CN105713721A - Method for concentrating DHA and EPA in fish oil - Google Patents
Method for concentrating DHA and EPA in fish oil Download PDFInfo
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- CN105713721A CN105713721A CN201610161177.9A CN201610161177A CN105713721A CN 105713721 A CN105713721 A CN 105713721A CN 201610161177 A CN201610161177 A CN 201610161177A CN 105713721 A CN105713721 A CN 105713721A
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- 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
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
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- 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
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/12—Refining fats or fatty oils by distillation
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C1/00—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids
- C11C1/02—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids from fats or fatty oils
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C1/00—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids
- C11C1/08—Refining
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C1/00—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids
- C11C1/08—Refining
- C11C1/10—Refining by distillation
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The invention discloses a method for concentrating DHA and EPA in fish oil. The method includes the following steps that 1, supercritical CO2 extraction, rectification and separation are conducted on the raw material fish oil in sequence to collect grease; 2, after parameters of supercritical CO2 extraction and rectification are set to be second-stage extraction parameters and rectification parameters, supercritical CO2 extraction, rectification and separation are sequentially conducted on the raw material fish oil treated in the step 1 to collect EPA; 3, after the parameters of supercritical CO2 extraction and rectification are set to be third-stage extraction and rectification parameters, supercritical CO2 extraction, rectification and separation are sequentially conducted on the raw material fish oil treated in the step 2 to collect DHA. DHA and EPA can be collected and concentrated separately, and the content of concentrated DHA and the content of concentrated EPA are high.
Description
Technical field
The invention belongs to biological pharmacy technical field, particularly relate to a kind of method of DHA and EPA in fish oil concentrated.
Background technology
The application of bathypelagic fish oil widely, can be applicable to the fields such as health care, medicine, food, chemical industry and feedstuff.In bathypelagic fish oil, n-3 polyunsaturated fatty acid (n-3PUFA) has important biological significance in human body, its characteristic fatty acid eicosapentaenoic acid (EicosapentaenoicAcid, and docosahexenoic acid (DocosahexaenoicAcid EPA), DHA) clearly, EPA has prevention coronary heart disease, blood pressure lowering, allaying tiredness to physiologically active, prevention of arterial is atherosis and cerebral thrombosis, the physiologically active such as anticancer；Human brain health-nutrition (if being obviously promoted the intelligent development of baby, improving cerebral function, improve memory), raising immunity, alzheimer's disease treatment field are played an important role by DHA.But at present in the fish oil of market, DHA content is generally at 20%-35%, and EPA content is generally at 5%-35%.Such low content not only can not meet health care demand, and cannot realize its good medical value, therefore, if well to play DHA and EPA function, it is necessary to DHA and the EPA in fish oil is further concentrated.
But the polyenoic fatty acid in bathypelagic fish oil, it is belong to heat and chemically unstable material including EPA and DHA, it is isolated purification and difficulty thereof, at present, the separating and purifying technology of DHA and EPA is mainly had following several: 1. urea adduct method, mainly utilize urea molecule can form stable crystal clathrate with linear saturated fatty acids or monounsaturated fatty acid in crystallization process to precipitate out, thus obtaining highly purified DHA and EPA mixed product, its shortcoming is response time length, product yield is low, be difficult to divide out DHA and EPA, residual urea is serious；2. low-temperature solvent crystallization process, mainly utilizes the difference of different fatty acid (salt) dissolubility in organic solvent under low temperature to separate purification.Its shortcoming is to need response time length, reclaim a large amount of organic solvent, and separation efficiency is not high；3. lipase concentration method, carries out selective hydrolysis to the triglyceride containing DHA/EPA, final enrichment polyvalent unsaturated fatty acid triglyceride, and its shortcoming is response time length, enrichment DHA and EPA melting concn is more than 60% still comparatively difficulty；4. adsorption method of separation, utilizes the fatty acid of the different saturation partition coefficient on adsorbent (such as silver ion) different and separates.Its shortcoming is the easy polluted product of eluant and to separate scale less；5. molecularly distilled, utilizes the difference of component of mixture molecular free path to be separated.Its shortcoming is to need high-vacuum apparatus, and temperature is high, and energy consumption is high；6. supercritical CO2Extraction, utilizes extractant CO2Excellent solvent character is had when uniform temperature and certain pressure, its advantage is the pigment, stink substance such as aldehydes, ketone and a portion free fatty etc. that are not only able to extract in fish oil, avoid the loaded down with trivial details techniques such as tradition deacidification, decolouring, degumming, deodorize, and can accepting in scope removal monounsaturated fatty acid, satisfied fatty acid, thus separating concentration DHA and EPA, its concentration time is short, it is simple and easy to operate, cost is low, do not have dissolvent residual simultaneously.
