Preparation method for moderately processing ARA (arachidonic acid) grease

Abstract

The invention discloses a preparation method of moderately processed ARA grease, and belongs to the technical field of grease processing, the key point of the technical scheme is that the preparation method of moderately processed ARA grease comprises the following steps: S1, degumming: heating ARA grease to 55-60 DEG C, adding protease to react for 0.5-1 hour, then cooling to 50-55 DEG C, keeping the temperature for 1-2 hours, then heating to 60 DEG C to react for 0.5-1 hour, and then cooling to 50-55 DEG C to react for 0.5-1 hour; centrifuging the reacted grease to remove precipitates so as to obtain clear liquid; s2, desugaring: heating the clear liquid obtained in the step S1 to 70-80 DEG C, adding activated carbon, stirring for 30-45 minutes, and then filtering to obtain desugarized clear liquid; s3, extraction: carrying out supercritical extraction on the clear liquid obtained in the step S2, separating, and collecting the clear liquid; s4, ultrafiltration: carrying out ultrafiltration treatment on the clear liquid obtained in the step S3; s5, decoloration: carrying out decoloration treatment on the clear liquid obtained in the step S4, and S6, deodorization: carrying out deodorization treatment on the clear liquid obtained in the step S5 to obtain the ARA grease, thereby achieving the technical effect of improving the purity and stability of the ARA grease.

Description

Technical Field

[0001] The invention relates to the technical field of oil processing, in particular to a preparation method of moderately processed ARA oil. Background Art

[0002] ARA (arachidonic acid) oil is an important oil. It is widely used in food, health products, cosmetics and other fields because of its various physiologically active functions, such as anti-inflammatory, anti-allergic, and brain development promotion. In the field of food, ARA oil is a high-quality food additive, and its preparation method and process have a crucial impact on its quality. In the field of pharmaceutical intermediate synthesis technology, ARA oil is also an important pharmaceutical intermediate, and its application in the pharmaceutical field is mainly concentrated in anti-inflammatory, anti-allergic and other aspects. Therefore, how to prepare high-purity and high-stability ARA oil is also an important research direction in the field of pharmaceutical intermediate synthesis technology. However, the content of ARA oil in nature is low, and it is easily affected by environmental factors. Therefore, how to efficiently obtain high-purity and high-stability ARA oil is an important research direction in the current field of oil processing technology. The existing preparation methods mainly include physical processing and chemical processing. The physical processing method mainly obtains ARA oil by physical means such as pressing and extraction. Although this method is simple and easy, the purity and stability of the obtained ARA oil are poor. The chemical processing method mainly uses chemical reagents to treat oils. Although it can improve the purity and stability of ARA oils, the use of chemical reagents will pollute the environment and may cause potential harm to human health, which limits its application in food, health products, cosmetics and other fields. In addition, the existing technology in the preparation of ARA oils cannot maintain the original physiological activity of the device well, which also limits its application in the medical field.

[0003] Therefore, how to prepare ARA oil with high purity, high stability and maintaining its original physiological activity function is the main problem facing current technology. Summary of the invention

[0004] In order to solve the problems in the prior art, the present invention provides a method for preparing ARA oil by moderately processing the oil, so as to achieve the technical effect of improving the purity and stability of the ARA oil.

[0005] The present invention provides a method for preparing moderately processed ARA oil by adopting the following technical scheme:

[0006] A method for preparing moderately processed ARA oil comprises the following steps:

[0007] S1. Degumming: Heat the ARA oil to 55-60°C, add protease to react for 0.5-1h, then cool to 50-55°C and keep warm for 1-2h, then raise the temperature to 60°C and react for 0.5-1h, centrifuge the oil after the reaction to remove the precipitate and obtain a clear liquid;

[0008] S2, desugaring: heat the clear liquid obtained in step S1 to 70-80°C, add activated carbon and stir for 30-45 minutes, then filter to obtain the desugared clear liquid;

[0009] S3, extraction: subjecting the clear solution obtained in step S2 to supercritical extraction and separation, and then collecting the clear solution;

[0010] S4, ultrafiltration: ultrafiltration treatment of the clear liquid obtained in step S3;

[0011] S5, decolorization: decolorizing the clear solution obtained in step S4,

[0012] S6, deodorization: The clear liquid obtained in step S5 is deodorized to obtain ARA oil.

[0013] By adopting the above-mentioned technical scheme, the present application can effectively remove proteins, sugars, small molecules, pigments and impurities in ARA oil after degumming, desugaring, extraction, ultrafiltration, decolorization and deodorization, so that the ARA oil has good color and taste, and at the same time, it also effectively increases the ARA content in the ARA oil and the purity of the ARA oil, and can maintain its original physiological activity function; in addition, the coordinated use of each step in the present application also makes the ARA oil have good oxidative stability, and there is no need to use highly toxic chemical reagents in each preparation step of the present application, which is environmentally friendly and will not cause potential harm to human health. Therefore, the ARA oil obtained in the present application can be widely used in food, health products, cosmetics and other fields.

[0014] Preferably, during the supercritical extraction, the carbon dioxide flow rate is 25-30 L / h, the extraction pressure is 40-45 MPa, the extraction time is 100-150 min, and the extraction temperature is 35-40°C.

