CN112940848B - EPA-enriched microalgae grease with different polarities and preparation method thereof - Google Patents
EPA-enriched microalgae grease with different polarities and preparation method thereof Download PDFInfo
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- CN112940848B CN112940848B CN201911265923.9A CN201911265923A CN112940848B CN 112940848 B CN112940848 B CN 112940848B CN 201911265923 A CN201911265923 A CN 201911265923A CN 112940848 B CN112940848 B CN 112940848B
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- 239000005909 Kieselgur Substances 0.000 description 4
- 241000206744 Phaeodactylum tricornutum Species 0.000 description 4
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 4
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- 239000002253 acid Substances 0.000 description 1
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- JAZBEHYOTPTENJ-JLNKQSITSA-N all-cis-5,8,11,14,17-icosapentaenoic acid Chemical compound CC\C=C/C\C=C/C\C=C/C\C=C/C\C=C/CCCC(O)=O JAZBEHYOTPTENJ-JLNKQSITSA-N 0.000 description 1
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- JAZBEHYOTPTENJ-UHFFFAOYSA-N eicosapentaenoic acid Natural products CCC=CCC=CCC=CCC=CCC=CCCCC(O)=O JAZBEHYOTPTENJ-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
-
- 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
- C11B3/10—Refining fats or fatty oils by adsorption
Abstract
The invention relates to the field of microalgae grease extraction, and discloses microalgae grease rich in EPA with different polarities and a preparation method thereof, wherein the method comprises the following steps: extracting microalgae biomass by an organic solvent for at least two times, and separating the extracted materials to obtain microalgae grease and raffinate after each extraction; wherein, the 1+n-th organic solvent extraction takes raffinate obtained by separating the n-th organic solvent extraction as a raw material, and the dielectric constant of the organic solvent used in each extraction is sequentially increased; wherein n is an integer not less than 1. The preparation method has the advantages of short treatment time, low preparation temperature, low organic solvent consumption and the like, and reduces the production cost. The EPA-enriched microalgae grease with different polarities contains EPA algae oil with different physicochemical properties and molecular structures, the EPA content in the algae oil is high, the content of pollutants such as heavy metals is low, and the requirements of different health fields can be met.
Description
Technical Field
The invention relates to the field of microalgae grease preparation, in particular to EPA-enriched microalgae grease with different polarities and a preparation method thereof.
Background
EPA, eicosapentaenoic acid (Eicosapntemacnioc Acid), is an omega-3 series polyunsaturated fatty acid, the molecule of which contains 20 carbon atoms and 5 double bonds, the first double bond is located on the third carbon atom of the methyl end, and is a fatty acid which cannot be synthesized by human body, and a large number of researches prove that EPA has multiple physiological functions.
In recent years, various extraction techniques for extraction of microalgae oil and fat and EPA therein are gradually developed: 1) The organic solvent extraction method is simple and easy to operate, and the main solvents include methanol, ethanol, acetone, ethyl acetate, diethyl ether, n-hexane and the like; 2) The supercritical extraction method has the characteristics of convenient and easy operation, entrainer use and certain selectivity, but has the defects of long extraction time, high pressure, high requirement on equipment and difficult mass production; 3) The microwave extraction method has the characteristics of low extraction temperature, short time, targeted extraction and the like, ethanol is commonly used as an extraction solvent, but the disadvantage is that the extracted substances are easy to undergo degradation reaction in the extraction process; 4) The ultrasonic extraction method has the characteristics of strengthening external field intervention, enhancing solvent penetration capacity and improving extraction efficiency, but has the defect that the extracts are easy to undergo chemical reactions such as oxidation and the like in the extraction process; 5) The accelerating solvent extraction method has the characteristics of short extraction time and small solvent consumption, but has the defects of high temperature and pressure, high equipment requirement and easy isomerization, oxidation and other chemical reactions of extraction in the extraction process; 6) The enzyme-assisted extraction method has the advantages of high extraction efficiency, small solvent consumption and maintained antioxidant activity, but has the disadvantages of difficult maintenance of enzyme activity, common use of dimethyl ether as an extraction solvent and high extraction cost. In the method, the organic solvent extraction method basically has no problems as in the above 2) -6), can be used for realizing the large-scale production of EPA-containing microalgae grease, and has industrial application prospect.
