacuum filtration device.

[0021] In order to achieve the above object, the present invention also provides a degummed tuna oil, wherein the degummed tuna oil is prepared by the above-mentioned preparation method of the degummed tuna oil.

[0022] The present invention has at least the following beneficial effects:

[0023] The method for preparing degummed tuna oil provided by the present invention comprises the following steps: heating crude tuna oil to a first preset temperature, adding a mixed adsorbent, stirring and degumming at the first preset temperature, and centrifuging to obtain a first degummed solution, wherein the mixed adsorbent comprises attapulgite and activated clay, the mass ratio of the attapulgite to the activated clay is 1:(3-7), the first preset temperature is 75°C-78°C, and the mass ratio of the mixed adsorbent to the crude tuna oil is (5-10):100; heating the first solution obtained by degumming to a second preset temperature, Add citric acid solution to the system liquid, perform ultrasonic treatment, stir at 60°C-65°C, cool and centrifuge to obtain a system liquid, wherein the second preset temperature is 62°C-68°C; heat the system liquid to a third preset temperature, adjust the pH to 5.8-6.2, add a composite enzyme for degumming, take an upper oil sample after the reaction is complete, perform microwave treatment, remove moisture from the oil sample and inactivate the enzyme to obtain degummed tuna oil, wherein the third preset temperature is 45°C-50°C, the amount of the composite enzyme added is 1.0%-1.3%, and the composite phospholipase degumming ratio is PLA. 1 :PLC=1:3(v / v), the composite phospholipase includes phospholipase A 1 Compared with phospholipase C, which has a single effect and high cost, the present invention adds an adsorbent for degumming before enzymatic degumming, which can effectively remove the macromolecular phospholipids in the fish oil, so that the subsequent enzymatic degumming effect is better and the phospholipid content is lower. At the same time, it can also adsorb the pigment substances in the fish oil, save resources for subsequent decolorization and refining, and the obtained degummed oil has better appearance quality.

[0024] Furthermore, after the adsorbent reacts, a citric acid solution is added for acid reaction, which can complex the metal ions in the fish oil and ensure the stability of the refined oil. After adsorption degumming, adding a composite phospholipase for enzymatic degumming saves more reaction time and enzyme raw materials than traditional enzymatic degumming, has more economic and environmental benefits, significantly reduces the phospholipid content and acid value of tuna oil, and reduces the generation of harmful substances such as benzopyrene. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 The present invention is a schematic diagram of a method for preparing degummed tuna oil.

[0026] The realization of the purpose, functional features and advantages of the present invention will be further explained in conjunction with embodiments and with reference to the accompanying drawings. DETAILED DESCRIPTION

[0027] In the embodiments of the present invention, the term "and / or" describes the association relationship of associated objects, indicating that three relationships may exist. For example, A and / or B may represent three situations: A exists alone, A and B exist at the same time, and B exists alone. The character " / " generally indicates that the associated objects before and after are in an "or" relationship.

[0028] It should be noted that the terms "first", "second", etc. in the specification and claims of the present invention and the above-mentioned drawings are used to distinguish similar objects, and are not necessarily used to describe a specific order or sequence.

[0029] In the embodiments of the present invention, the term "plurality" refers to two or more than two, and other quantifiers are similar.

[0030] In order to make the purpose, technical scheme and advantages of the embodiments of the present invention clearer, the embodiments of the present invention will be described in detail below in conjunction with the accompanying drawings. However, it can be understood by those skilled in the art that in the embodiments of the present invention, many technical details are proposed in order to enable the reader to better understand the present invention. However, even without these technical details and various changes and modifications based on the following embodiments, the technical scheme claimed in the present invention can also be implemented. The division of the following embodiments is for the convenience of description and should not constitute any limitation on the specific implementation of the present invention. The various embodiments can be combined and referenced with each other under the premise of no contradiction.