[0015] Preferably, the separation pressure after supercritical extraction is 5-10 MPa and the separation temperature is 40-60°C.

[0016] By adopting the above technical scheme, the activity of the ARA oil can be effectively maintained after the desugared ARA oil is extracted, and because the extraction temperature is low and the extraction and separation are combined into one, the oxidation and decomposition of heat-sensitive substances in the ARA oil can be prevented, thereby making the extraction efficiency of the ARA oil high, and the whole process is safe, low in energy consumption, and cost-saving.

[0017] Preferably, the added amount of the protease is 0.5-2% of the weight of the ARA oil, and the protease is composed of phospholipase B and phospholipase A1 in a weight ratio of 1: (0.5-0.8).

[0018] By adopting the above-mentioned technical scheme, when the added amount of protease in the present application is 0.5-2% of the weight of the ARA oil, the phospholipids can be effectively hydrolyzed and the colloid content in the oil can be reduced, thereby effectively removing the protein and other impurities in the ARA oil and improving the purity and stability of the ARA oil. However, when the added amount of protease is small, the phospholipid hydrolysis is incomplete and the degumming effect is not obvious, thereby affecting the clarity and taste of the ARA oil. When the protease is added in excess, too much protease will cause excessive hydrolysis reaction, resulting in the destruction of the beneficial ingredients in the ARA oil and even the production of undesirable by-products. Therefore, when the added amount of protease in the present application is 0.5-2% of the weight of the ARA oil, the stability and quality of the ARA oil can be effectively guaranteed.

[0019] When the protease is composed of phospholipase B and phospholipase A1, it can effectively hydrolyze the main phospholipids PC, PE and PA in the oil, and convert the non-hydratable phospholipids into more water-soluble glyceryl phospholipids and lysophospholipids, thereby improving the quality of ARA oil.

[0020] Preferably, the amount of activated carbon added is 2-3% of the weight of the clear liquid obtained in step S1.

[0021] Preferably, the ultrafiltration membrane in step S4 has a molecular weight cutoff of 4000-6000Da.

[0022] By adopting the above technical solution, when the ultrafiltration membrane has a molecular weight cutoff of 4000-6000Da, it can not only effectively remove impurities in ARA oil, but also ensure the beneficial ingredients in ARA oil and improve the purity of ARA oil.

[0023] Preferably, in step S5, the decolorization treatment temperature is 70-90° C., the treatment time is 20-40 min, and the amount of decolorizer added is 1-2% of the weight of the clear liquid.

[0024] Preferably, the decolorizing agent is attapulgite and silica gel in a weight ratio of 1:1.

[0025] By adopting the above-mentioned technical scheme, the limitation of the decolorization treatment temperature and treatment time in this application can not only effectively improve the adsorption of pigments and other impurities in ARA oil, thereby improving the clarity and quality of ARA oil, but also avoid the problem of oxidation of ARA oil caused by excessively high temperature and excessively long treatment time, thereby effectively ensuring the stability of ARA oil.

[0026] In addition, after the decolorizing agent in the present application is composed of attapulgite and silica gel, the cooperation between the two can effectively adsorb soap impurities and other polar impurities, which helps the decolorizing agent to more effectively exert its ability to adsorb pigments.

[0027] Preferably, the vacuum degree of the deodorization treatment is -0.005 MPa, the treatment temperature is 160-180°C, and the treatment time is 30-40 min.

[0028] By adopting the above technical scheme, when the deodorization treatment temperature is limited to the range of 160-180°C in this application, the volatile substances in the ARA oil can be quickly volatilized, thereby effectively reducing the odor substances in the oil, while also avoiding damage to the heat-sensitive substances in the ARA oil. When the treatment time is within the range of 30-40 minutes, the oxidation of the oil can be effectively reduced, so that the ARA oil has good stability.

[0029] Preferably, the centrifugal speed in step S1 is 4000-6000 r / min, and the centrifugal time is 10-15 min.

[0030] In summary, the present invention has the following beneficial effects:

[0031] 1. The present application can destroy the reticular structure of the cell wall in the oil and reduce the stability of the interfacial film by subjecting the ARA oil to protease hydrolysis treatment, while making the protein structure in the cells loose, so that the macromolecules in the oil are decomposed into small molecules, which are more easily adsorbed by activated carbon. At the same time, the remaining substances after the activated carbon adsorption are also easily dissolved and extracted by supercritical carbon dioxide. The reason may be that after the oil is treated with protease, the surface area of ​​the oil raw material can be increased, and the contact and diffusion rate of small molecules with the supercritical fluid can be increased. Therefore, after the ultrafiltration, decolorization and deodorization steps, the protein, sugar, small molecules, pigments and impurities in the ARA oil can be effectively removed, so that the ARA oil has good color and taste, and at the same time, the ARA content in the ARA oil and the purity of the ARA oil are effectively increased, and its original physiological activity function can be maintained.

[0032] 2. When processing ARA oil in this application, no chemical reagents are needed, which is environmentally friendly and will not cause potential harm to human health. Therefore, the ARA oil obtained in this application can be widely used in the fields of food, health products and cosmetics. DETAILED DESCRIPTION

[0033] The present invention is further described in detail below with reference to the embodiments.