However, the existing organic solvent extraction method mainly obtains lipid mixtures with extremely complex physical and chemical properties and molecular structures, and the EPA content in the microalgae grease can be further improved and the quality is improved through a complex separation and purification process. In addition, the obtained microalgae grease contains a mixture of lipid compounds with different physical and chemical properties and molecular structures, so that the functions of the different types of lipid compounds are not fully exerted, the process route is complex, and industrial production is difficult to realize.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provide a preparation method of EPA-enriched microalgae grease with different polarities.
In order to achieve the above object, the present invention provides a method for preparing microalgae grease rich in EPA with different polarities, which comprises: extracting microalgae biomass by an organic solvent for at least two times, and separating the extracted materials to obtain microalgae grease and raffinate after each extraction;
wherein, the 1+n-th organic solvent extraction takes raffinate obtained by separating the n-th organic solvent extraction as a raw material, and the dielectric constant of the organic solvent used in each extraction is sequentially increased;
wherein n is an integer not less than 1.
Preferably, the method further comprises:
1) Adding a nonpolar organic solvent into the microalgae biomass, performing first extraction, and separating to obtain microalgae grease I and raffinate I;
2) Adding a polar organic solvent I into the raffinate I, performing second extraction, and separating to obtain microalgae grease II and raffinate II;
3) Adding a polar organic solvent II into the raffinate II, performing third extraction, and separating to obtain microalgae grease III and raffinate III;
wherein the polarity of the polar organic solvent I is smaller than the dielectric constant of the polar organic solvent II.
Preferably, the microalgae grease obtained after each extraction is respectively adsorbed by an adsorbent;
wherein the adsorbents used for adsorbing the microalgae grease obtained after each extraction are the same or different from each other.
In another aspect, the invention provides EPA-enriched microalgae grease with different polarities prepared by the method.
The technical scheme provided by the invention also has the following technical advantages:
(1) In the extraction process, because the organic solvents with different physical and chemical properties such as polarity are used for step extraction, different types of lipid substances can be selectively extracted, other components with larger difference with the physical and chemical properties of the solvents are only partially extracted or not extracted, and microalgae grease with higher EPA content is obtained by each extraction. And the physicochemical properties, molecular structures and biological activities of at least two microalgae grease obtained are different, so that different biological demands can be met, and selective application can be performed.
(2) The impurities in the microalgae grease obtained through selective extraction basically have similar or similar physicochemical properties to the used organic solvent, and pigments such as chlorophyll and other impurities can be removed by preferably adopting a simple decoloring and purifying process, namely the removal rate of the impurities is improved, the EPA content in the microalgae grease is further improved, and a plurality of different impurity removal methods are not required to be adopted for the properties of different impurities.
(3) Compared with the prior art, the method has the advantages that the same microalgae samples are treated, the content of pollutants such as heavy metals in at least two microalgae grease is lower, the requirements in the national standard of related fields (such as food fields) can be met, and the requirements of different health fields can be met.
(4) The preparation method has the advantages of short treatment time, low preparation temperature, low organic solvent consumption and the like, and reduces the production cost.
(5) The invention is applicable to various microalgae, has wide application range and is easy to realize scale.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Detailed Description
The following describes specific embodiments of the present invention in detail. It should be understood that the detailed description and specific examples, while indicating and illustrating the invention, are not intended to limit the invention.
In the present invention, the term "polarity" refers chemically to a covalent bond or the non-uniformity of charge distribution in a covalent molecule. If the charge distribution is not uniform, the bond or molecule is said to be polar; if uniform, it is referred to as nonpolar. The polarity of the solvent can be judged according to the dielectric constant of the solvent, and the larger the dielectric constant is, the larger the polarity is.
In the present invention, the inventors found that EPA has different content distribution in various lipid compounds (such as free fatty acid, fatty glyceride, glycolipid, phospholipid, membrane lipid, etc.), and it is understood that these lipid compounds having different physicochemical properties and molecular structures have different biological activities.
In one aspect, the invention provides a method for preparing EPA-enriched microalgae grease with different polarities, comprising the following steps: extracting microalgae biomass by an organic solvent for at least two times, and separating the extracted materials to obtain microalgae grease and raffinate after each extraction;
wherein, the 1+n-th organic solvent extraction takes raffinate obtained by separating the n-th organic solvent extraction as a raw material, and the dielectric constant of the organic solvent used in each extraction is sequentially increased;
wherein n is an integer not less than 1.