Adopt supercritical CO in recent years2Extracting rectifying extracts high-purity EPA-EE, DHA-EE at home and abroad attracts great attention; but EPA and DHA is the mixture preparing into both in prior art; owing to EPA and DHA is as incomplete same in both respective functions above-mentioned; EPA is better than DHA in the effect of preventing and treating cardiovascular and cerebrovascular disease, aspect of inflammation; but promoting nervous function; prevention senile dementia; protection vision aspect is that EPA does not possess; and EPA is not suitable for baby clothes use, cause that the application of fish oil is subject to certain restrictions.In published document, also there is trial by EPA and DHA separate collection, but need to by urea clathration technology in its separation process, and thus result in the complex process collecting EPA and DHA respectively, cost is high, the problem that purity is relatively low.
Summary of the invention
It is an object of the invention to provide a kind of method of DHA and EPA in fish oil concentrated.To solve to collect respectively the complex process of EPA and DHA, cost is high, the problem that purity is relatively low.
In order to realize foregoing invention purpose, one aspect of the present invention, it is provided that a kind of method of DHA and EPA in fish oil concentrated.The method of DHA and EPA in described fish oil concentrated, comprises the following steps:
By raw material fish oil through supercritical CO2Extraction processes, rectification process, and separating treatment collects oils and fats；Wherein, described supercritical CO2The Stress control extracted is 10MPa-25MPa；The rectification Stress control of described rectification process is 9MPa-13Mpa；The time of described rectification is 0.5h-3h；Then
By described supercritical CO2The pressure extracted adjusts to 10MPa-25MPa；It is 12MPa-15Mpa by the rectification Stress control of described rectification process；The rectification time is 0.5h-3h, and separating treatment collects concentration EPA；Again
By described supercritical CO2The pressure extracted adjusts to 10MPa-25MPa；It is 14MPa-17Mpa by the rectification Stress control of described rectification process；The rectification time is 0.5h-2h, and separating treatment collects concentration DHA.
Wherein, described supercritical CO2The temperature that extraction processes is 32 DEG C-52 DEG C.
Compared with prior art, in fish oil concentrated of the present invention, the method for DHA and EPA is by the adjustment of temperature, pressure, first most satisfied fatty acid, monounsaturated fatty acid in fish oil is removed, then DHA and EPA in fish oil is collected respectively, and their content improves with the raising of raw material fish oil concentration respectively, and wherein DHA content can be 4-5 times of raw material fish oil, is up to more than 85%, EPA content can be 2-3 times of raw material fish oil, reaches as high as more than 65%.It is simple and easy and easily-controllable that this crosses the inventive method technique, reaches concentrated effect within a short period of time, and efficiency is high, and DHA and the EPA of concentration is relatively stable, and producing for high concentration DHA and EPA industrialization provides technical support, and no solvent residue, safety.
Accompanying drawing explanation
Fig. 1 is the process flow diagram of the method for DHA and EPA in embodiment of the present invention fish oil concentrated.
Fig. 2 is the subcritical enzymatic reaction schematic diagram of the fatty acid triglycercide for preparing EPA, DHA that the embodiment of the present invention provides.
Detailed description of the invention
In order to make the technical problem to be solved in the present invention, technical scheme and beneficial effect clearly understand, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein is only in order to explain the present invention, is not intended to limit the present invention.