[0034] Example 1

[0035] A method for preparing moderately processed ARA oil comprises the following steps:

[0036] S1, degumming: 10kg ARA oil with an ARA content of 40% was heated to 55°C, and a protease (the weight ratio of phospholipase B and phospholipase A1 was 1:0.5) of 0.5% by weight of the ARA oil was added to react at 55°C for 1 hour, and then the temperature was lowered to 50°C, reacted for 2 hours, and then the temperature was raised to 60°C for 1 hour, and the reacted oil was centrifuged at 4000r / min for 15 minutes to remove the protein precipitate to obtain a clear liquid;

[0037] S2, desugaring: heat the clear liquid obtained in step S1 to 70°C, add 2% activated carbon by weight of the clear liquid, stir for 30 minutes, and then filter to obtain the desugared clear liquid;

[0038] S3, extraction: the sugar-free clear liquid obtained in step S2 is added into an extraction kettle for supercritical carbon dioxide extraction, specifically: carbon dioxide flow rate 25L / h, extraction pressure 40MPa, extraction temperature 35°C, extraction time 100min, after separation at a temperature of 40°C and a separation pressure of 5MPa, the clear liquid is collected;

[0039] S4, ultrafiltration: The clear liquid obtained in step S3 is subjected to ultrafiltration treatment using an ultrafiltration membrane, wherein the molecular weight cut-off of the ultrafiltration membrane is 4000Da;

[0040] S5, decolorization: the clear liquid obtained in step S4 is decolorized, specifically: the decolorization temperature is 70°C, the treatment time is 20 minutes, the weight ratio of the decolorizer attapulgite to silica gel is 1:1, and the total addition amount is 1% of the weight of the clear liquid,

[0041] S6, deodorization: The clear liquid obtained in step S5 is subjected to deodorization treatment to obtain ARA oil, wherein the vacuum degree of the deodorization treatment is -0.005 MPa, the treatment temperature is 160°C, and the treatment time is 30 min.

[0042] After testing, the final ARA oil mass was 9.54kg, the recovery rate was 95.4%, the impurity content was 0.08%, the peroxide value was 0.012mmol / kg, and after a high-temperature destructive test at 62°C, the peroxide value was 0.045mmol / kg after 28 days.

[0043] Example 2

[0044] A method for preparing moderately processed ARA oil comprises the following steps:

[0045] S1, degumming: 10kg ARA oil with an ARA content of 40% was heated to 60°C, and a protease (the weight ratio of phospholipase B and phospholipase A1 was 1:0.5) of 1% by weight of the ARA oil was added to react at 60°C for 0.5h, and then the temperature was lowered to 50°C for reaction for 2h, and then the temperature was raised to 60°C for reaction for 0.5h, and the reacted oil was treated at a speed of 5000r / min for 15min to remove protein precipitation to obtain a clear liquid;

[0046] S2, desugaring: the clear liquid obtained in step S1 is heated to 75°C, activated carbon in an amount of 2.5% by weight of the clear liquid is added, stirred for 40 minutes, and then filtered to obtain a desugared clear liquid;

[0047] S3, extraction: the sugar-free clear liquid obtained in step S2 is added to an extraction kettle for supercritical carbon dioxide extraction, specifically: carbon dioxide flow rate 25L / h, extraction pressure 40MPa, extraction temperature 35°C, extraction time 130min, after separation at a temperature of 50°C and a separation pressure of 5MPa, the clear liquid is collected;

[0048] S4, ultrafiltration: The clear liquid obtained in step S3 is subjected to ultrafiltration treatment using an ultrafiltration membrane, wherein the molecular weight cut-off of the ultrafiltration membrane is 5000Da;

[0049] S5, decolorization: the clear liquid obtained in step S4 is decolorized, specifically: the decolorization temperature is 80°C, the treatment time is 30 minutes, the weight ratio of the decolorizer attapulgite to silica gel is 1:1, and the total addition amount is 1% of the weight of the clear liquid,

[0050] S6, deodorization: The clear liquid obtained in step S5 is subjected to deodorization treatment to obtain ARA oil, wherein the vacuum degree of the deodorization treatment is -0.005 MPa, the treatment temperature is 170°C, and the treatment time is 35 min.

[0051] After testing, the final ARA oil mass was 9.71kg, the recovery rate was 97.1%, the impurity content was 0.05%, the peroxide value was 0.022mmol / kg, and after a high-temperature destructive test at 62°C, the peroxide value was 0.039mmol / kg after 28 days.

[0052] Example 3

[0053] A method for preparing moderately processed ARA oil comprises the following steps:

[0054] S1, degumming: 10kg ARA oil with an ARA content of 40% was heated to 60°C, and 1.5% protease (the weight ratio of phospholipase B and phospholipase A1 was 1:0.5) by weight of the ARA oil was added to react at 60°C for 0.5h, then the temperature was lowered to 55°C for reaction for 1h, and finally the temperature was raised to 60°C for reaction for 1h, and the reacted oil was treated at a speed of 6000r / min for 15min to remove protein precipitation to obtain a clear liquid;

[0055] S2, desugaring: the clear liquid obtained in step S1 is heated to 80°C, activated carbon in an amount of 2% by weight of the clear liquid is added, stirred for 45 minutes, and then filtered to obtain a desugared clear liquid;

