CN116355682A - Method for preparing hermetia illucens oil by taking fresh hermetia illucens larvae as raw materials - Google Patents
Method for preparing hermetia illucens oil by taking fresh hermetia illucens larvae as raw materials Download PDFInfo
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- CN116355682A CN116355682A CN202310296833.6A CN202310296833A CN116355682A CN 116355682 A CN116355682 A CN 116355682A CN 202310296833 A CN202310296833 A CN 202310296833A CN 116355682 A CN116355682 A CN 116355682A
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- 241000709785 Hermetia illucens Species 0.000 title claims abstract description 161
- 238000000034 method Methods 0.000 title claims abstract description 39
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- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 153
- 238000000605 extraction Methods 0.000 claims abstract description 108
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Images
Classifications
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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
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/02—Pretreatment
- C11B1/025—Pretreatment by enzymes or microorganisms, living or dead
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07K—PEPTIDES
- C07K1/00—General methods for the preparation of peptides, i.e. processes for the organic chemical preparation of peptides or proteins of any length
- C07K1/14—Extraction; Separation; Purification
- C07K1/145—Extraction; Separation; Purification by extraction or solubilisation
-
- 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
- C11B1/108—Production of fats or fatty oils from raw materials by extracting after-treatment, e.g. of miscellae
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P21/00—Preparation of peptides or proteins
- C12P21/06—Preparation of peptides or proteins produced by the hydrolysis of a peptide bond, e.g. hydrolysate products
Abstract
The invention discloses a method for preparing hermetia illucens oil by taking fresh hermetia illucens larvae as raw materials, which comprises the steps of adding citric acid into the fresh hermetia illucens larvae to obtain fresh worm slurry through crushing or adding citric acid solution into the fresh hermetia illucens larvae to obtain fresh worm slurry through treatment; adding an extraction solvent into the fresh insect slurry to leach the three-phase mixture, carrying out solid-liquid separation and oil-water separation on the three-phase mixture to obtain a mixed oil phase, removing the extraction solvent in the mixed oil phase, and removing residues and impurities to obtain the fresh hermetia illucens larva oil. The invention utilizes the citric acid to treat the fresh hermetia illucens larvae, and the acidic environment provided by the citric acid is beneficial to separating partial lipid from protein and sugar substances in biological cells, so that the active substances (such as protein) of the fresh hermetia illucens larvae can be protected, the protein quality can be improved, and the oil extraction rate (up to more than 90%) can be improved; the chelation of the citric acid reduces the catalytic activity of the enzyme, so that the brown stain participated by the enzyme is effectively inhibited, the color of the extracted grease is lighter, and the quality of the hermetia illucens oil is improved.
Description
Technical Field
The invention relates to a preparation method of hermetia illucens oil, in particular to a method for preparing the hermetia illucens oil by taking fresh hermetia illucens larvae as raw materials.
Background
Hermetia illucens (Black soldier fly) and hermetia illucens of the academic nameHermetia illucens L.) Is an insect of diptera and hermetia, can cultivate and promote the growth of the living, and can convert huge organic wastes into high-added-value biological substances. The hermetia illucens larva biomass is rich in protein, lipid and trace elements, contains 29.26% -45.10% of crude protein and 32.40% -54.88% of crude fat, and has high feeding value. The lipid is one of the main components in the black soldier fly larva, the saturated fatty acid is mainly lauric acid and palmitic acid, the content is 25.34% and 16.17% respectively, and the polyunsaturated fatty acid is mainly linoleic acid and reaches 27.25%. Therefore, the black soldier fly nutrient substances are utilized to carry out deep processing utilization on the black soldier flies, for example, the black soldier fly oil prepared by the black soldier flies has better economic and social benefits for reflecting the added value of the resource type insects.
The extraction of the hermetia illucens oil is divided into two main types of extraction of dried insects and fresh insects according to raw materials. The extraction of the dried insects adopts a plurality of extraction methods such as a squeezing method, an extraction method and the like, wherein the extraction method is widely applied due to lower cost and higher extraction rate, but has the defects of consuming a large amount of heat energy to dry the raw materials, consuming long time and destroying active nutrient substances (especially protein) of the insects.