Embodiments provide one and utilize supercritical CO2The method of DHA and the EPA in extraction fish oil concentrated respectively.In one embodiment, in the embodiment of the present invention fish oil concentrated method technological process of DHA and EPA as it is shown in figure 1, it comprises the following steps:
Step S01: by supercritical CO2The parameter setting of extraction process and rectification process is after first stage extraction, rectification parameters, and raw material fish oil is sequentially passed through supercritical CO2Extraction processes, rectification process, and separating treatment collects oils and fats；
Step S02: by supercritical CO2The parameter setting of extraction process and rectification process is after second stage extraction, rectification parameters, and the raw material fish oil after above-mentioned steps S01 processes is sequentially passed through supercritical CO again2Extraction process, rectification process and separating treatment, it is achieved the collection of EPA；
Step S03: by supercritical CO2The parameter setting of extraction process and rectification process is after phase III extraction, rectification parameters, and the raw material fish oil after above-mentioned steps S02 processes also is sequentially passed through supercritical CO2Extraction process, rectification process and separating treatment, it is achieved the collection of DHA；
Specifically, in above-mentioned steps S01, through the supercritical CO of first stage2Extraction process, rectification and separating treatment are to remove except the purpose of satisfied fatty acid most in raw material fish oil, monounsaturated fatty acid, to realize collecting in subsequent step DHA and the EPA of concentration high concentration.Therefore, in order to effectively remove the purpose of most satisfied fatty acid, monounsaturated fatty acid in raw material fish oil, in one embodiment, first stage supercritical CO2The temperature that extraction processes is set as 32 DEG C-52 DEG C, and Stress control is 10MPa-25MPa；The Stress control of rectification process described in the first stage is 9MPa-13Mpa；The time of described rectification is 0.5h-3h.
In a further embodiment, this first stage rectification process is to adopt level Four temperature control, is followed successively by: rectification I temperature is 35 DEG C-50 DEG C, and rectification II temperature is 40 DEG C-60 DEG C, and rectification III temperature is 42 DEG C-55 DEG C, and rectification IV temperature is 70 DEG C-85 DEG C.In a particular embodiment, this rectification process can adopt level Four rectifying column equipment to realize, and respectively the temperature of rectifying columns at different levels is adjusted and controls, level Four rectifying column 3 as shown in Figure 2.
The supercritical CO of this first stage2Extraction processes can directly adopt supercritical CO2Extraction equipment realizes.Separating treatment in this step S01 can adopt separating still to realize, and in one embodiment, the condition of separating treatment is: temperature is 35 DEG C-55 DEG C, and pressure is 4MPa-10MPa.
Raw material fish oil in this step S01 can be bathypelagic fish oil product commercially available on the market.Can be through the crude fish oil that bathypelagic fish refines voluntarily.In a particular embodiment, this raw material fish oil is ethyl ester type fish oil, and after measured, DHA content contained in this ethyl ester type fish oil is generally at 10%-30%, and EPA content is generally at 10%-35%.
Through for raw material fish oil carry out the first stage supercritical extraction process, rectification process, separating treatment collect major part be satisfied fatty acid, monounsaturated fatty acid oils and fats can as other use, such as raw material etc..
In above-mentioned steps S02, the separation again that the raw material fish oil after step S01 processes is carried out is the EPA in order to obtain high concentration.Therefore, in one embodiment, second stage supercritical CO2The temperature that extraction processes is set as 32 DEG C-52 DEG C, and Stress control is 10MPa-25MPa；The Stress control of rectification process described in second stage is 12MPa-15Mpa；The time of described rectification is 0.5h-3h.
In a further embodiment, as described in above-mentioned steps S01, this second stage rectification process is to adopt level Four temperature control, it is followed successively by: rectification I temperature is 35 DEG C-50 DEG C, rectification II temperature is 40 DEG C-60 DEG C, and rectification III temperature is 42 DEG C-55 DEG C, and rectification IV temperature is 70 DEG C-85 DEG C.In a particular embodiment, this rectification process can adopt level Four rectifying column equipment to realize, and respectively the temperature of rectifying columns at different levels is adjusted and controls, level Four rectifying column 3 as shown in Figure 2.
As described in above-mentioned steps S01, the supercritical CO of this second stage2Extraction processes can directly adopt supercritical CO2Extraction equipment realizes.The separating treatment of second stage can adopt separating still to realize, and in one embodiment, the condition of separating treatment is: temperature is 35 DEG C-55 DEG C, and pressure is 4MPa-10MPa.
By to above-mentioned critical CO2The control of extraction process and rectification process temperature and pressure and time, the concentration that separating treatment collects concentration EPA is made to be not less than 60%, and the content being as EPA in raw material fish oil raises and raises, it can be 2-3 times of raw material fish oil as collection can be made to concentrate EPA content, reach as high as more than 65%, certainly less than 100%；Through concentrating DHA content≤10% being mixed in EPA as described in recording.