[0056] S3, extraction: the sugar-free clear liquid obtained in step S2 is added into an extraction kettle for supercritical carbon dioxide extraction, specifically: carbon dioxide flow rate 25L / h, extraction pressure 40MPa, extraction temperature 35°C, extraction time 130min, after separation at a temperature of 50°C and a separation pressure of 10MPa, the clear liquid is collected;

[0057] S4, ultrafiltration: The clear liquid obtained in step S3 is subjected to ultrafiltration treatment using an ultrafiltration membrane, wherein the molecular weight cut-off of the ultrafiltration membrane is 4000Da;

[0058] S5, decolorization: the clear liquid obtained in step S4 is decolorized, specifically: the decolorization temperature is 80°C, the treatment time is 40 minutes, the weight ratio of the decolorizer attapulgite to silica gel is 1:1, and the total addition amount is 1% of the weight of the clear liquid,

[0059] S6, deodorization: The clear liquid obtained in step S5 is subjected to deodorization treatment to obtain ARA oil, wherein the vacuum degree of the deodorization treatment is -0.005 MPa, the treatment temperature is 170°C, and the treatment time is 40 min.

[0060] After testing, the final ARA oil mass was 9.73kg, the recovery rate was 97.3%, the impurity content was 0.05%, the peroxide value was 0.025mmol / kg, and after a high-temperature destructive test at 62°C, the peroxide value was 0.041mmol / kg after 28 days.

[0061] Example 4

[0062] A method for preparing moderately processed ARA oil comprises the following steps:

[0063] S1, degumming: 10kg ARA oil with an ARA content of 40% was heated to 60°C, and a protease (the weight ratio of phospholipase B and phospholipase A1 was 1:0.5) of 2% by weight of the ARA oil was added to react at 60°C for 0.5h, and then the temperature was lowered to 55°C for reaction for 1h, and finally the temperature was raised to 60°C for reaction for 1h, and the reacted oil was treated at a speed of 6000r / min for 15min to remove protein precipitation to obtain a clear liquid;

[0064] S2, desugaring: the clear liquid obtained in step S1 is heated to 80°C, activated carbon is added at 3% by weight of the clear liquid, stirred for 45 minutes, and then filtered to obtain a desugared clear liquid;

[0065] S3, extraction: the sugar-free clear liquid obtained in step S2 is added into an extraction kettle for supercritical carbon dioxide extraction, specifically: carbon dioxide flow rate 30L / h, extraction pressure 45MPa, extraction temperature 40°C, extraction time 150min, after separation at a temperature of 60°C and a separation pressure of 10MPa, the clear liquid is collected;

[0066] S4, ultrafiltration: The clear liquid obtained in step S3 is subjected to ultrafiltration treatment using an ultrafiltration membrane, wherein the molecular weight cut-off of the ultrafiltration membrane is 6000Da;

[0067] S5, decolorization: the clear liquid obtained in step S4 is decolorized, specifically: the decolorization temperature is 90°C, the treatment time is 40 minutes, the weight ratio of the decolorizer attapulgite to silica gel is 1:1, and the total addition amount is 2% of the weight of the clear liquid,

[0068] S6, deodorization: The clear liquid obtained in step S5 is subjected to deodorization treatment to obtain ARA oil, wherein the vacuum degree of the deodorization treatment is -0.005 MPa, the treatment temperature is 180°C, and the treatment time is 40 min.

[0069] After testing, the final ARA oil mass was 9.65kg, the recovery rate was 96.5%, the impurity content was 0.03%, the peroxide value was 0.038mmol / kg, and after a high-temperature destructive test at 62°C, the peroxide value was 0.056mmol / kg after 28 days.

[0070] Example 5

[0071] A method for preparing moderately processed ARA oil, which is different from Example 3 in that the weight ratio of phospholipase B to phospholipase A1 is 1:0.8, and the rest is the same as Example 3.

[0072] After testing, the final ARA oil mass was 9.75kg, the recovery rate was 97.5%, the impurity content was 0.04%, the peroxide value was 0.022mmol / kg, and after a high-temperature destructive test at 62°C, the peroxide value was 0.038mmol / kg after 28 days.

[0073] Example 6

[0074] A method for preparing moderately processed ARA oil is different from that of Example 3 in that only phospholipase B is used as the protease, that is, phospholipase A1 is replaced by phospholipase B in an equal amount, and the rest is the same as that of Example 3.

[0075] After testing, the final ARA oil mass was 9.66kg, the recovery rate was 96.6%, the impurity content was 0.09%, the peroxide value was 0.031mmol / kg, and after a high-temperature destructive test at 62°C, the peroxide value was 0.056mmol / kg after 28 days.

[0076] Example 7

[0077] A method for preparing moderately processed ARA oil is different from that of Example 3 in that only phospholipase A1 is used as the protease, that is, phospholipase A1 is used to replace phospholipase B in an equal amount, and the rest is the same as that of Example 3.

[0078] After testing, the final ARA oil mass was 9.68kg, the recovery rate was 96.8%, the impurity content was 0.10%, the peroxide value was 0.033mmol / kg, and after a high-temperature destructive test at 62°C, the peroxide value was 0.059mmol / kg after 28 days.

[0079] Example 8

[0080] A method for preparing moderately processed ARA oil is different from Example 3 in that only attapulgite is used as the decolorizing agent, and the rest are the same as Example 3.