At present, less researches are carried out on grease extraction by adopting fresh insects, and Chinese patent CN115109641A discloses a method for separating and extracting Tabanus proteins and grease, but an enzyme preparation is required to be added for enzymolysis in the extraction process of the method, so that the cost of the enzyme is high and the oil yield is low (only 78%). Weiliang Feng, xiong Huan and the like take fresh hermetia illucens larvae as raw materials, and adopt a homogenate method to prepare hermetia illucens oil: mixing the organic extraction solvent with the insect body, directly homogenizing at high speed for 1min, extracting, separating, and purifying to obtain hermetia illucens oil. The method is simple and low in energy consumption, but solvent vortex is easy to form when the solvent is directly homogenized at a high speed, the solvent is easy to volatilize, the risk coefficient is high, the requirement on production equipment is high, large-scale production is difficult to realize, and the oil extraction rate is only 75.92%.
Disclosure of Invention
The invention aims to provide a method for preparing black soldier fly oil by using fresh black soldier fly larvae as raw materials, which not only can protect bioactive substances (such as proteins) in the black soldier fly bodies so as to facilitate the finish processing of the proteins in the black soldier fly bodies, but also can improve the oil extraction rate (up to 95%) of the fresh black soldier fly larvae on the premise of ensuring the quality of the black soldier fly oil, is convenient for industrial production, and has better economic and social benefits.
In order to achieve the above purpose, the present invention may adopt the following technical scheme:
the method for preparing the hermetia illucens oil by taking fresh hermetia illucens larvae as raw materials comprises the following steps of:
s1, adding citric acid solids into the fresh hermetia illucens larvae and crushing to obtain fresh worm slurry or adding citric acid solution into the fresh hermetia illucens larvae to obtain fresh worm slurry, wherein the concentration of the citric acid solution is 3.0-6.0%, and the ratio of the fresh hermetia illucens larvae to the citric acid solution is 1g:1.0 ml-1 g:2.0ml;
s2, adding the treated fresh insect slurry into an extraction solvent, wherein the feed liquid ratio of the fresh insect slurry to the extraction solvent is more than or equal to 1 g/3 ml; leaching for 2-5 times at 30-70 ℃ to obtain a three-phase mixture of a solid phase, a water phase and a mixed oil phase;
s3, performing solid-liquid separation on the three-phase mixture obtained in the step S2, and then performing oil-water separation to obtain a mixed oil phase of the extraction solvent and the fresh hermetia illucens larva oil;
s4, removing the extraction solvent in the mixed oil phase to obtain a crude oil extract of the fresh hermetia illucens larva;
s5, removing residues and impurities from the crude extract of the fresh hermetia illucens larva oil to obtain the fresh hermetia illucens larva oil.
According to the method, the fresh hermetia illucens larvae are treated by using citric acid, and the acidic environment provided by the citric acid is beneficial to separating partial lipid from protein and sugar substances in biological cells in the subsequent leaching process, so that the oil extraction rate (the oil extraction rate is over 90 percent and even up to 95 percent) is improved, the protein in the crude protein of the fresh hermetia illucens larvae is protected, and the protein quality is improved; citric acid also chelates Cu 2＋ 、Mg 2＋ 、Fe 2＋ Polyvalent metal ions, which are usually acting prosthetic groups of enzymes, and chelation of citric acid can effectively reduce catalytic activity of the enzymes, further effectively inhibit browning participated by the enzymes, make extracted grease light in color and improve quality of black soldier fly oil. In addition, the invention further adopts the high shearing force and high-strength centrifugal action provided by high-pressure homogenization to fully crush the cells of the fresh soldier fly larvae, is beneficial to release of fat, increases the contact area of the fat and the solvent, and further improves the extraction rate of the grease.
In a more preferred embodiment of the present invention, in the step S1, the step of adding citric acid solution to the hermetia illucens larvae to obtain the fresh insect slurry specifically comprises: adding citric acid solution into the fresh hermetia illucens larva according to the feed-liquid ratio of 1g to 1.0ml to 1g to 2.0ml, and homogenizing under high pressure at room temperature, wherein the high-pressure homogenizing rotating speed is more than or equal to 8000r/min, so as to obtain fresh worm slurry. The high shear force and high-strength centrifugal effect provided by high-pressure homogenization can fully crush cells of the hermetia illucens fresh larvae, is favorable for releasing fat, increases the contact area of the fat and the solvent, and further improves the extraction rate of the grease.