[0031] Figure 1 The process of the preparation method of degummed tuna oil provided by the present invention is schematically illustrated.

[0032] At step 100, the crude tuna oil is obtained by using an ultrasonic wave-assisted n-hexane method, and impurities in the crude oil are removed by using a vacuum filtration device. In some feasible implementations, the crude tuna oil can also be obtained by other methods, which are not specifically limited here.

[0033] For example, the hexane-oil phase and impurities are separated by centrifugation, and then small molecular impurities are removed by vacuum filtration, and then the hexane is removed by rotary evaporation to obtain crude tuna oil. In this embodiment, the centrifuge speed is 9000 r / min, the centrifugation time is 10 min, the membrane used for vacuum filtration is a 0.45 μm PES polyethersulfone filter membrane, and the rotary evaporation temperature is 65°C.

[0034] At step 200, after the crude tuna oil is heated to a first preset temperature, a mixed adsorbent is added, and the mixture is stirred and degummed at the first preset temperature, and the degummed first solution is obtained by centrifugation, wherein the mixed adsorbent includes attapulgite and activated clay. The mass ratio of the attapulgite to the activated clay is 1:(3-7), the first preset temperature is 75°C-78°C, and the mass ratio of the mixed adsorbent to the crude tuna oil is (5-10):100. The stirring speed during the stirring and degumming in step 200 is 400r / min-450r / min, the reaction time is 25min-30min, and the centrifugal speed is 5000r / min-6000r / min.

[0035] In other embodiments, the stirring speed during the degumming in step 200 is 400 r / min, the reaction time is 25 min, the centrifugal speed is 5000 r / min, and the centrifugal time is 10 min.

[0036] The first preset temperature may also be 76° C. or 77° C. The mass ratio of the mixed adsorbent to the crude tuna oil may also be 6 g / 100 g, 7 g / 100 g, 8 g / 100 g, 9 g / 100 g, or 10 g / 100 g.

[0037] The mass ratio of the attapulgite to the activated clay is 1:4 or 1:5.

[0038] At step 300, the first solution obtained by degumming is heated to a second preset temperature, a citric acid solution is added to the system solution, ultrasonic treatment is performed, and stirring is performed at 60°C-65°C, cooling and centrifugation are performed to obtain a system solution. The second preset temperature is 62°C-68°C;

[0039] Specifically, the first solution obtained by degumming is heated to a second preset temperature of 62°C-68°C, a citric acid solution is added to the system liquid, 2%-5% deionized water is added, ultrasonic treatment is performed for 5 minutes, and stirring is performed at 60°C-65°C for 25 minutes-30 minutes, cooling and centrifuging at 4600r / min-4800r / min, and centrifuging for 10 minutes to obtain a system liquid.

[0040] The second preset temperature may be 62°C, 63°C, 64°C, 65°C, 66°C, 67°C, or 68°C.

[0041] The ratio of the citric acid solution to the crude tuna oil is (1.0 ml-1.5 ml): 100 g. The mass fraction of the citric acid solution is 65%. The ratio of the citric acid solution to the crude tuna oil can also be 1.0 ml / 100 g, 1.1 ml / 100 g, 1.2 ml / 100 g, 1.3 ml / 100 g, 1.4 ml / 100 g, 1.5 ml / 100 g.

[0042] By adding deionized water, the phospholipids are hydrated, the critical temperature of coagulation is changed, and the flocculation of the particles is promoted.

[0043] At step 400, the system liquid is heated to a third preset temperature, the pH is adjusted to 5.8-6.2, a composite enzyme is added for degumming, and after the reaction is complete, an upper layer oil sample is taken, microwave treatment is performed, the oil sample water is removed and the enzyme is inactivated to obtain degummed tuna oil. The third preset temperature is 45°C-50°C.

[0044] In some other embodiments, the third preset temperature may be 46° C., 47° C., 48° C., or 49° C. The pH may also be adjusted to 5.9, 6.0, or 6.1.