[0081] After testing, the final ARA oil mass was 9.62kg, the recovery rate was 96.2%, the impurity content was 0.12%, the peroxide value was 0.041mmol / kg, and after a high-temperature destructive test at 62°C, the peroxide value was 0.065mmol / kg after 28 days.

[0082] Example 9

[0083] A method for preparing moderately processed ARA oil is different from Example 3 in that only silica gel is used as the decolorizing agent, and the rest are the same as Example 3.

[0084] After testing, the final ARA oil mass was 9.65kg, the recovery rate was 96.5%, the impurity content was 0.09%, the peroxide value was 0.034mmol / kg, and after a high-temperature destructive test at 62°C, the peroxide value was 0.052mmol / kg after 28 days.

[0085] Comparative Example 1

[0086] A method for preparing moderately processed ARA oil, which is different from Example 4 in that only the degumming process is used to process the ARA oil, that is, 10 kg of ARA oil with an ARA content of 40% is heated to 60°C, 2% of the weight of protease (the weight ratio of phospholipase B and phospholipase A1 is 1:0.5) of the ARA oil is added, and the reaction is carried out at 60°C for 0.5h, then the temperature is lowered to 55°C for reaction for 1h, and finally the temperature is raised to 60°C for reaction for 1h, and the reacted oil is treated at a speed of 6000r / min for 15min to remove protein precipitates to obtain ARA oil.

[0087] After testing, the final ARA oil mass was 9.31kg, the recovery rate was 93.1%, the impurity content was 4.7%, the peroxide value was 0.87mmol / kg, and after a high-temperature destructive test at 62°C, the peroxide value was 15.8mmol / kg after 28 days.

[0088] Comparative Example 2

[0089] A method for preparing moderately processed ARA oil, which is different from Example 4 in that only the desugaring process is used to process the ARA oil, that is, 10 kg of ARA oil with an ARA content of 40% is heated to 80°C, 2% of the weight of activated carbon of the ARA oil is added, stirred at 80°C for 45 minutes, and then filtered to obtain the ARA oil.

[0090] After testing, the final ARA oil mass was 9.25kg, the recovery rate was 92.5%, the impurity content was 0.38%, the peroxide value was 0.73mmol / kg, and after a high-temperature destructive test at 62°C, the peroxide value was 16.3mmol / kg after 28 days.

[0091] Comparative Example 3

[0092] A method for preparing moderately processed ARA oil, which is different from Example 4 in that only supercritical extraction process is used to process ARA oil, that is, 10 kg of ARA oil with an ARA content of 40% is added to the extraction kettle, the carbon dioxide flow rate is 30 L / h, the extraction pressure is 45 MPa, the extraction temperature is 40°C, and the extraction time is 150 min. After separation, the ARA oil is collected under the conditions of temperature of 60°C and separation pressure of 10 MPa.

[0093] After testing, the final ARA oil mass was 9.62kg, the recovery rate was 96.2%, the impurity content was 0.12%, the peroxide value was 0.27mmol / kg, and after a high-temperature destructive test at 62°C, the peroxide value was 9.6mmol / kg after 28 days.

[0094] Comparative Example 4

[0095] A method for preparing moderately processed ARA oil is different from Example 4 in that only ultrafiltration technology is used to process ARA oil, that is, 10 kg of ARA oil with an ARA content of 40% is ultrafiltered using an ultrafiltration membrane with a molecular weight cutoff of 6000Da, and ARA oil is obtained after ultrafiltration.

[0096] After testing, the final ARA oil mass was 9.40kg, the recovery rate was 94%, the impurity content was 0.23%, the peroxide value was 0.81mmol / kg, and after a high-temperature destructive test at 62°C, the peroxide value was 13.2mmol / kg after 28 days.

[0097] Comparative Example 5

[0098] A method for preparing moderately processed ARA oil, which is different from Example 4 in that only a decolorization process is used to process the ARA oil, that is, 10 kg of ARA oil with an ARA content of 40% is heated to 90°C, a decolorizer of 2% by weight of the ARA oil is added, and the decolorizer is composed of attapulgite and silica gel in a weight ratio of 1:1, stirred at 90°C for 40 minutes, and then filtered to obtain the ARA oil.

[0099] After testing, the final ARA oil mass was 9.42kg, the recovery rate was 94.2%, the impurity content was 0.45%, the peroxide value was 0.59mmol / kg, and after a high-temperature destructive test at 62°C, the peroxide value was 11.3mmol / kg after 28 days.

[0100] Comparative Example 6

[0101] A method for preparing moderately processed ARA oil is different from Example 4 in that only a deodorization process is used to process the ARA oil, that is, 10 kg of ARA oil with an ARA content of 40% is treated at a vacuum degree of -0.005 MPa and a treatment temperature of 180°C for 40 minutes to obtain the ARA oil.

[0102] After testing, the final ARA oil mass was 9.31kg, the recovery rate was 93.1%, the impurity content was 0.62%, the peroxide value was 0.62mmol / kg, and after a high-temperature destructive test at 62°C, the peroxide value was 10.1mmol / kg after 28 days.

[0103] Comparative Example 7

[0104] A method for preparing moderately processed ARA oil is different from Example 4 in that extraction is missing in the processing step, and the rest is the same as Example 4.