In a preferred embodiment of the present invention, the extraction solvent used in the step S2 includes any one or a combination of two or more of n-hexane, vegetable oil extraction solvent, petroleum ether or isopropyl ether.
More preferably, the extracting solvent adopted in the step S2 is vegetable oil extracting solvent or petroleum ether with the boiling range of 60-90 ℃, and the feed liquid ratio of the fresh insect slurry to the extracting solvent is 1g:3.5 ml-1 g:7.0ml. More preferably, the feed to liquid ratio of the fresh insect slurry to the extraction solvent is 1g:5.0ml.
In a preferred embodiment of the present invention, the low temperature leaching in step S2 is performed at a temperature of 30 ℃ to 70 ℃ for a leaching time of 0.5h to 2.0h. More preferably, the leaching temperature is controlled between 40 and 60 ℃.
In a preferred embodiment of the present invention, in the step S4, the removing the extraction solvent in the mixed oil phase includes: and (3) evaporating and recycling the organic solvent in the oil phase at the temperature of 45-65 ℃ and under the pressure of minus 0.045MPa to minus 0.095 MPa. In actual production, the extraction solvent in the oil phase can be removed by a recovery pot, a thin film evaporator or a molecular distillation technology to obtain crude oil of the fresh hermetia illucens larva.
Compared with the prior art, the method has the advantages that the fresh hermetia illucens larvae are treated by using the citric acid, and the acidic environment provided by the citric acid is beneficial to separating partial lipid, protein and saccharide substances in biological cells in the subsequent leaching process, so that the oil extraction rate is improved, the protein in the crude protein of the fresh hermetia illucens larvae is protected, and the protein quality is improved; citric acid also chelates Cu 2＋ 、Mg 2＋ 、Fe 2＋ Polyvalent metal ions, which are usually acting prosthetic groups of enzymes, and chelation of citric acid can effectively reduce catalytic activity of the enzymes, further effectively inhibit browning participated by the enzymes, make extracted grease light in color and improve quality of black soldier fly oil. In addition, the invention further adopts the high shearing force and high-strength centrifugal action provided by high-pressure homogenization to fully crush the cells of the fresh soldier fly larvae, is beneficial to release of fat, increases the contact area of the fat and the solvent, and further improves the extraction rate of the grease.
According to the invention, the fresh hermetia illucens larva is used as a raw material for grease extraction, fresh worm slurry is obtained by reasonably treating the fresh hermetia illucens larva, and the extraction process parameters of the fresh worm slurry are optimized, so that the extraction rate of grease in the fresh hermetia illucens larva is improved to more than 90 percent (even up to 95 percent), the technical problem of low grease extraction rate of the existing fresh hermetia illucens larva is overcome, and the obtained hermetia illucens oil has the advantages of excellent quality, low peroxide value, light color and light peculiar smell, and is beneficial to the preparation of deep-processed products such as later-stage microcapsule powder; in addition, the extraction process is mild, the extraction rate of the grease is high, and the industrialized mass production can be realized; moreover, the invention can protect the active substances such as the insect protein from being damaged on the basis of ensuring the oil product, is beneficial to the deep processing of the insect protein, and has important significance for improving the quality of the deep processed product of the insect protein.
The oil extraction process is safe and reasonable, has low requirements on equipment, can meet the production requirements by conventional equipment, and is beneficial to large-scale production; compared with the extraction of the dried insects, the larva drying step is omitted, so that the production cost is reduced, and the inactivation of natural active ingredients caused by the larva drying and extraction can be avoided. In addition, in actual production, the organic solvent recovered after each leaching can be reused, so that the production cost is reduced.
Drawings
FIG. 1 is a process scheme of the preparation method of the present invention.
FIG. 2 shows the extraction of the fresh hermetia illucens larva oil by using the vegetable oil extraction solvent as the extraction solvent in example 4.
FIG. 3 shows the extraction of the fresh hermetia illucens larva oil from example 2 using petroleum ether as the extraction solvent.
FIG. 4 is a diagram showing the state of the treated oil of the fresh hermetia illucens larva in example 2 after degumming and alkali refining drying.