[0045] Compound phospholipase degumming ratio for PLA 1 :PLC=1:3(v / v), the composite phospholipase includes phospholipase A 1 and phospholipase C.

[0046] When adding compound phospholipase, the ratio of adding PLA 1 :PLC=1:3(v / v), then adjust the temperature of the enzyme reaction system to 45℃-48℃, react for 2h-4h (preferably, the reaction time can be 3h) at a stirring rate of 350r / min, take the upper oil sample for microwave treatment (to remove oil sample moisture and inactivate enzyme) after the reaction is complete, the microwave treatment parameter is 600w-800w (the microwave treatment power can also be 700w), treat for 4-5min, and then obtain degummed tuna oil.

[0047] In step 400, the pH may also be adjusted to 5.9, 6.0 or 6.1.

[0048] Phospholipase A 1 Both the enzyme and phospholipase C are Lecitase Ultra. The amount of compound enzyme added is 1.0%-1.3%, and the proportion of compound phospholipase added is PLA 1 :PLC=1:3 (v / v). The amount of the complex enzyme added can also be 1.1% or 1.2%. It should be noted that the amount of the complex enzyme added is the ratio of the system liquid.

[0049] The present invention also provides a degummed tuna oil, wherein the degummed tuna oil is prepared by adopting the preparation method of the degummed tuna oil.

[0050] In order to verify the beneficial effects of the present invention, the present invention adopts embodiments and comparative examples for comparative explanation.

[0051] Example 1

[0052] S1, obtaining crude tuna oil by using n-hexane assisted by ultrasonic wave, and removing impurities in the crude oil by using a vacuum filtration device;

[0053] S2, heating 100g of crude tuna oil to a first preset temperature of 76°C, adding 8g of a mixed adsorbent, stirring and degumming at a speed of 400r / min at the first preset temperature, reacting for 25min, cooling and centrifuging to obtain a first degummed solution, wherein the mixed adsorbent includes 2g of attapulgite and 6g of activated clay;

[0054] S3, heating the first solution obtained by degumming to a second preset temperature of 66° C., adding 1.3 ml of a 65% mass fraction citric acid solution to the system liquid, adding 3 ml of deionized water, ultrasonically treating for 5 min, stirring at 63° C. for 25 min, cooling and centrifuging at a speed of 4800 r / min for 10 min to obtain a system liquid;

[0055] S4, heating the system liquid to a third preset temperature, adjusting the pH to 5.8-6.2, adding a composite enzyme for degumming, reacting for 2 hours at a stirring rate of 350 r / min, taking an upper layer oil sample after the reaction is complete, and subjecting it to microwave treatment, wherein the microwave treatment parameter is a power of 700 w, and the treatment is performed for 4 minutes to remove moisture from the oil sample and inactivate the enzyme, thereby obtaining degummed tuna oil, wherein the third preset temperature is 48°C. The composite enzyme degumming includes phospholipase A 1 and phospholipase C, phospholipase A 1 Both PLA1 and phospholipase C were Lecitase Ultra. The amount of compound enzyme added was 1.00 ml, and the compound phospholipase addition ratio was PLA1:PLC=1:3 (v / v).

[0056] Example 2

[0057] S1, obtaining crude tuna oil by using n-hexane assisted by ultrasonic wave, and removing impurities in the crude oil by using a vacuum filtration device;

[0058] S2, heating 100g of crude tuna oil to a first preset temperature of 76°C, adding 8g of a mixed adsorbent, stirring and degumming at a speed of 400r / min at the first preset temperature, reacting for 25min, cooling and centrifuging to obtain a first degummed solution, wherein the mixed adsorbent includes 1.33g of attapulgite and 6.67g of activated clay;