It is understood that the number of extractions may be selected according to practical needs, for example, 2, 3, 4, 5 or more extractions may be performed, and the dielectric constant of the organic solvent used for each extraction increases sequentially. For example, when the number of extractions is 2, the dielectric constant of the organic solvent used for the second extraction is greater than that of the organic solvent used for the first extraction. For another example, when the number of extractions is 3, the dielectric constant of the organic solvent used in the first extraction is smaller than that of the organic solvent used in the second extraction, and the dielectric constant of the organic solvent used in the second extraction is smaller than that of the organic solvent used in the third extraction. And in other times of extraction, selecting an organic solvent according to the same rule to finish extraction of the microalgae grease.
It will be appreciated that when the number of extractions is small, a certain amount of microalgae grease and EPA may remain in the raffinate obtained from the last extraction, and as the number of extractions increases, the amount of microalgae grease and EPA remaining in the raffinate obtained from the last extraction may be reduced or even reduced, but this may result in an increase in the amount of organic solvent, an increase in the treatment steps, etc., and there may be a case where the amount of extracted microalgae grease and EPA is small. Therefore, the person skilled in the art can determine the appropriate number of extractions, preferably 2-4, according to the actual need.
According to a preferred embodiment of the present invention, the number of times of extraction is 3, and specifically, the preparation method of the microalgae lipid may include:
1) Adding a nonpolar organic solvent into the microalgae biomass, performing first extraction, and separating to obtain microalgae grease I and raffinate I;
2) Adding a polar organic solvent I into the raffinate I, performing second extraction, and separating to obtain microalgae grease II and raffinate II;
3) And adding a polar organic solvent II into the raffinate II, performing third extraction, and separating to obtain microalgae grease III and raffinate III.
It is understood that the dielectric constant of the nonpolar organic solvent is smaller than that of the polar organic solvent I, which is further smaller than that of the polar organic solvent II.
In the present invention, the nonpolar organic solvent may be a nonpolar organic solvent conventionally used in the art. In the present invention, the dielectric constant of the nonpolar organic solvent is preferably 4.5 or less, and the nonpolar organic solvent is preferably n-hexane and/or diethyl ether. According to the similar principle of miscibility, most of the components in the microalgae grease I extracted by adopting the nonpolar organic solvent have lower polarity, namely the polarity of the components is relatively close to that of the nonpolar organic solvent. Theoretically, the main component in the microalgae grease I is triglyceride.
Wherein the term "triglyceride" is also known as a fatty acyl glycerol, and is a constituent of a lipid, which is a lipid formed from glycerol and 3 fatty acids.
In the present invention, the polar organic solvent may be a polar organic solvent conventionally used in the art. In the present invention, the polar organic solvents are classified into two major categories according to the magnitude of the dielectric constants thereof, namely, the organic solvent 1 and the organic solvent II, wherein the dielectric constant of the organic solvent I is lower than that of the organic solvent II, and it is understood that the boundary point of the dielectric constants of the organic solvent 1 and the organic solvent II may be any one value, such as a value of 5, 10, 15, 20, 25, 30, 40, 50, 60 or even higher and any value between any two values.
In the present invention, the polar organic solvent I is preferably any organic solvent having a dielectric constant in the range of more than 4.5 and less than 15. The polar organic solvent I is preferably ethyl acetate and/or chloroform. According to the similar principle of miscibility, the polarity of most of the components in the microalgae grease II extracted by adopting the polar organic solvent I is higher than that of most of the components in the microalgae grease I. In theory, the main component in the microalgae grease II is glycolipid.
Wherein the term "glycolipid" refers to a lipid compound containing a glycosyl ligand.
In the present invention, the polar organic solvent II is preferably any organic solvent having a dielectric constant of 15 or more. The polar organic solvent II is preferably selected from at least one of ethanol, acetone and methanol. According to the similar principle of compatibility, most of components in the microalgae grease III extracted by adopting the polar organic solvent II have the highest polarity. In theory, the main component in the microalgae grease III is phospholipids.
Wherein the term "phospholipid" refers to a lipid containing phosphoric acid.
In the present invention, the organic solvent used in each extraction may be a mixed solvent of different solvents or may be a single solvent, and preferably a single solvent is used, that is, one organic solvent is used in each extraction. Under the preferred condition, the solvent can be recycled, so that the loss of the organic solvent is reduced, and the production cost is saved.