In above-mentioned steps S03, the also separation that the raw material fish oil after step S02 processes is carried out is the DHA in order to obtain high concentration.Therefore, in one embodiment, phase III supercritical CO2The temperature that extraction processes is set as 32 DEG C-52 DEG C, and Stress control is 10MPa-25MPa；The Stress control of rectification process described in second stage is 14MPa-17Mpa；The time of described rectification is 0.5h-2h.
In a further embodiment, as described in above-mentioned steps S01, this phase III rectification process is to adopt level Four temperature control, it is followed successively by: rectification I temperature is 35 DEG C-50 DEG C, rectification II temperature is 40 DEG C-60 DEG C, and rectification III temperature is 42 DEG C-55 DEG C, and rectification IV temperature is 70 DEG C-85 DEG C.In a particular embodiment, this rectification process can adopt level Four rectifying column equipment to realize, and respectively the temperature of rectifying columns at different levels is adjusted and controls, level Four rectifying column 3 as shown in Figure 2.
As described in above-mentioned steps S01, the supercritical CO of this phase III2Extraction processes can directly adopt supercritical CO2Extraction equipment realizes.The separating treatment of phase III can adopt separating still to realize, and in one embodiment, the condition of separating treatment is: temperature is 35 DEG C-55 DEG C, and pressure is 4MPa-10MPa..
By to above-mentioned critical CO2The control of extraction process and rectification process temperature and pressure and time, the concentration that separating treatment collects concentration DHA is made to be not less than 70%, and the content being as DHA in raw material fish oil raises and raises, it can be 4-5 times of raw material fish oil as collection can be made to concentrate DHA content, reach as high as more than 85%, certainly less than 100%；Through concentrating EPA content≤10% being mixed in DHA as described in recording.
It addition, in order to improve the effect extracting concentration further, improve concentration DHA and concentration EPA purity, in whole extraction concentration process, as one embodiment of the invention, control CO2Flow velocity be 1L/h-20L/h.
Therefore, in embodiment of the present invention fish oil concentrated, the method for DHA and EPA is by the adjustment of temperature, the adjustment of pressure and extraction process, it is capable of separate collection and the concentration of DHA and EPA, the DHA content making concentration can for 4-5 times of raw material fish oil, it is up to more than 85%, the EPA content making concentration for 2-3 times of raw material fish oil, can reach as high as more than 65%.And, embodiment of the present invention method technique is simple and easy and easily-controllable, reaches concentrated effect within a short period of time, and efficiency is high, and DHA and the EPA of concentration is relatively stable, and producing for high concentration DHA and EPA industrialization provides technical support, and no solvent residue, safety.
It is further described below in conjunction with specific embodiment.
Case study on implementation 1
The present embodiment provides a kind of can distinguish the method for DHA and EPA in fish oil concentrated.For the device connection diagram of DHA and EPA such as accompanying drawing 2 in fish oil concentrated, the present embodiment method comprises the steps:
Step S11: put in supercritical extraction reactor 2 by raw material fish oil 50mL, extraction kettle 2 pressure adjusts to 12.3MPa, and rectifying column 3 pressure adjusts to 11.1Mpa, and the response time is 1.5h, and separating still 4 collects to obtain fat A 1；
Step S12: on step S11 basis, adjusts extraction kettle 2 pressure to 13MPa, increases rectifying column 3 pressure to 12.1Mpa, and the response time is 0.75h, and separating still 4 collects to obtain fat A 2, is namely concentration EPA；
Step S13: on step S12 basis, extraction kettle 2 pressure adjusts to 15MPa, increases rectifying column 3 pressure to 14.2Mpa, and the response time is 1h, and separating still 4 collects to obtain fat A 3, is namely concentration DHA.
Wherein, the raw material fish oil in above-mentioned steps S11 be the DHA content that market is bought reach 25%, EPA content reach 32% ethyl ester type fish oil, in step S11 to step S13, extraction kettle 2 temperature is 50 DEG C；Separating still 4 temperature is 45 DEG C, and pressure is 5.9MPa；In rectifying column 3, rectification I temperature is 35 DEG C, and rectification II temperature is 45 DEG C, and rectification III temperature is 65 DEG C, and rectification IV temperature is 80 DEG C；CO in whole extraction concentration2By CO2Steel cylinder 1 provides, and controls CO2Flow velocity is 6L/h.