[0059] S3, heating the first solution obtained by degumming to a second preset temperature of 66° C., adding 1.5 ml of a 65% mass fraction citric acid solution to the system liquid, adding 3 ml of deionized water, ultrasonically treating for 5 min, stirring at 63° C. for 25 min, cooling and centrifuging at a speed of 4800 r / min for 10 min to obtain a system liquid;

[0060] S4, heating the system liquid to a third preset temperature, adjusting the pH to 5.8-6.0, adding a composite enzyme for degumming, reacting for 3 hours at a stirring rate of 350 r / min, taking an upper layer oil sample after the reaction is complete, and subjecting it to microwave treatment, wherein the microwave treatment parameter is a power of 700 w, and the treatment is performed for 4 minutes to remove moisture from the oil sample and inactivate the enzyme, thereby obtaining degummed tuna oil, wherein the third preset temperature is 48°C. The composite enzyme degumming includes phospholipase A 1 and phospholipase C, phospholipase A 1 Both PLA1 and phospholipase C were Lecitase Ultra. The amount of compound enzyme added was 1.2 ml, and the compound phospholipase addition ratio was PLA1:PLC=1:3 (v / v).

[0061] Example 3

[0062] S1, obtaining crude tuna oil by using n-hexane assisted by ultrasonic wave, and removing impurities in the crude oil by using a vacuum filtration device;

[0063] S2, heating 100g of crude tuna oil to a first preset temperature of 76°C, adding 8g of a mixed adsorbent, stirring and degumming at a speed of 400r / min at the first preset temperature, reacting for 25min, cooling and centrifuging to obtain a first degummed solution, wherein the mixed adsorbent includes 1.33g of attapulgite and 6.67g of activated clay;

[0064] S3, heating the first solution obtained by degumming to a second preset temperature of 66° C., adding 1.3 ml of a 65% mass fraction citric acid solution to the system liquid, adding 3 ml of deionized water, ultrasonically treating for 5 min, stirring at 63° C. for 25 min, cooling and centrifuging at a speed of 4800 r / min for 10 min to obtain a system liquid;

[0065] S4, heating the system liquid to a third preset temperature, adjusting the pH to 5.8-6.0, adding a composite enzyme for degumming, reacting for 2 hours at a stirring rate of 350r / min, taking an upper layer oil sample after the reaction is complete, and subjecting it to microwave treatment, wherein the microwave treatment parameter is a power of 700w, and the treatment is performed for 4 minutes to remove moisture from the oil sample and inactivate the enzyme, thereby obtaining degummed tuna oil, wherein the third preset temperature is 48°C. The composite enzyme degumming includes phospholipase A 1 and phospholipase C, phospholipase A 1Both PLA1 and phospholipase C were Lecitase Ultra. The amount of compound enzyme added was 1.0 ml, and the compound phospholipase addition ratio was PLA1:PLC=1:3 (v / v).

[0066] Example 4

[0067] S1, obtaining crude tuna oil by using n-hexane assisted by ultrasonic wave, and removing impurities in the crude oil by using a vacuum filtration device;

[0068] S2, heating 100g of crude tuna oil to a first preset temperature of 76°C, adding 8g of a mixed adsorbent, stirring and degumming at a speed of 400r / min at the first preset temperature, reacting for 25min, cooling and centrifuging to obtain a first degummed solution, wherein the mixed adsorbent includes 2g of attapulgite and 6g of activated clay;

[0069] S3, heating the first solution obtained by degumming to a second preset temperature of 66° C., adding 1.3 ml of a 65% mass fraction citric acid solution to the system liquid, adding 3 ml of deionized water, ultrasonically treating for 5 min, stirring at 63° C. for 25 min, cooling and centrifuging at a speed of 4800 r / min for 10 min to obtain a system liquid;

[0070] S4, heating the system liquid to a third preset temperature, adjusting the pH to 5.8-6.0, adding a composite enzyme for degumming, reacting for 2 hours at a stirring rate of 350r / min, taking an upper layer oil sample after the reaction is complete, and subjecting it to microwave treatment, wherein the microwave treatment parameter is a power of 700w, and the treatment is performed for 4 minutes to remove moisture from the oil sample and inactivate the enzyme, thereby obtaining degummed tuna oil, wherein the third preset temperature is 48°C. The composite enzyme degumming includes phospholipase A 1 and phospholipase C, phospholipase A 1 Both PLA1 and phospholipase C were Lecitase Ultra. The amount of compound enzyme added was 1.2 ml, and the compound phospholipase addition ratio was PLA1:PLC=1:3 (v / v).