In a preferred embodiment of the present invention, the number of times of extraction is 3, and specifically, the preparation method of the microalgae lipid may include: 1) Adding normal hexane into the microalgae biomass, performing first extraction, and separating to obtain microalgae grease I and raffinate I; 2) Adding ethyl acetate into the raffinate I, performing second extraction, and separating to obtain microalgae grease II and raffinate II; 3) And adding ethanol into the raffinate II, performing third extraction, and separating to obtain microalgae grease III and raffinate III. Under the condition, a plurality of microalgae grease with different physicochemical properties and higher EPA content can be obtained, and higher grease extraction rate and higher EPA total amount can be realized in each extraction process.
In the present invention, in the at least two organic solvent extractions, the method of each extraction is not particularly limited, and for example, water bath heating extraction, oil bath heating extraction, air bath heating extraction, or the like may be used; preferably, each organic solvent extraction is independently a water bath heating extraction.
In the present invention, in the at least two organic solvent extractions, the liquid-to-material ratio of each extraction process is not particularly limited, and one skilled in the art can determine according to the nature of the organic solvent and microalgae. In the preferred case, in the at least two organic solvent extractions, the liquid-to-material ratio of the organic solvent used for each extraction to the microalgae biomass is 2-40mL/g, preferably 3-10mL/g, independently, so that the extraction rate of the microalgae oil can be further improved. It should be understood that the microalgae biomass is based on the dry weight of the microalgae biomass initially added, rather than the dry weight of the raffinate during extraction.
In the present invention, in the at least two organic solvent extractions, the time of each extraction may not be particularly limited, and for example, the time of each extraction may be 10 to 60 minutes each independently.
In the present invention, in the at least two organic solvent extractions, the temperature of each extraction may not be particularly limited, and for example, the temperature of each extraction may be 25 to 40 ℃ each independently.
In the present invention, in order to improve the extraction efficiency, each extraction may be combined with other methods conventionally used in the art, such as stirring, shaking, grinding, ultrasonic or microwave, and the like, and those skilled in the art may choose according to the actual situation.
In the present invention, after each extraction is completed, the post-treatment may be performed according to technical means conventionally used in the art. For example, the materials after each extraction may be separated by centrifugation into an organic solvent phase containing the microalgae oils and fats and a raffinate phase, it being understood that the organic solvent phase contains the extracted microalgae oils and fats containing EPA. The parameters of the centrifugation are not particularly limited and may be adjusted according to actual conditions.
In the present invention, the organic solvent in the organic solvent phase may be separated by using a technical means conventionally used in the art (for example, a nitrogen blower may be used for purging), and the separated microalgae grease may be dried.
The condition of the nitrogen blowing instrument for purging and separating can be selected in a wider range, for example, the flow rate of the nitrogen in the nitrogen blowing instrument can be 0.5-5.0mL/min, the working temperature can be 30-60 ℃, and the nitrogen blowing is finished when the volume of the organic solvent phase is not changed obviously any more.
Wherein the drying conditions may be selected within a wide range as long as the activity of the microalgae lipid, particularly EPA, is not substantially impaired, preferably the drying is performed under vacuum at room temperature (20-40 ℃) and the extent of the drying is preferably such that the microalgae lipid is constant in weight.
According to the method, the microalgae grease in the microalgae biomass is extracted, so that the microalgae grease with higher EPA content and different physicochemical properties can be obtained, and the higher grease extraction rate and higher EPA total amount can be realized in each extraction process; preferably, in order to further increase the content of EPA in the microalgae grease obtained after each extraction, the method may further include performing adsorption treatment on the microalgae grease obtained after each extraction by using an adsorbent. Through adsorption treatment, impurities such as pigment, protein, polysaccharide and the like in the microalgae grease can be removed, so that the EPA content in the microalgae grease is improved.
In the present invention, the adsorbent may be added directly to the microalgae lipid or may exist in the form of an adsorption column. Preferably, the adsorption treatment is performed in the form of an adsorption column. The step of performing the adsorption treatment using the adsorption column may include column loading, eluting, and collecting operations. When the adsorption column is a commercially available adsorption column, loading, elution and collection operations may be performed directly.
In the present invention, the type of the adsorbent is not particularly limited, and may be, for example, one or more of magnesium silicate, silica gel, activated carbon, diatomaceous earth, activated clay, and resin, and the adsorbents used for adsorbing the microalgae fat obtained after each extraction may be the same or different from each other.