[0105] After testing, the final ARA oil mass was 9.62kg, the recovery rate was 96.2%, the impurity content was 0.09%, the peroxide value was 0.098mmol / kg, and after a high-temperature destructive test at 62°C, the peroxide value was 1.68mmol / kg after 28 days.

[0106] Comparative Example 8

[0107] A method for preparing moderately processed ARA oil is different from Example 4 in that the oil is first extracted in the processing steps, and then degummed, desugared, ultrafiltered, decolorized and deodorized, and the process parameters of each step are the same as those in Example 4.

[0108] After testing, the final ARA oil mass was 9.62kg, the recovery rate was 96.2%, the impurity content was 0.09%, the peroxide value was 0.043mmol / kg, and after a high-temperature destructive test at 62°C, the peroxide value was 0.069mmol / kg after 28 days.

[0109] Comparative Example 9

[0110] A method for preparing moderately processed ARA oil is different from Example 4 in that the amount of protease added is 3% of the weight of the ARA oil, and the rest is the same as Example 4.

[0111] After testing, the final ARA oil mass was 9.64kg, the recovery rate was 96.4%, the impurity content was 0.06%, the peroxide value was 0.065mmol / kg, and after a high-temperature destructive test at 62°C, the peroxide value was 0.32mmol / kg after 28 days.

[0112] Comparative Example 10

[0113] A method for preparing moderately processed ARA oil, which is different from Example 4 in that in step S1, 10 kg of ARA oil with an ARA content of 40% is heated to 60°C, 2% of the weight of protease (the weight ratio of phospholipase B and phospholipase A1 is 1:0.5) of the ARA oil is added and reacted at 60°C for 4 hours, the reacted oil is treated at a speed of 4000 r / min for 15 minutes, and the protein precipitate is removed to obtain a clear liquid; the other steps are the same as Example 4.

[0114] After testing, the final ARA oil mass was 9.59kg, the recovery rate was 95.9%, the impurity content was 0.09%, the peroxide value was 0.072mmol / kg, and after a high-temperature destructive test at 62°C, the peroxide value was 0.38mmol / kg after 28 days.

[0115] Comparative Example 11

[0116] A method for preparing moderately processed ARA oil, which is different from Example 4 in that in step S1, 10 kg of ARA oil with an ARA content of 40% is heated to 70°C, 2% of the weight of protease (the weight ratio of phospholipase B and phospholipase A1 is 1:0.5) by weight of the ARA oil is added and reacted at 70°C for 0.5h, then the temperature is lowered to 60°C for reaction for 1h, and finally the temperature is raised to 70°C for reaction for 1h, and the reacted oil is treated at a speed of 6000r / min for 15min to remove the protein precipitate to obtain a clear liquid; the other steps are the same as Example 4.

[0117] After testing, the final ARA oil mass was 9.55kg, the recovery rate was 95.5%, the impurity content was 0.12%, the peroxide value was 0.085mmol / kg, and after a high-temperature destructive test at 62°C, the peroxide value was 0.43mmol / kg after 28 days.

[0118] Comparative Example 12

[0119] A method for preparing moderately processed ARA oil is different from Example 4 in that in step S2, the clear liquid obtained in step S1 is heated to 90°C, 3% activated carbon by weight of the clear liquid is added and stirred for 45 minutes, and then filtered to obtain a sugar-free clear liquid, and the other steps are the same as Example 4.

[0120] After testing, the final ARA oil mass was 9.58kg, the recovery rate was 95.8%, the impurity content was 0.10%, the peroxide value was 0.075mmol / kg, and after a high-temperature destructive test at 62°C, the peroxide value was 0.21mmol / kg after 28 days.

[0121] Comparative Example 13

[0122] A method for preparing moderately processed ARA oil, which is different from Example 4 in that the decolorization treatment temperature in step S5 is 100°C, the treatment time is 40 minutes, the weight ratio of the decolorizing agent attapulgite to silica gel is 1:1, and the total added amount is 2% of the weight of the clear liquid; the deodorization treatment temperature in step S6 is 190°C, the treatment time is 40 minutes, and the other steps and parameters are the same as those in Example 4.

[0123] After testing, the final ARA oil mass was 9.49kg, the recovery rate was 94.9%, the impurity content was 0.14%, the peroxide value was 0.15mmol / kg, and after a high-temperature destructive test at 62°C, the peroxide value was 1.1mmol / kg after 28 days.

[0124] Comparative Example 14

[0125] A method for preparing moderately processed ARA oil is different from that of Example 4 in that the molecular weight cutoff of the ultrafiltration membrane in step S4 is 7000Da, and the other steps and parameters are the same as those in Example 4.

[0126] After testing, the final ARA oil mass was 9.46kg, the recovery rate was 94.6%, the impurity content was 0.04%, the peroxide value was 0.11mmol / kg, and after a high-temperature destructive test at 62°C, the peroxide value was 0.56mmol / kg after 28 days.

[0127] Comparative Example 15

[0128] A method for preparing moderately processed ARA oil is different from that of Example 4 in that the molecular weight cutoff of the ultrafiltration membrane in step S4 is 3000Da, and the other steps and parameters are the same as those in Example 4.