[0071] Example 5

[0072] S1, obtaining crude tuna oil by using n-hexane assisted by ultrasonic wave, and removing impurities in the crude oil by using a vacuum filtration device;

[0073] S2, heating 100g of crude tuna oil to a first preset temperature of 76°C, adding 8g of a mixed adsorbent, stirring and degumming at a speed of 400r / min at the first preset temperature, reacting for 25min, cooling and centrifuging to obtain a first degummed solution, wherein the mixed adsorbent includes 1.14g of attapulgite and 6.86g of activated clay;

[0074] S3, heating the first solution obtained by degumming to a second preset temperature of 66° C., adding 1.5 ml of a 65% mass fraction citric acid solution to the system liquid, adding 3 ml of deionized water, ultrasonically treating for 5 min, stirring at 63° C. for 25 min, cooling and centrifuging at a speed of 4800 r / min for 10 min to obtain a system liquid;

[0075] S4, heating the system liquid to a third preset temperature, adjusting the pH to 5.8-6.0, adding a composite enzyme for degumming, reacting for 3 hours at a stirring rate of 350 r / min, taking an upper layer oil sample after the reaction is complete, and subjecting it to microwave treatment, wherein the microwave treatment parameter is a power of 700 w, and the treatment is performed for 4 minutes to remove moisture from the oil sample and inactivate the enzyme, thereby obtaining degummed tuna oil, wherein the third preset temperature is 48°C. The composite enzyme degumming includes phospholipase A 1 and phospholipase C, phospholipase A 1 Both PLA1 and phospholipase C were Lecitase Ultra. The amount of compound enzyme added was 1.0 ml, and the compound phospholipase addition ratio was PLA1:PLC=1:3 (v / v).

[0076] Example 6

[0077] S1, obtaining crude tuna oil by using n-hexane assisted by ultrasonic wave, and removing impurities in the crude oil by using a vacuum filtration device;

[0078] S2, heating 100g of crude tuna oil to a first preset temperature of 76°C, adding 8g of a mixed adsorbent, stirring and degumming at a speed of 400r / min at the first preset temperature, reacting for 25min, cooling and centrifuging to obtain a first degummed solution, wherein the mixed adsorbent includes 1.33g of attapulgite and 6.67g of activated clay;

[0079] S3, heating the first solution obtained by degumming to a second preset temperature of 66° C., adding 1.3 ml of a 65% mass fraction citric acid solution to the system liquid, adding 3 ml of deionized water, ultrasonically treating for 5 min, stirring at 63° C. for 25 min, cooling and centrifuging at a speed of 4800 r / min for 10 min to obtain a system liquid;

[0080] S4, heating the system liquid to a third preset temperature, adjusting the pH to 5.8-6.0, adding a composite enzyme for degumming, reacting for 2 hours at a stirring rate of 350r / min, taking an upper layer oil sample after the reaction is complete, and subjecting it to microwave treatment, wherein the microwave treatment parameter is a power of 700w, and the treatment is performed for 4 minutes to remove moisture from the oil sample and inactivate the enzyme, thereby obtaining degummed tuna oil, wherein the third preset temperature is 48°C. The composite enzyme degumming includes phospholipase A 1 and phospholipase C, phospholipase A 1Both PLA1 and phospholipase C were Lecitase Ultra. The amount of compound enzyme added was 1.3 ml, and the compound phospholipase addition ratio was PLA1:PLC=1:3 (v / v).