In a preferred embodiment of the invention, the method further comprises: adsorption treatment is carried out on microalgae grease I by using an adsorbent I, wherein the adsorbent I is at least one selected from silica gel, diatomite and activated clay; adsorption treatment is carried out on microalgae grease II by using an adsorbent II, wherein the adsorbent II is selected from at least one of silica gel and resin; and (3) carrying out adsorption treatment on the microalgae grease III by using an adsorbent III, wherein the adsorbent III is at least one selected from activated carbon and magnesium silicate.
In a preferred embodiment of the invention, the method further comprises: 1) Adding a nonpolar organic solvent into microalgae biomass, performing first extraction, separating to obtain microalgae grease I and raffinate I, and then performing adsorption treatment on the microalgae grease I by using an adsorbent I;
2) Adding a polar organic solvent I into the raffinate I, performing second extraction, separating to obtain microalgae grease II and raffinate II, and then performing adsorption treatment on the microalgae grease II by using an adsorbent II;
3) Adding a polar organic solvent II into the raffinate II, performing third extraction, separating to obtain microalgae grease III and raffinate III, and then performing adsorption treatment on the microalgae grease III by using an adsorbent III;
wherein the dielectric constant of the polar organic solvent I is smaller than that of the polar organic solvent II; the adsorbent I is at least one selected from silica gel, diatomite and activated clay; the adsorbent II is at least one selected from silica gel and resin; the adsorbent III is at least one selected from activated carbon and magnesium silicate.
In a more preferred embodiment of the present invention, the adsorbent I is silica gel, the adsorbent II is silica gel, and the adsorbent III is activated carbon, and under such conditions, the removal amount of impurities such as pigments in the microalgae grease I, the microalgae grease II, and the microalgae grease III can be increased, thereby further increasing the content of EPA in the microalgae grease.
It will be appreciated that the method of the invention may also be used for extraction of microalgae oils enriched in other active substances, which may be microalgae pigments, monounsaturated fatty acids and other polyunsaturated fatty acids, etc.
In the present invention, the form of the microalgae biomass is not particularly limited, and may be any form containing microalgae cells, such as slurry, algae mud or algae powder. In the present invention, microalgae biomass of any form can be extracted by the above method to obtain microalgae oil, preferably, the microalgae biomass is algae powder, and in this preferred case, the extraction process can be directly performed without any treatment.
The method of the present invention is applicable to extraction of EPA-rich microalgae oil of different polarities from various microalgae, that is, the type of microalgae is not particularly limited, and microalgae having rich EPA content and oil content are preferable, and for example, at least one selected from nannochloropsis, diatom, yellow silk algae, flat algae, synechocystis and oocyst may be used. One skilled in the art can select a target algal species based on the target EPA or lipid content.
The extraction method provided by the invention can obtain EPA microalgae grease with different physicochemical properties and molecular structures so as to meet various living requirements. It is understood that the microalgae grease can be applied to human diets, livestock and poultry feeds and aquatic product feeds, and can be further processed to be used in health products, cosmetics or medicines.
In another aspect, the invention provides EPA-enriched microalgae grease with different polarities prepared by the method.
The present invention will be described in detail by examples. In the following examples and comparative examples:
the microalgae is Phaeodactylum tricornutum (Phaeodactrylum tricornutum GT) which is the own algae species of the national center for microalgae biotechnology investment, which is the national center for biotechnology investment.
The EPA content determination method comprises the following steps: quantitative analysis was performed using an Agilent gas chromatograph (7890B) using a Flame Ionization Detector (FID) with column DB-23 (Agilent, cat# 122-2361).
The method for measuring heavy metals comprises the following steps: qualitative and quantitative analysis was performed using an Agilent inductively coupled plasma Mass Spectrometry (ICP-MS 7700X).
The method for measuring the content of the microalgae grease comprises the following steps: the measurement was performed by a weighing method.
The silica gel is 200 mesh silica gel purchased from Qingdao ocean chemical Co.
The resin was 60-160 mesh resin available from Tianjin resin technologies Inc.
The diatomaceous earth was food grade diatomaceous earth purchased from atanan Jin Xuyuan new materials limited.
The activated carbon is food grade decolorized activated carbon purchased from Hebei Technophora limited.