[0129] After testing, the final ARA oil mass was 9.48kg, the recovery rate was 94.8%, the impurity content was 0.19%, the peroxide value was 0.13mmol / kg, and after a high-temperature destructive test at 62°C, the peroxide value was 0.68mmol / kg after 28 days.

[0130] Comparative Example 16

[0131] A method for preparing moderately processed ARA oil, which is different from Example 4 in that step S1 degumming adopts a hydration degumming method, specifically, 10 kg of ARA oil with an ARA content of 40% is heated to 60°C, 8% water by weight of the ARA oil is added, and the reaction is carried out at 60°C for 2.5 hours. The reacted oil is treated at a speed of 6000 r / min for 15 minutes to remove the protein precipitate to obtain a clear liquid. The other steps and parameters are the same as those in Example 4.

[0132] After testing, the final ARA oil mass was 9.57kg, the recovery rate was 95.7%, the impurity content was 0.13%, the peroxide value was 0.075mmol / kg, and after a high-temperature destructive test at 62°C, the peroxide value was 0.25mmol / kg after 28 days.

[0133] Comparative Example 17

[0134] A method for preparing moderately processed ARA oil, which is different from Example 4 in that step S1 degumming adopts an acid degumming method, specifically, 10 kg of ARA oil with an ARA content of 40% is heated to 60°C, 2% of the weight of the ARA oil and a volume concentration of 85% food-grade phosphoric acid is added, and the reaction is carried out at 60°C for 2.5 hours. The reacted oil is treated at a speed of 6000 r / min for 15 minutes to remove the protein precipitate to obtain a clear liquid. The other steps and parameters are the same as those in Example 4.

[0135] After testing, the final ARA oil mass was 9.53kg, the recovery rate was 95.3%, the impurity content was 0.15%, the peroxide value was 0.079mmol / kg, and after a high-temperature destructive test at 62°C, the peroxide value was 0.31mmol / kg after 28 days.

[0136] Comparison Example

[0137] The unprocessed ARA oil was tested and found to have a mass of 10 kg, an impurity content of 5.9%, and a peroxide value of 1.2 mmol / kg. After a high-temperature destructive test at 62°C, the peroxide value was 18.6 mmol / kg after 28 days.

[0138] Analysis of the Examples and Comparative Examples data:

[0139] After the ARA oil is treated by the process steps of Examples 1-4 of the present application, compared with the untreated ARA oil in the control example, the ARA oil recovery rate obtained in Examples 1-4 is above 95%, the impurity content is ≤0.08%, the peroxide value is less than 0.04%, and after a destruction test at 62°C, the peroxide value after 28 days is less than 0.06%. It can be seen that after the ARA oil is moderately processed in the present application, the impurity content in the ARA oil is reduced, the purity is improved, and the stability of the ARA oil is also improved.

[0140] Compared with Example 3, when only phospholipase B or phospholipase A1 was used as the protease in Example 6-7, the impurity content in the ARA oil obtained in Example 6-7 increased and the stability performance was also reduced, indicating that the combined use of the two proteases effectively improved the stability and quality of the ARA oil.

[0141] Compared with Example 3, when only silica gel or attapulgite is used as the decolorizing agent, the impurity content in the ARA oil obtained in Examples 8-9 increases and the stability performance decreases. The reason may be that when only attapulgite is used as the decolorizing agent, its active sites are occupied when adsorbing soap impurities, resulting in a decrease in decolorization ability.

[0142] Compared with Example 4, when only degumming or desugaring or extraction or ultrafiltration or decolorization or deodorization treatment is used, the recovery rate of ARA oil obtained in Comparative Examples 1-6 is lower than that in Example 4, and the impurity content and peroxide value are significantly increased compared with the impurity content and peroxide value in Example 4, and after the destruction test at 62°C, the peroxide value of ARA oil is increased by a hundred times compared with the peroxide value in Example 4. It can be seen that only degumming or desugaring or extraction or ultrafiltration or decolorization or deodorization treatment cannot improve the stability and purity of ARA oil. Therefore, the combination of the process steps of degumming, desugaring, extraction, ultrafiltration, decolorization and deodorization in this application can effectively improve the purity and stability of ARA oil.

[0143] Compared with Example 4, when the preparation step lacks supercritical extraction, the impurities and peroxide value of the ARA oil obtained in Comparative Example 7 are increased compared with those in Example 4, and after a destructive test at 62°C, the peroxide value of the ARA oil at 28 days is significantly increased compared with that in Example 4. It can be seen that the thermal stability of the ARA oil will also decrease without supercritical extraction.

[0144] Compared with Example 4, when the oil is first extracted and then degummed, desugared, etc., the peroxide value of the oil finally obtained in Comparative Example 8 is higher than that in Example 4. It can be seen that the processing sequence of the present application can make the final oil have high quality and good stability.

[0145] Compared with Example 4, when the amount of protease added is 3% exceeding the limit of the present application, the peroxide value of the ARA oil obtained in Comparative Example 8 is higher than that in Example 4, and after a destructive test at 62°C, its peroxide value is also much higher than that in Example 4. It can be seen that the addition of excessive protease may cause the destruction of beneficial ingredients and reduce the stability of ARA oil.