[0081] Comparative Example 1

[0082] S1, obtaining crude tuna oil by using n-hexane assisted by ultrasonic wave, and removing impurities in the crude oil by using a vacuum filtration device;

[0083] S2, heating 100g of crude tuna oil to a first preset temperature of 76°C, adding 0g of a mixed adsorbent, and stirring at a speed of 400r / min for degumming at the first preset temperature, reacting for 25min, cooling and centrifuging, the centrifuge speed is 5500r / min, the centrifugation time is 10min, and a first degummed solution is obtained;

[0084] S3, heating the first solution obtained by degumming to a second preset temperature of 66° C., adding 1.3 ml of a 65% mass fraction citric acid solution to the system liquid, adding 3 ml of deionized water, ultrasonically treating for 5 min, stirring at 63° C. for 25 min, cooling and centrifuging at a speed of 4800 r / min for 10 min to obtain a system liquid;

[0085] S4, heating the system liquid to a third preset temperature, adjusting the pH to 5.8-6.0, adding a composite enzyme for degumming, reacting for 3 hours at a stirring rate of 350 r / min, taking an upper layer oil sample after the reaction is complete, and subjecting it to microwave treatment, wherein the microwave treatment parameter is a power of 700 w, and the treatment is performed for 4 minutes to remove moisture from the oil sample and inactivate the enzyme, thereby obtaining degummed tuna oil, wherein the third preset temperature is 48°C. The composite enzyme degumming includes phospholipase A 1 and phospholipase C, phospholipase A 1 Both PLA1 and phospholipase C were Lecitase Ultra. The amount of compound enzyme added was 1.0 ml, and the compound phospholipase addition ratio was PLA1:PLC=1:3 (v / v).

[0086] Comparative Example 2

[0087] S1, obtaining crude tuna oil by using n-hexane assisted by ultrasonic wave, and removing impurities in the crude oil by using a vacuum filtration device;

[0088] S2, heating 100g of crude tuna oil to a first preset temperature of 76°C, adding 0g of a mixed adsorbent, and stirring at a speed of 400r / min for degumming at the first preset temperature, reacting for 25min, cooling and centrifuging, the centrifuge speed is 5500r / min, the centrifugation time is 10min, and a first degummed solution is obtained;

[0089] S3, heating the first solution obtained by degumming to a second preset temperature of 66° C., adding 1.5 ml of a 65% mass fraction citric acid solution to the system liquid, adding 3 ml of deionized water, ultrasonically treating for 5 min, stirring at 63° C. for 25 min, cooling and centrifuging at a speed of 4800 r / min for 10 min to obtain a system liquid;

[0090] S4, heating the system liquid to a third preset temperature, adjusting the pH to 5.8-6.0, adding a composite enzyme for degumming, reacting for 3 hours at a stirring rate of 350 r / min, taking an upper layer oil sample after the reaction is complete, and subjecting it to microwave treatment, wherein the microwave treatment parameter is a power of 700 w, and the treatment is performed for 4 minutes to remove moisture from the oil sample and inactivate the enzyme, thereby obtaining degummed tuna oil, wherein the third preset temperature is 48°C. The composite enzyme degumming includes phospholipase A 1 and phospholipase C, phospholipase A 1 Both PLA1 and phospholipase C were Lecitase Ultra. The amount of compound enzyme added was 1.0 ml, and the compound phospholipase addition ratio was PLA1:PLC=1:3 (v / v).