The reagents and materials used in the following examples and comparative examples were all of conventional type unless otherwise specified.
In the following examples and comparative examples, five parallel experiments were performed for each experiment. The data obtained from the experiments were analyzed using spss, where the following data were all significantly different (i.e., p < 0.05) and are not shown in Table 1.
Example 1
The embodiment is used for explaining the extraction method of the microalgae grease
1) 200mg of Phaeodactylum tricornutum algae powder was weighed into a conical reaction tube.
2) First extraction: adding n-hexane according to the liquid-to-material ratio of 6mL/g, mixing uniformly by vortex, heating in a preheated water bath at 30 ℃, stirring at 150rpm, starting the first extraction, and starting timing. After 30min, centrifugation was carried out at 3000rpm for 5min at 4 ℃. The organic solvent layer containing microalgae grease I is sucked by a dropper, and collected by a brown sample bottle, and the raffinate I is extracted next time.
3) And (3) second extraction: and extracting raffinate I according to the same process as the first extraction, wherein the organic solvent is ethyl acetate. The organic solvent layer containing microalgae grease II is sucked by a dropper, collected by a brown sample bottle and the raffinate II is extracted next time.
4) And (3) third extraction: and extracting raffinate II according to the same process as the first extraction, wherein the organic solvent is ethanol. The organic solvent layer containing microalgae grease III is sucked by a dropper, and collected by a brown sample bottle, and the raffinate III is discarded.
5) And the organic solvent layer containing the microalgae grease I, the organic solvent layer containing the microalgae grease II and the organic solvent layer containing the microalgae grease III are respectively used for eliminating the organic solvent by a nitrogen blowing instrument, the eliminating temperature is 30 ℃, and the microalgae grease I, the microalgae grease II and the microalgae grease III are respectively obtained after the microalgae grease I, the microalgae grease II and the microalgae grease III are dried at room temperature in a vacuum drying oven to constant weight. The microalgae grease weight is calculated after weighing, and EPA content is measured, and the result is shown in A1 group in table 1.
6) The adsorption column I filled with the adsorbent I is used for carrying out adsorption treatment on the microalgae grease I to obtain a product I; adsorbing the microalgae grease II by using an adsorption column II obtained by filling an adsorbent II to obtain a product II; and (3) carrying out adsorption treatment on the microalgae grease III by using an adsorption column III obtained by filling an adsorbent III to obtain a product III.
Wherein the adsorbent I is silica gel, the adsorbent II is silica gel, and the adsorbent III is activated carbon.
And weighing the obtained products I, II and III to obtain the weights of the microalgae grease of the products I, II and III, and measuring the EPA content in the products I, II and III, wherein the results are shown in the T1 group in the table 1.
Example 2
The embodiment is used for explaining the extraction method of the microalgae grease
1) 200mg of Phaeodactylum tricornutum algae powder was weighed into a conical reaction tube.
2) First extraction: diethyl ether was added at a liquid-to-material ratio of 3mL/g, and after vortexing, the mixture was placed in a preheated water bath for heating at 25℃with stirring at 50rpm, and the first extraction was started and at the same time the timing was started. After 60min, centrifugation was performed at 5000rpm for 3min at 4 ℃. The organic solvent layer containing microalgae grease I is sucked by a dropper, and collected by a brown sample bottle, and the raffinate I is extracted next time.
3) And (3) second extraction: the raffinate I is extracted according to the same process as the first extraction, wherein the organic solvent is chloroform. The organic solvent layer containing microalgae grease II is sucked by a dropper, collected by a brown sample bottle and the raffinate II is extracted next time.
4) And (3) third extraction: and extracting raffinate II according to the same process as the first extraction, wherein the organic solvent is acetone. The organic solvent layer containing microalgae grease III is sucked by a dropper, and collected by a brown sample bottle, and the raffinate III is discarded.
5) The organic solvent layer containing microalgae grease I, the organic solvent layer containing microalgae grease II and the organic solvent layer containing microalgae grease III are respectively used for eliminating organic solvents by a nitrogen blowing instrument, the eliminating temperature is 30 ℃, and the microalgae grease I, the microalgae grease II and the microalgae grease III are respectively obtained after the vacuum drying oven is dried at room temperature. The microalgae grease weight is calculated after weighing, and EPA content is measured, and the result is shown in A2 group in table 1.