Case study on implementation 2
The present embodiment provides a kind of can distinguish the method for DHA and EPA in fish oil concentrated.For the device connection diagram of DHA and EPA such as accompanying drawing 2 in fish oil concentrated, the present embodiment method comprises the steps:
Step S21: put in still supercritical extraction reactor 2 by raw material fish oil 50mL, extraction kettle 2 pressure adjusts to 25MPa, and rectifying column 3 pressure adjusts to 12Mpa, and the response time is 2h, and separating still 4 collects to obtain fat A 1；
Step S22: on step S21 basis, extraction kettle 2 pressure adjusts to 25MPa, increases rectifying column 3 pressure to 14Mpa, and the response time is 45min, and separating still 4 collects to obtain fat A 2, is namely concentration EPA；
Step S23: on step S22 basis, extraction kettle 2 pressure adjusts to 25MPa, increases rectifying column 3 pressure to 17Mpa, and the response time is 0.5h, and separating still 4 collects to obtain fat A 3, is namely concentration DHA.
Wherein, the raw material fish oil in above-mentioned steps S21 be the DHA content that market is bought reach 25%, EPA content reach 32% ethyl ester type fish oil, in step S21 to step S23, extraction kettle 2 temperature is 40 DEG C；Separating still 4 temperature is 55 DEG C, and pressure is 8MPa；In rectifying column 3, rectification I temperature is 45 DEG C, and rectification II temperature is 55 DEG C, and rectification III temperature is 65 DEG C, and rectification IV temperature is 75 DEG C；CO in whole extraction concentration2By CO2Steel cylinder 1 provides, and controls CO2Flow velocity is 9L/h.
Case study on implementation 3
The present embodiment provides a kind of can distinguish the method for DHA and EPA in fish oil concentrated.For the device connection diagram of DHA and EPA such as accompanying drawing 2 in fish oil concentrated, the present embodiment method comprises the steps:
Step S31: put in still supercritical extraction reactor 2 by raw material fish oil 50mL, extraction kettle 2 pressure adjusts to 15MPa, and rectifying column 3 pressure adjusts to 10.8Mpa, and the response time is 1.75h, collects to obtain fat A 1 at separating still 4；
Step S32: on step S31 basis, extraction kettle 2 pressure adjusts to 15MPa, increases rectifying column 3 pressure to 12Mpa, and the response time is 45min, collects to obtain fat A 2 at separating still 4, is namely concentration EPA；
Step S33: on step S32 basis, extraction kettle 2 pressure adjusts to 20MPa, increases rectifying column 3 pressure to 15Mpa, and the response time is 45min, collects to obtain fat A 3 at separating still 4, is namely concentration DHA.
Wherein, the raw material fish oil in above-mentioned steps S31 be the DHA content that market is bought reach 25%, EPA content reach 32% ethyl ester type fish oil, in step S31 to step S33, extraction kettle 2 temperature is 40 DEG C；Separating still 4 temperature is 50 DEG C, and pressure is 4.6MPa；In rectifying column 3, rectification I temperature is 40 DEG C, and rectification II temperature is 50 DEG C, and rectification III temperature is 65 DEG C, and rectification IV temperature is 85 DEG C；CO in whole extraction concentration2By CO2Steel cylinder 1 provides, and controls CO2Flow velocity is 6L/h.
Comparative example 1
This comparative example provides a kind of method of DHA and EPA in fish oil concentrated, and this comparative example method comprises the steps:
Step S11: putting in reactor by raw material fish oil 50mL, extraction kettle pressure adjusts to 20MPa, increases rectifying column pressure to 12Mpa, and the response time is 0.75h, and separating still collects to obtain fat A 2；
Step S12: extraction kettle pressure adjusts to 20MPa, increases rectifying column pressure to 15Mpa, and the response time is 0.75h, and separation reactor I collects to obtain fat A 3.