[0091] Comparative Example 3

[0092] S1, obtaining crude tuna oil by using n-hexane assisted by ultrasonic wave, and removing impurities in the crude oil by using a vacuum filtration device;

[0093] S2, heating 100g of crude tuna oil to a first preset temperature of 76°C, adding 0g of a mixed adsorbent, and stirring at a speed of 400r / min for degumming at the first preset temperature, reacting for 25min, cooling and centrifuging, the centrifuge speed is 5500r / min, the centrifugation time is 10min, and a first degummed solution is obtained;

[0094] S3, heating the first solution obtained by degumming to a second preset temperature of 66° C., adding 1.3 ml of a 65% mass fraction citric acid solution to the system liquid, adding 3 ml of deionized water, ultrasonically treating for 5 min, stirring at 63° C. for 25 min, cooling and centrifuging at a speed of 4800 r / min for 10 min to obtain a system liquid;

[0095] S4, heating the system liquid to a third preset temperature, adjusting the pH to 5.8-6.0, adding a composite enzyme for degumming, reacting for 3 hours at a stirring rate of 350 r / min, taking an upper layer oil sample after the reaction is complete, and subjecting it to microwave treatment, wherein the microwave treatment parameter is a power of 700 w, and the treatment is performed for 4 minutes to remove moisture from the oil sample and inactivate the enzyme, thereby obtaining degummed tuna oil, wherein the third preset temperature is 48°C. The composite enzyme degumming includes phospholipase A 1 and phospholipase C, phospholipase A 1Both PLA1 and phospholipase C were Lecitase Ultra. The amount of compound enzyme added was 1.2 ml, and the compound phospholipase addition ratio was PLA1:PLC=1:3 (v / v).

[0096] Table 1 Comparative Examples and Examples

[0097]

[0098]

[0099] It can be seen from Table 1 that the scheme provided by the present invention not only saves the time of simple enzymatic degumming, increases the oil yield to a certain extent, and significantly improves the decolorization rate, so that the appearance quality of tuna degummed oil is better.

[0100] Furthermore, the present invention can effectively remove the macromolecular phospholipids in the fish oil, significantly reduce the phospholipid content in the oil, greatly retain the active ingredients in the oil, and save time and reduce the amount of enzyme for subsequent enzymatic degumming by adding a mixed adsorbent (attapulgite: activated white clay), and degumming the attapulgite and activated white clay according to a preset ratio.

[0101] Compared with simple enzymatic degumming, the present invention utilizes mixed adsorbent (attapulgite: activated clay) and composite phospholipase (phospholipase A 1 and phospholipase C), the decolorization rate result is quite significant, which can significantly reduce the color and turbidity of fish oil, provide degummed tuna crude fish oil with better appearance quality, and also provide convenience for subsequent decolorization and refining.

[0102] Obviously, the embodiments described above are only some embodiments of the present invention, rather than all embodiments. Based on the embodiments of the present invention, ordinary technicians in this field can make other different forms of changes or modifications without creative work, which should fall within the scope of protection of the present invention.

Claims

1. A method for preparing degummed tuna oil, characterized in that: include: After heating the crude tuna oil to a first preset temperature, adding a mixed adsorbent, stirring and degumming at the first preset temperature, and centrifuging to obtain a first degummed solution, wherein the mixed adsorbent comprises attapulgite and activated clay, the mass ratio of the attapulgite to the activated clay is 1:(3-7), the first preset temperature is 75°C-78°C, and the mass ratio of the mixed adsorbent to the crude tuna oil is (5-10):100; The first solution obtained by degumming is heated to a second preset temperature, a citric acid solution is added to the system liquid, ultrasonic treatment is performed, and the system liquid is stirred at 60° C.-65° C., cooled and centrifuged to obtain a system liquid, wherein the second preset temperature is 62° C.-68° C.; The system liquid is heated to a third preset temperature, the pH is adjusted to 5.8-6.2, and then a composite enzyme is added for degumming. After the reaction is complete, an upper layer oil sample is taken, microwave treatment is performed, water in the oil sample is removed, and the enzyme is inactivated to obtain degummed tuna oil. The third preset temperature is 45° C.-50° C., the amount of composite enzyme added is 1.0%-1.3%, and the composite phospholipase degumming ratio is PLA1:PLC=1:3 (v / v), and the composite phospholipase includes phospholipase A1 and phospholipase C.