6) The adsorption column I filled with the adsorbent I is used for carrying out adsorption treatment on the microalgae grease I to obtain a product I; adsorbing the microalgae grease II by using an adsorption column II obtained by filling an adsorbent II to obtain a product II; and (3) carrying out adsorption treatment on the microalgae grease III by using an adsorption column III obtained by filling an adsorbent III to obtain a product III.
Wherein the adsorbent I is silica gel, the adsorbent II is silica gel, and the adsorbent III is activated carbon.
And weighing the obtained products I, II and III to obtain the weights of the microalgae grease of the products I, II and III, and measuring the EPA content in the products I, II and III, wherein the results are shown in the T2 group in the table 1.
Example 3
The embodiment is used for explaining the extraction method of the microalgae grease
1) 200mg of Phaeodactylum tricornutum algae powder was weighed into a conical reaction tube.
2) First extraction: adding n-hexane according to the liquid-material ratio of 10mL/g, mixing uniformly by vortex, heating in a preheated water bath at 40 ℃ and stirring at 300rpm, starting the first extraction, and starting timing. After 10min, centrifugation was carried out at 8000rpm for 2min at 4 ℃. The organic solvent layer containing microalgae grease I is sucked by a dropper, and collected by a brown sample bottle, and the raffinate I is extracted next time.
3) And (3) second extraction: the raffinate I is extracted according to the same process as the first extraction, wherein the organic solvent is chloroform. The organic solvent layer containing microalgae grease II is sucked by a dropper, collected by a brown sample bottle and the raffinate II is extracted next time.
4) And (3) third extraction: and extracting raffinate II according to the same process as the first extraction, wherein the organic solvent is methanol. The organic solvent layer containing microalgae grease III is sucked by a dropper, and collected by a brown sample bottle, and the raffinate III is discarded.
5) The organic solvent layer containing microalgae grease I, the organic solvent layer containing microalgae grease II and the organic solvent layer containing microalgae grease III are respectively used for eliminating organic solvents by a nitrogen blowing instrument, the eliminating temperature is 30 ℃, and the microalgae grease I, the microalgae grease II and the microalgae grease III are respectively obtained after the vacuum drying oven is dried at room temperature. The microalgae grease weight is calculated after weighing, and EPA content is measured, and the result is shown in A3 group in table 1.
6) The adsorption column I filled with the adsorbent I is used for carrying out adsorption treatment on the microalgae grease I to obtain a product I; adsorbing the microalgae grease II by using an adsorption column II obtained by filling an adsorbent II to obtain a product II; and (3) carrying out adsorption treatment on the microalgae grease III by using an adsorption column III obtained by filling an adsorbent III to obtain a product III.
Wherein the adsorbent I is silica gel, the adsorbent II is silica gel, and the adsorbent III is activated carbon.
The obtained products I, II and III were weighed to obtain the weights of microalgae grease of the products I, II and III, and EPA content was measured, and the results are shown in the T3 group in Table 1.
Example 4
The embodiment is used for explaining the preparation method of the microalgae grease
Microalgae grease was prepared according to the method of example 1, except that the adsorbent I was diatomaceous earth, the adsorbent II was resin, and the adsorbent III was magnesium silicate.
The weights of microalgae grease I, microalgae grease II and microalgae grease III obtained after the extraction step are weighed, and EPA content is measured, and the results are shown in A4 group in Table 1.
The microalgae grease weight of the product I, the product II and the product III obtained after the adsorption step is measured, and EPA content is measured, and the result is shown in a T4 group in Table 1.
Example 5
The embodiment is used for explaining the preparation method of the microalgae grease
Microalgae lipid preparation was performed as in example 1, except that the organic solvent used in the first extraction was diethyl ether, the organic solvent used in the second extraction was chloroform, and the organic solvent used in the third extraction was methanol.
The weights of microalgae grease I, microalgae grease II and microalgae grease III obtained after the extraction step are weighed, and EPA content is measured, and the results are shown in A5 group in Table 1.
The microalgae grease weight of the product I, the product II and the product III obtained after the adsorption step is measured, and EPA content is measured, and the result is shown in a T5 group in Table 1.
Comparative example 1
Comparative example preparation method of microalgae grease for reference
The microalgae lipid preparation was performed according to the method of example 1, except that the organic solvent used in the first extraction was ethanol, the organic solvent used in the second extraction was ethyl acetate, and the organic solvent used in the third extraction was n-hexane.