Wherein, extraction kettle temperature is 32 DEG C；Separating still temperature is 40 DEG C, and pressure is 5.9MPa；In rectifying column, rectification I temperature is 35 DEG C, and rectification II temperature is 45 DEG C, and rectification III temperature is 55 DEG C, and rectification IV temperature is 65 DEG C；CO in whole extraction concentration2By CO2Steel cylinder 1 provides, and controls CO2Flow velocity is 18L/h.
DHA and EPA content in concentrate in embodiment 1-3 and comparative example 1 are measured.Wherein, DHA and EPA content analyzing detecting method are to detect according to GB/T17377-2008 " analysis of animal and plant fat fatty acid methyl ester chromatography of gases ".Result is as shown in table 1 below:
Table 1
By upper table 1 it can be seen that the method for DHA and EPA is by the adjustment of temperature, the adjustment of pressure and extraction process in embodiment of the present invention fish oil concentrated, it is possible to realize separate collection and the concentration of DHA and EPA so that the DHA of concentration and EPA content are high.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all any amendment, equivalent replacement and improvement etc. made within the spirit and principles in the present invention, should be included within protection scope of the present invention.
Claims (6)
1. a method of DHA and EPA in fish oil concentrated, comprises the following steps:
By raw material fish oil through supercritical CO2Extraction processes, rectification process, and separating treatment collects oils and fats；Wherein, described supercritical CO2The Stress control extracted is 10MPa-25MPa；The rectification Stress control of described rectification process is 9MPa-13Mpa；The time of described rectification is 0.5h-3h；Then
By described supercritical CO2The pressure extracted adjusts to 10MPa-25MPa；It is 12MPa-15Mpa by the rectification Stress control of described rectification process；The rectification time is 0.5h-3h, and separating treatment collects concentration EPA；Again
By described supercritical CO2The pressure extracted adjusts to 10MPa-25MPa；It is 14MPa-17Mpa by the rectification Stress control of described rectification process；The rectification time is 0.5h-2h, and separating treatment collects concentration DHA.
Wherein, described supercritical CO2The temperature that extraction processes is 32 DEG C-52 DEG C.
2. the method for claim 1, it is characterised in that: described rectification process is to adopt level Four temperature control, is followed successively by: rectification I temperature is 35 DEG C-50 DEG C, and rectification II temperature is 40 DEG C-60 DEG C, and rectification III temperature is 42 DEG C-55 DEG C, and rectification IV temperature is 70 DEG C-85 DEG C.
3. the method for claim 1, it is characterised in that: the temperature of described separating treatment is 35 DEG C-55 DEG C, and pressure is 4MPa-10MPa.
4. the method as described in as arbitrary in claim 1-3, it is characterised in that: described CO2Flow velocity be 1L/h-20L/h.
5. the method as described in as arbitrary in claim 1-3, it is characterised in that: described concentration DHA concentration is not less than 70%, less than 100%；Wherein, EPA content≤10% being mixed in described concentration DHA.
6. the method as described in as arbitrary in claim 1-3, it is characterised in that: described concentration EPA concentration is not less than 60%, less than 100%；Wherein, DHA content≤10% being mixed in described concentration EPA.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110668945A (en) * | 2019-09-29 | 2020-01-10 | 青岛利和生物科技有限公司 | Method for extracting DHA and EPA in fish oil by combining supercritical fluid |
| CN111995517A (en) * | 2020-08-19 | 2020-11-27 | 中国科学院深圳先进技术研究院 | Preparation method of eicosapentaenoic acid ethyl ester |
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| CN110668945A (en) * | 2019-09-29 | 2020-01-10 | 青岛利和生物科技有限公司 | Method for extracting DHA and EPA in fish oil by combining supercritical fluid |
| CN110668945B (en) * | 2019-09-29 | 2022-02-15 | 青岛利和生物科技有限公司 | Method for extracting DHA and EPA in fish oil by combining supercritical fluid |
| CN111995517A (en) * | 2020-08-19 | 2020-11-27 | 中国科学院深圳先进技术研究院 | Preparation method of eicosapentaenoic acid ethyl ester |
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Inventor after: Chen Lijuan Inventor after: Wang Jianyun Inventor after: Dou Shuhua Inventor after: Zhong Zhou Inventor after: Li Yue Inventor after: Huang Shishu Inventor before: Chen Lijuan Inventor before: Wang Jianyun Inventor before: Dou Shuhua Inventor before: Zhong Zhou Inventor before: Li Yue |
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