2. The method for preparing degummed tuna oil according to claim 1, characterized in that: After the crude tuna oil is heated to a first preset temperature, a mixed adsorbent is added, and degumming is carried out by stirring at the first preset temperature, and the first solution after degumming is obtained by centrifugation. The stirring speed is 400r / min-450r / min, the reaction time is 25min-30min, and the centrifugal speed is 5000r / min-6000r / min.

3. The method for preparing degummed tuna oil according to claim 1, characterized in that: The first solution obtained by degumming is heated to a second preset temperature, a citric acid solution is added to the system solution, ultrasonic treatment is performed, and stirring is performed at 60° C.-65° C., cooling and centrifugation are performed to obtain a system solution, including: The first solution obtained by degumming is heated to a second preset temperature of 62°C-68°C, a citric acid solution is added to the system liquid, 2%-5% deionized water is added, ultrasonic treatment is performed for 5 minutes, and stirring is performed at 60°C-65°C for 25 minutes-30 minutes, and cooling and centrifugation is performed at 4600r / min-4800r / min to obtain a system liquid.

4. The method for preparing degummed tuna oil according to claim 1, characterized in that: The ratio of the citric acid solution to the crude tuna oil is (1.0 ml-1.5 ml): 100 g.

5. The method for preparing degummed tuna oil according to claim 1, characterized in that: The system liquid is heated to a third preset temperature, the pH is adjusted to 5.8-6.2, and then a composite enzyme is added for degumming. After the reaction is complete, an upper layer oil sample is taken, microwave treatment is performed, water in the oil sample is removed, and the enzyme is inactivated to obtain degummed tuna oil, in which the amount of the composite enzyme added is 1.2% or 1.3%.

6. The method for preparing degummed tuna oil according to claim 1, characterized in that: The system liquid is heated to a third preset temperature, the pH is adjusted to 5.8-6.2, and then a composite enzyme is added for degumming. After the reaction is complete, an upper oil sample is taken, microwave treatment is performed, moisture in the oil sample is removed, and the enzyme is inactivated to obtain degummed tuna oil. The third preset temperature is 45° C.-48° C., the stirring rate is 350 r / min, and the reaction time is 2h-4h.

7. The method for preparing degummed tuna oil according to claim 6, characterized in that: The system liquid is heated to a third preset temperature, the pH is adjusted to 5.8-6.2, and then a composite enzyme is added for degumming. After the reaction is complete, an upper layer oil sample is taken, and microwave treatment is performed to remove moisture from the oil sample and inactivate the enzyme to obtain degummed tuna oil. The power of the microwave treatment is 600w-800w, and the treatment time is 4-5min.

8. The method for preparing degummed tuna oil according to claim 6, characterized in that: The system liquid is heated to a third preset temperature, the pH is adjusted to 5.8-6.2, and then a composite enzyme is added for degumming. After the reaction is complete, an upper layer oil sample is taken, microwave treatment is performed, water in the oil sample is removed, and the enzyme is inactivated to obtain degummed tuna oil. The pH is adjusted to 6, the microwave treatment power is 700w, and the treatment time is 4min.

9. The method for preparing degummed tuna oil according to claim 1, characterized in that: After the crude tuna oil is heated to a first preset temperature, a mixed adsorbent is added, and the mixture is stirred and degummed at the first preset temperature, and before the degummed first solution is obtained by centrifugation, the preparation method further comprises: The crude tuna oil was obtained by ultrasonic-assisted n-hexane method, and the impurities in the crude oil were removed by vacuum filtration device.

10. A degummed tuna oil, characterized in that: The degummed tuna oil is prepared by the method for preparing the degummed tuna oil according to any one of claims 1 to 9.

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