The weights of microalgae grease I, microalgae grease II and microalgae grease III obtained after the extraction step are weighed, and EPA content is measured, and the results are shown in a D1 group in Table 1.
The microalgae grease weight of the products I, II and III obtained after the adsorption step is measured, and EPA content is measured, and the results are shown in the dt1 group in Table 1.
Comparative example 2
Comparative example preparation method of microalgae grease for reference
The microalgae lipid preparation was performed according to the method of example 1, except that the organic solvent used in the first extraction was ethanol, the organic solvent used in the second extraction was ethanol, and the organic solvent used in the third extraction was ethanol. And (3) obtaining microalgae grease I, microalgae grease II and microalgae grease III.
The weights of microalgae grease I, microalgae grease II and microalgae grease III obtained after the extraction step are weighed, and EPA content is measured, and the results are shown in a D2 group in Table 1.
The microalgae grease weight of the products I, II and III obtained after the adsorption step is measured, and EPA content is measured, and the results are shown in the dt2 group in Table 1.
TABLE 1
The technical scheme of the invention is used for obtaining a plurality of microalgae grease with different physicochemical properties, the total amount of the microalgae grease and the total amount of EPA are relatively high, and the impurity removal rate of the obtained microalgae grease is higher, so that the higher EPA content is ensured, and the value can be further improved under the preferable condition.
The inventor finds that the organic solvent with low dielectric constant to high dielectric constant can realize good extraction effect, and when the order of the dielectric constants of the organic solvents is opposite, different EPA grease cannot be well separated according to the polarity. Further, as can be seen from the comparison of the data of example 1 and comparative example 1, the EPA content in the extracted oils and fats decreases when the dielectric constant of the organic solvent is changed from high to low.
In comparative example 2, when the organic solvents are the same solvent, i.e., the extraction method conventional in the art, the mixture of EPA lipids obtained by extraction cannot be specifically obtained as EPA glycolipids, EPA phospholipids and EPA neutral lipids. As can be seen from the data in table 1, in comparative example 2, the EPA content increase ratio in the 3 microalgae oils after adsorption treatment was lower than before adsorption treatment, indicating that the impurity removal rate was lower.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. The technical solution of the invention can be subjected to a plurality of simple variants within the scope of the technical idea of the invention. Including the various specific features being combined in any suitable manner. The various possible combinations of the invention are not described in detail in order to avoid unnecessary repetition. Such simple variations and combinations are likewise to be regarded as being within the scope of the present disclosure.
Claims (2)
1. A preparation method of EPA-enriched microalgae grease with different polarities is characterized by comprising the following steps: extracting microalgae biomass by an organic solvent for at least two times, and separating the extracted materials to obtain microalgae grease and raffinate after each extraction;
wherein, the 1+n-th organic solvent extraction takes raffinate obtained by separating the n-th organic solvent extraction as a raw material, and the dielectric constant of the organic solvent used in each extraction is sequentially increased;
wherein n is an integer not less than 1;
wherein the method further comprises:
1) Adding a nonpolar organic solvent into the microalgae biomass, performing first extraction, and separating to obtain microalgae grease I and raffinate I;
2) Adding a polar organic solvent I into the raffinate I, performing second extraction, and separating to obtain microalgae grease II and raffinate II;
3) Adding a polar organic solvent II into the raffinate II, performing third extraction, and separating to obtain microalgae grease III and raffinate III;
wherein the dielectric constant of the polar organic solvent I is smaller than that of the polar organic solvent II;
wherein the nonpolar organic solvent is n-hexane and/or diethyl ether;
wherein the polar organic solvent I is ethyl acetate and/or chloroform;
wherein the polar organic solvent II is at least one selected from ethanol, acetone and methanol;
wherein the method further comprises:
adsorption treatment is carried out on microalgae grease I by using an adsorbent I, wherein the adsorbent I is selected from at least one of silica gel and activated clay;
adsorption treatment is carried out on microalgae grease II by using an adsorbent II, wherein the adsorbent II is selected from silica gel;
adsorption treatment is carried out on microalgae grease III by using an adsorbent III, wherein the adsorbent III is selected from activated carbon;
wherein in the at least two organic solvent extractions, the liquid-to-material ratio of the organic solvent used for each extraction to the microalgae biomass is 3-10mL/g independently.
2. The EPA-rich microalgae lipid of different polarities prepared by the method of claim 1.
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