Detailed Description
The raw materials of the fresh hermetia illucens larvae used in the invention are commercial 5-year-old fresh larvae (purchased from Tabanus source biotechnology limited company in Henan) or frozen fresh larvae, and the larvae are ensured to be clean and not brown. It should be noted that the petroleum ether used in the examples below refers to petroleum ether having a boiling range of 60 to 90℃unless otherwise specified.
The invention provides a method for preparing black soldier fly oil by taking fresh black soldier fly larvae as raw materials, which comprises the steps of adding citric acid into the fresh black soldier fly larvae to directly crush to obtain fresh worm slurry, or adding citric acid solution into the fresh black soldier fly larvae to carry out homogenate crushing, so that the extraction rate of the fresh black soldier fly larvae oil can be ensured, the quality of the fresh black soldier fly larvae oil can be ensured, the subsequent deep processing of microcapsule powder and the like can be facilitated, the protein of the fresh black soldier fly larvae can be protected from being damaged, the quality of the fresh black soldier fly larvae protein can be improved, and the deep processing of the fresh black soldier fly larvae protein can be facilitated.
The method for preparing the hermetia illucens oil by taking the fresh hermetia illucens larvae as the raw material has the process route shown in figure 1, and comprises the following specific steps:
s1, adding citric acid solution (prepared from soft water and anhydrous citric acid) into purchased clean and non-browned 5-year-old fresh hermetia illucens larvae according to the proportion of 1g to 1ml to 1g to 2ml, homogenizing and crushing to obtain fresh hermetia illucens larva slurry; the mass concentration of the citric acid solution is controlled to be 3.0% -6.0% (preferably 3.5% -5.5%);
or, adding anhydrous citric acid (namely, adding 50g of citric acid into 1000g of fresh hermetia illucens larvae) into the fresh hermetia illucens larvae according to the mass ratio of 1g to 0.05g, and then directly crushing to obtain fresh hermetia illucens larva slurry;
s2, adding the treated fresh insect slurry into an extraction solvent, and extracting for 2-5 times at a low temperature of 20-70 ℃ for 45-120 min each time to obtain a three-phase mixture of insect residues, a water phase and a mixed oil solution;
wherein the extracting solvent is n-hexane, vegetable oil extracting solvent, petroleum ether or isopropyl ether, the extracting solvent is preferably vegetable oil extracting solvent or petroleum ether, and the feed liquid ratio of the fresh insect slurry to the extracting solvent is 1g:3 ml-1 g:7ml (preferably 1g:3.5 ml-1 g:6.0 ml); the leaching time is 0.5 to 2.0 hours, preferably 40 to 90 minutes, more preferably 60 minutes; the leaching temperature is preferably 30-65 ℃, more preferably 40-50 ℃; the leaching times are preferably 2-3 times, more preferably 2 times;
s3, centrifugally separating the three-phase mixture obtained in the step S2, and then separating an oil phase and a water phase by utilizing an oil-water separator to obtain a mixed oil phase of the extraction solvent and the grease;
s4, removing and recovering the leaching solvent in the mixed oil phase at the temperature of 45-65 ℃ and the pressure of minus 0.045MPa to minus 0.095MPa (the recovered leaching solvent can be reused, and the production cost is reduced), so as to obtain the crude extract of the fresh black soldier fly larva oil; wherein, when the leaching solvent is removed, a recovery pot, a thin film evaporator, a molecular distillation technology, or the like can be adopted;
s5, removing residues and impurities from the crude oil extract of the fresh hermetia illucens to obtain a finished product of the fresh hermetia illucens larva oil;
the nitrogen is preferably filled to remove residues during actual residue removal, the residue removal temperature is controlled at 60-65 ℃, and the nitrogen is utilized to remove residual extraction solvent in the crude extract of the fresh black soldier fly larva oil; removing impurities with a bag filter.
The present invention will be described in more detail by way of specific examples below to facilitate understanding by those skilled in the art. It should be noted that, in the following examples, the oil extraction rate of the hermetia illucens larvae was calculated by a conventional method, and the oil extraction rate was calculated as follows:
wherein, the water content of the fresh insects is measured by adopting a direct drying method in GB 5009.3-2016; the crude fat content of the dried insects is obtained by taking the dried fresh insects as raw materials and measuring the raw materials by referring to a Soxhlet extraction method in GB 5009.6-2016;
when the oil extraction method is used for calculating, the weight of the fresh insects, the crude fat content of the dried insects and the water content of the fresh insects are known parameters, and the oil extraction rate can be calculated according to the weight of the extracted fresh hermetia illucens larva oil finished product.