[0146] Compared with Example 4, when the ARA oil is not subjected to staged heat preservation treatment during the degumming process or when the staged heat preservation temperature exceeds the limit of the present application, the peroxide value of the ARA oil obtained in Comparative Examples 9-10 is increased compared with that in Example 4, and when the temperature is high during the degumming process, the reaction rate of the ARA oil with oxygen will be accelerated, and the ARA oil will be oxidized to produce hydroperoxides, which will further decompose to produce small molecules such as aldehydes and ketones, thereby reducing the stability of the oil. In addition, too high a degumming temperature may cause chemical changes in the phospholipids. For example, some phospholipids may be carbonized to produce black impurity particles, which affect the color and purity of the oil. It can be seen that the gradient heat preservation setting in the degumming process of the present application can make the ARA oil react quickly in the early stage, reduce the temperature in the middle stage to ensure a stable degumming rate, and slightly increase the temperature in the later stage, which can promote the effective removal of the remaining impurities, not only ensuring the purity of the ARA oil, but also avoiding the destruction of the beneficial ingredients in the ARA oil, thereby improving the stability of the ARA oil.

[0147] Compared with Example 4, when the desugaring treatment temperature or the decolorization and deodorization treatment temperature exceeds the limit of the present application, the result is that the peroxide value of the ARA oil obtained in Comparative Examples 11-12 increases, indicating that the stability of the ARA oil is reduced due to the high temperature.

[0148] Compared with Example 4, in Comparative Examples 14-15, when the molecular weight cutoff of the ultrafiltration membrane is too large or too small, the peroxide value of the ARA oil is increased compared with that in Example 4. The reason may be that when the molecular weight cutoff of the ultrafiltration membrane is too large, some large molecular beneficial components in the ARA oil are also filtered out, resulting in a decrease in the stability of the ARA oil. When the molecular weight cutoff is too small, some impurity components cannot be effectively removed, which not only affects the purity of the ARA oil, but also reduces the stability of the oil.

[0149] Compared with Example 4, the purity and stability of the oils and fats obtained by supercritical extraction after enzymatic degumming are better than those obtained by supercritical extraction after other degumming methods. The reason may be that after the oil and fat are treated with protease, the surface area of ​​the oil and fat raw material can be increased, the contact and diffusion rate between small molecules and supercritical fluid can be improved, which is more conducive to improving the extraction capacity of supercritical fluid, thereby improving the purity and stability of the oil and fat.

[0150] The embodiments of this specific implementation method are all preferred embodiments of the present invention, and are not intended to limit the protection scope of the present invention. Therefore, any equivalent changes made based on the structure, shape, and principle of the present invention should be included in the protection scope of the present invention.

Claims

1. A method for preparing moderately processed ARA oil, characterized in that: The following steps are involved: S1. Degumming: Heat the ARA oil to 55-60°C, add protease to react for 0.5-1h, then cool to 50-55°C and keep warm for 1-2h, then raise the temperature to 60°C and react for 0.5-1h, centrifuge the oil after the reaction to remove the precipitate and obtain a clear liquid; S2, desugaring: heat the clear liquid obtained in step S1 to 70-80°C, add activated carbon and stir for 30-45 minutes, then filter to obtain the desugared clear liquid; S3, extraction: subjecting the clear solution obtained in step S2 to supercritical extraction and separation, and then collecting the clear solution; S4, ultrafiltration: ultrafiltration treatment of the clear liquid obtained in step S3; S5, decolorization: decolorizing the clear solution obtained in step S4, S6, deodorization: The clear liquid obtained in step S5 is deodorized to obtain ARA oil.

2. A method for preparing a moderately processed ARA oil according to claim 1, characterized in that: During the supercritical extraction, the carbon dioxide flow rate is 25-30 L / h, the extraction pressure is 40-45 MPa, the extraction time is 100-150 min, and the extraction temperature is 35-40°C.

3. A method for preparing a moderately processed ARA oil according to claim 1, characterized in that: The separation pressure after supercritical extraction is 5-10 MPa and the separation temperature is 40-60°C.

4. A method for preparing a moderately processed ARA oil according to claim 1, characterized in that: The added amount of the protease is 0.5-2% of the weight of the ARA oil, and the protease is composed of phospholipase B and phospholipase A1 in a weight ratio of 1: (0.5-0.8).

5. A method for preparing a moderately processed ARA oil according to claim 1, characterized in that: The amount of activated carbon added is 2-3% of the weight of the clear solution obtained in step S1.

6. A method for preparing a moderately processed ARA oil according to claim 1, characterized in that: The ultrafiltration membrane in step S4 has a molecular weight cut-off of 4000-6000Da.

7. The method for preparing a moderately processed ARA oil according to claim 1, characterized in that: In step S5, the decolorization treatment temperature is 70-90° C., the treatment time is 20-40 min, and the amount of decolorizer added is 1-2% of the weight of the clear liquid.

8. A method for preparing a moderately processed ARA oil according to claim 5, characterized in that: The decolorizing agent is attapulgite and silica gel in a weight ratio of 1:

1.

9. The method for preparing a moderately processed ARA oil according to claim 1, characterized in that: The vacuum degree of the deodorization treatment is -0.005MPa, the treatment temperature is 160-180°C, and the treatment time is 30-40min.

10. The method for preparing a moderately processed ARA oil according to claim 1, characterized in that: The centrifugal speed in step S1 is 4000-6000 r / min, and the centrifugal time is 10-15 min.