Example 1 this example uses a direct crushing method of citric acid to treat the larvae of hermetia illucens
S1, adding 10g of anhydrous citric acid into 200g of 5-year-old fresh hermetia illucens larvae and crushing to obtain fresh hermetia illucens larva slurry (hereinafter referred to as fresh worm slurry);
s2, adding petroleum ether into the treated fresh insect slurry, wherein the ratio of the fresh insect slurry to the petroleum ether is 1g to 5ml, and leaching for 2 times at 50 ℃ for 60 minutes each time;
s3, carrying out centrifugal separation on the three-phase mixture obtained in the step S2 to obtain a water phase, a solid phase and a mixed oil phase, and separating the oil phase and the water phase by using an oil-water separator to obtain a mixed oil phase of the extraction solvent and the grease;
s4, removing the leaching solvent in the mixed oil phase by using a recovery pot at the temperature of 45-65 ℃ and under the pressure of minus 0.045MPa to minus 0.095MPa, and recovering (the recovered leaching solvent can be reused) to obtain the crude oil extract of the fresh black soldier fly larvae;
s5, nitrogen is filled into the crude oil extract of the fresh hermetia illucens, the residue removal temperature is controlled at 60-65 ℃, nitrogen is utilized to take away the residual extraction solvent in the crude oil extract of the fresh hermetia illucens, and a bag filter is utilized to filter after residue removal.
The oil extraction rate of the fresh hermetia illucens larvae in the embodiment is calculated to be 90.14%.
In the embodiment, the fresh hermetia illucens larvae are treated by the citric acid solution to obtain fresh hermetia illucens larva slurry, and the acidic environment provided by the citric acid solution is beneficial to separating partial lipid, protein and saccharide substances in biological cells in the subsequent leaching process, so that the oil extraction rate is improved, the protein in crude proteins of the fresh hermetia illucens larvae is protected, and the protein quality is improved; citric acid also chelates Cu 2＋ 、Mg 2＋ 、Fe 2＋ Polyvalent metal ions, which are usually acting prosthetic groups of enzymes, and chelation of citric acid can effectively reduce catalytic activity of the enzymes, further effectively inhibit browning participated by the enzymes, make extracted grease light in color and improve quality of black soldier fly oil.
EXAMPLE 2 this example uses citric acid solution+high pressure homogenization treatment of the larvae of hermetia illucens
S1, adding 5% citric acid solution into 2000g of 5-year-old fresh hermetia illucens larvae according to the ratio of 1g to 1ml, and homogenizing under high pressure at room temperature, wherein the high-pressure homogenizing speed is 10000r/min, so as to obtain fresh hermetia illucens larva slurry (abbreviated as fresh worm slurry);
s2, adding petroleum ether into the treated fresh insect slurry, wherein the ratio of the fresh insect slurry to the petroleum ether is 1g to 5ml, and leaching for 2 times at 50 ℃ for 60 minutes each time;
s3, centrifugally separating the three-phase mixture obtained in the step S2 to obtain a water phase, a solid phase and a mixed oil phase containing petroleum ether, and performing oil-water separation on the water phase and the mixed oil phase by adopting an oil-water separator to obtain a mixed oil phase;
s4, removing the leaching solvent in the mixed oil phase by using a recovery pot at the temperature of 45-65 ℃ and under the pressure of minus 0.045MPa to minus 0.095MPa, and recovering (the recovered leaching solvent can be reused) to obtain the crude oil extract of the fresh black soldier fly larvae;
s5, nitrogen is filled into the crude oil extract of the fresh black soldier fly larvae to remove residues, the residue removing temperature is controlled at 60-65 ℃, nitrogen is utilized to take away residual extraction solvent in the crude oil extract of the fresh black soldier fly larvae, and a centrifugal filter is utilized to remove impurities after the residues are removed, so as to obtain 168.74g of finished product of the fresh black soldier fly larvae oil.
Calculated, the extraction rate of the fresh hermetia illucens oil in the embodiment is 95.35%.
Compared with the embodiment 1, in the embodiment, the citric acid solution and the high-pressure homogenization are adopted to treat the fresh hermetia illucens larvae, and the shearing force provided by the high-pressure homogenization and the high-strength centrifugation can fully crush biological cells of the fresh hermetia illucens larvae, so that the grease extraction rate of the fresh hermetia illucens larvae is further improved.
Example 3 this example uses different concentrations of lemon solution to treat the larvae of hermetia illucens
This example differs from example 2 in the concentration of aqueous citric acid solution. In the embodiment, the fresh black soldier fly larvae are taken as raw materials, the fresh black soldier fly larvae are divided into five groups, citric acid solutions with the concentrations of 3.5%, 4.0%, 4.5%, 5.0% and 5.5% are respectively added to the fresh black soldier fly larvae according to the ratio of 1g to 1ml, and then high-pressure homogenization is carried out, wherein the grease extraction rates of the five groups of fresh black soldier fly larvae are shown in table 1.
TABLE 1
The table shows that when the mass concentration of the citric acid solution is within the range of 3.5% -5.5%, the oil extraction rate of the fresh hermetia illucens larvae can reach more than 90%, and the oil extraction rate of the fresh hermetia illucens larvae is gradually increased and then kept balanced along with the increase of the concentration. Therefore, the concentration of the citric acid solution in the present invention is controlled within a range of 3.5% to 5.5%, preferably 4.0% to 5.0%, and most preferably 5% citric acid solution.
EXAMPLE 4 this example used vegetable oil extraction solvent to extract fresh hermetia illucens larva slurry
This embodiment differs from embodiment 2 in that: in the embodiment, the vegetable oil extraction solvent is used as an extraction solvent, and the specific contents are as follows: adding vegetable oil extraction solvent into the treated fresh insect slurry according to the feed liquid ratio of 1g to 5ml, and leaching for 60min at 50 ℃ for 2 times.
In this example, the usage amount of the fresh hermetia illucens larva is 2000g, and 167.43g of fresh hermetia illucens larva oil product can be finally obtained, and the product oil is clear and transparent and has the peculiar taste of the hermetia illucens, and specifically shown in fig. 2.
The extraction rate of the fresh hermetia illucens oil in the embodiment is 91.82 percent.
Example 5 this example examined the effect of feed to liquid ratio of fresh insect slurry to petroleum ether on extraction yield
This embodiment differs from embodiment 2 only in that: in the embodiment, the ratio of the petroleum ether to the fresh insect slurry is 1g to 3.5ml, 1g to 4ml and 1g to 6ml, and the extraction rates of the grease corresponding to different ratios of the materials are shown in Table 2.
TABLE 2
As shown in Table 2, when the feed liquid ratio of the fresh insect slurry to the petroleum ether is not less than 1g:3.5ml, the oil extraction rate is not less than 90%, which means that the feed liquid ratio of the fresh insect slurry to the petroleum ether is preferably controlled to be not less than 1g:3.5 ml. In addition, as the amount of petroleum ether increases, the oil extraction rate gradually increases and then gradually reaches equilibrium. Therefore, in actual production, in view of the safety production and economic principles, the feed liquid ratio of the fresh insect slurry to the petroleum ether is preferably 1g:4ml to 1g:6ml, wherein the ratio is optimally 1g:5 ml.
EXAMPLE 6 this example uses leaching temperature as a variable
This embodiment differs from embodiment 2 only in that: the extraction temperatures in step S2 of this example were 30℃and 40℃and 60℃and 65℃in this order, and the extraction rates of the oils corresponding to the different extraction temperatures are shown in Table 3.
TABLE 3 Table 3
As is clear from Table 3, the extraction rate of the oil and fat was more than 90% at the extraction temperature of 30℃to 65 ℃. Wherein, with the rising of the leaching temperature, the grease extraction rate is increased and then reduced, and the grease extraction rate reaches the maximum at 50 ℃. Thus, in actual production, the leaching temperature of the fresh insect slurry is preferably 40℃to 60℃and more preferably 50 ℃.
EXAMPLE 7 this example considers the leaching time as a variable
This embodiment differs from embodiment 2 only in that: the extraction time in step S2 of this example was 45min, 90min and 120min in this order, and the extraction rates of the oils corresponding to the different extraction temperatures are shown in table 4.
TABLE 4 Table 4
As shown in Table 4, the extraction rate of the oil was more than 90% at the extraction temperature of 45 to 120 min. Wherein, as the leaching time increases, the grease extraction rate increases and then decreases, and the grease extraction rate reaches the maximum when the single leaching time is 60min. In actual production, the leaching time of the fresh insect slurry in the invention is controlled within 90min, preferably controlled within 60min.
Example 8 this example considers the number of leaches as a variable
This embodiment differs from embodiment 2 only in that: the extraction temperatures in step S2 of this example were 3 times, 4 times and 5 times in this order, and the extraction rates of the oils corresponding to the different extraction temperatures are shown in table 5.
TABLE 5
As shown in Table 4, when the number of times of extraction was not less than 2, the extraction rate of oil corresponding to the number of times of extraction was not less than 94%, but the extraction rate of oil was not changed substantially with the increase of the number of times of extraction. Therefore, the leaching times are preferably 2 times in actual production, the consumption of the extracting solvent is reduced as much as possible, the oil extracting time is shortened, and the production cost of enterprises is reduced.
From examples 1-8, the invention uses citric acid or 3.5% -5% citric acid solution to treat the fresh hermetia illucens larva to obtain fresh hermetia illucens larva slurry,the acidic environment provided by the citric acid is beneficial to separating partial lipid, protein and saccharide substances in biological cells in the subsequent leaching process, so that the oil extraction rate is improved, the protein in the crude protein of the fresh hermetia illucens larva is protected, and the protein quality is improved; citric acid also chelates Cu 2＋ 、Mg 2＋ 、Fe 2＋ Polyvalent metal ions, which are usually acting prosthetic groups of enzymes, and chelation of citric acid can effectively reduce catalytic activity of the enzymes, further effectively inhibit browning participated by the enzymes, make extracted grease light in color and improve quality of black soldier fly oil. In addition, the shearing force and the high-strength centrifugal action provided by the high-pressure homogenization can fully crush biological cells of the fresh black soldier fly larvae, so that the oil extraction rate of the fresh black soldier fly larvae is further improved.
As can be seen from examples 2-8, the extraction rate of the oil from the fresh hermetia illucens larvae in the invention is above 90%, even as high as 95% (in example 2). The invention sequentially carries out conventional degumming, alkali refining deacidification and dehydration drying treatment on the hermetia illucens oil in the embodiment 2 to obtain fresh hermetia illucens alkali refined oil; the finished black soldier fly oil obtained in example 2 and the fresh black soldier fly alkali refined oil were subjected to physicochemical analysis, the physicochemical indexes are shown in table 6, and the fatty acid composition and content (analyzed by gas chromatography-mass spectrometry (GC-MS)) of the black soldier fly oil are shown in table 7.
TABLE 6 physicochemical index of fresh hermetia illucens larva oil and alkali-refined liquid thereof
From table 6, after degumming and deacidification drying treatment, the water content, volatile matter, acid value, peroxide value and solvent residue in the fresh black soldier fly larva oil are obviously reduced, and the oil color is transparent yellow brown (see fig. 3) and transparent dark yellow (see fig. 4) before and after refining, so that the oil has better quality, and the oil has low odor when being used for preparing microcapsule powder of the black soldier fly larva oil, and the quality of the microcapsule powder is improved.
TABLE 7 fatty acid composition of fresh hermetia illucens larva oil and fresh hermetia illucens alkali refined oil
As is clear from Table 7, the main saturated fatty acids in the black soldier fly larva oil were lauric acid (C12:0), palmitic acid (C16:0), myristic acid (C14:0) and stearic acid (C18:0); the monounsaturated fatty acid is mainly oleic acid (C18:1) and then palmitoleic acid (C16:1); polyunsaturated fatty acids are predominantly linoleic acid (C18:2);
after degumming and alkali refining deacidification drying treatment of the fresh hermetia illucens larva oil, the fatty acid content in the oil is increased from the original 53.61% to 83.94%, the lauric acid content in the oil is up to 29.97%, and the total content of unsaturated fatty acids (including oleic acid, linoleic acid and alpha-linolenic acid) is up to 35.59%, which indicates that the oil extraction process can effectively ensure the quality of refined oil.
The above-described embodiments are only preferred embodiments of the present invention, but are not intended to limit the present invention. Various changes and modifications may be made by one of ordinary skill in the pertinent art without departing from the spirit and scope of the present invention. Therefore, all the technical schemes obtained by adopting the equivalent substitution or equivalent transformation are within the protection scope of the invention.
Claims (8)
1. A method for preparing hermetia illucens oil by taking fresh hermetia illucens larvae as raw materials is characterized by comprising the following steps of: comprising the following steps:
s1, adding citric acid solids into the fresh hermetia illucens larvae and crushing to obtain fresh worm slurry or adding citric acid solution into the fresh hermetia illucens larvae to obtain fresh worm slurry, wherein the concentration of the citric acid solution is 3.0-6.0%, and the ratio of the fresh hermetia illucens larvae to the citric acid solution is 1g:1.0 ml-1 g:2.0ml;
s2, adding the treated fresh insect slurry into an extraction solvent, wherein the feed liquid ratio of the fresh insect slurry to the extraction solvent is more than or equal to 1 g/3 ml; leaching for 2-5 times at 30-70 ℃ to obtain a three-phase mixture of a solid phase, a water phase and a mixed oil phase;
s3, performing solid-liquid separation on the three-phase mixture obtained in the step S2, and then performing oil-water separation to obtain a mixed oil phase of the extraction solvent and the fresh hermetia illucens larva oil;
s4, removing the extraction solvent in the mixed oil phase to obtain a crude oil extract of the fresh hermetia illucens larva;
s5, removing residues and impurities from the crude extract of the fresh hermetia illucens larva oil to obtain the fresh hermetia illucens larva oil.
2. The method for preparing the hermetia illucens oil by taking fresh hermetia illucens larvae as raw materials, according to claim 1, wherein the method comprises the following steps of: in the step S1, adding citric acid solution into the fresh hermetia illucens larvae to obtain fresh insect slurry specifically comprises the following steps: adding citric acid solution into the fresh hermetia illucens larva according to the feed-liquid ratio of 1g to 1.0ml to 1g to 2.0ml, and homogenizing under high pressure at room temperature, wherein the high-pressure homogenizing rotating speed is more than or equal to 8000r/min, so as to obtain fresh worm slurry.
3. The method for preparing the hermetia illucens oil by taking fresh hermetia illucens larvae as raw materials, according to claim 1, wherein the method comprises the following steps of: the extraction solvent used in the step S2 comprises any one or more than two of normal hexane, vegetable oil extraction solvent, petroleum ether or isopropyl ether.
4. The method for preparing the hermetia illucens oil by taking fresh hermetia illucens larvae as raw materials, according to claim 2, wherein the method comprises the following steps of: the extraction solvent adopted in the step S2 is vegetable oil extraction solvent or petroleum ether with the boiling range of 60-90 ℃, and the feed liquid ratio of the fresh insect slurry to the extraction solvent is 1g:3.5 ml-1 g:7.0ml.
5. The method for preparing the hermetia illucens oil by taking fresh hermetia illucens larvae as raw materials, according to claim 1, wherein the method comprises the following steps of: the leaching temperature in the step S2 is 30-65 ℃, and the leaching time is 0.5-1.5 h each time.
6. The method for preparing the hermetia illucens oil by taking fresh hermetia illucens larvae as raw materials, according to claim 1, wherein the method comprises the following steps of: in the step S4, the removing the extraction solvent in the mixed oil phase includes the following steps: and (3) evaporating and recycling the extraction solvent in the oil phase at the temperature of 45-65 ℃ and under the pressure of minus 0.045MPa to minus 0.095 MPa.
7. The method for preparing the hermetia illucens oil by taking fresh hermetia illucens larvae as raw materials, according to claim 1, wherein the method comprises the following steps of: in the step S1, the concentration of the citric acid solution is 3.5% -5.5%.
8. The method for preparing the hermetia illucens oil by taking fresh hermetia illucens larvae as raw materials, according to claim 1, wherein the method comprises the following steps of: in the step S5, the residue removal temperature of the crude oil extract of the fresh hermetia illucens larva is 60-65 ℃.
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