CN112143763A - Method for extracting refined alligator oil - Google Patents
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- CN112143763A CN112143763A CN202011124782.1A CN202011124782A CN112143763A CN 112143763 A CN112143763 A CN 112143763A CN 202011124782 A CN202011124782 A CN 202011124782A CN 112143763 A CN112143763 A CN 112143763A
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- 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
- C12P7/00—Preparation of oxygen-containing organic compounds
- C12P7/64—Fats; Fatty oils; Ester-type waxes; Higher fatty acids, i.e. having at least seven carbon atoms in an unbroken chain bound to a carboxyl group; Oxidised oils or fats
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- 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
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- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
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- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
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- 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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- 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
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Abstract
The invention discloses a method for extracting refined alligator oil. The invention relates to a method for extracting refined alligator oil, which comprises the following steps: (1) pretreating crocodile oil adipose tissues: mixing crocodile fat and water in proportion and chopping into paste; (2) ultra-high pressure auxiliary enzymolysis: placing minced alligator fat in an ultrahigh pressure container, extracting alligator oil by using an ultrahigh pressure auxiliary complex enzymolysis method, then boosting pressure, inactivating enzyme, and separating meat residue, oil and water out-of-phase from enzymolysis liquid to obtain crude alligator oil; (3) decoloring and deodorizing: removing fishy smell of the crocodile oil crude product obtained in the step (2) by adopting a steam distillation method, performing oil-water separation to obtain crude oil, and adding activated carbon and carclazyte into the crude oil to decolor and remove fishy smell; (4) removing impurities and bacteria: removing foreign matters in the crude oil obtained in the step (3) and sterilizing to obtain the essential oil. The method has high enzymolysis efficiency, retains more active ingredients and flavor substances, and effectively removes fishy smell.
Description
Technical Field
The invention relates to the technical field of animal fat extraction and refining, in particular to a method for extracting and refining alligator oil.
Background
At present, domestic alligator oil is used as a cosmetic raw material, and two problems are the greatest in the aspect of refining, namely, the extraction efficiency is low; secondly, active ingredients such as unsaturated fatty acid and the like cannot be reserved; and thirdly, the fishy smell of the alligator oil is difficult to remove. The traditional method for preparing the alligator oil mainly adopts a high-temperature cooking method, the efficiency is low, the prepared alligator oil is dark yellow, has very heavy alligator fishy smell, has rancid smell after oxidation, is poor in stability and easy to oxidize, loses a plurality of active ingredients in the high-temperature process, cannot be accepted by consumers, and limits the wide application of the alligator oil in skin care.
Disclosure of Invention
The invention aims to provide a method for extracting and refining alligator oil, which has high enzymolysis efficiency, retains more active ingredients and flavor substances and effectively removes fishy smell, aiming at the defects in the prior art.
The invention relates to a method for extracting refined alligator oil, which comprises the following steps:
(1) pretreating crocodile oil adipose tissues: mixing crocodile fat and water in proportion and chopping into paste;
(2) ultra-high pressure auxiliary enzymolysis: placing minced alligator fat in an ultrahigh pressure container, extracting alligator oil by using an ultrahigh pressure auxiliary complex enzymolysis method, then boosting pressure, inactivating enzyme, and separating meat residue, oil and water out-of-phase from enzymolysis liquid to obtain crude alligator oil;
(3) decoloring and deodorizing: removing fishy smell of the crocodile oil crude product obtained in the step (2) by adopting a steam distillation method, performing oil-water separation to obtain crude oil, and adding activated carbon and carclazyte into the crude oil to decolor and remove fishy smell;
(4) removing impurities and bacteria: removing foreign matters in the crude oil obtained in the step (3) and sterilizing to obtain the essential oil.
Further, the specific steps of the step (3) are as follows: introducing steam into the crude alligator oil obtained in the step (2) by using a steam generator for 20-50min, and then carrying out oil-water separation; then adding a certain amount of activated carbon and argil, preserving the heat for 20-40min, and filtering; adding argil, keeping the temperature for 20-40min, centrifuging, filtering and taking the supernatant; adding active carbon and clay, maintaining the temperature for 20-40min, centrifuging, filtering, and collecting supernatant.
Further, in the step (2): the steam distillation method conditions are that the steam flow rate is 50-70m/s, the rotating speed is 100-200r/min, and the time is 20-50 min.
Further, the adding amount of the first activated carbon is 1-3% of the mass of the crude oil, the adding amount of the clay is 1-3% of the mass of the crude oil, the total adding amount of the second activated carbon and the clay is 1-3% of the mass of the crude oil, the temperature is 50-65 ℃, the centrifugation condition is 12000rpm, and the centrifugation condition is 15 min.
Further, the mass ratio of the activated carbon to the clay is 1: 1.
Further, in the step (1): the ratio of crocodile fat to water is between 1:0.5 and 1: 2.
Further, the conditions of the ultrahigh pressure auxiliary enzymolysis in the step (2) are 150-.
Further, after the enzymolysis in the step (2) is finished, the conditions of enzyme inactivation and inactivation are 450-600MPa and 15-30 min.
Further, in the step (4), the crude oil obtained in the step (3) is filtered by an organic membrane for removing impurities and bacteria.
Further, the organic membrane is a 0.22 μm pore size organic membrane.
The invention relates to a method for extracting and refining alligator oil, which adopts an ultrahigh pressure auxiliary composite enzymolysis method, and utilizes pressurization to reserve unsaturated fatty acids such as EPA, DHA and the like and other a large amount of active ingredients in grease, and further adopts lipase and keratinase to realize composite enzymolysis with high efficiency, wherein the extraction rate can reach 76-80 percent, and the efficiency can be effectively improved; the method has the advantages that the steam distillation method is combined with the activated carbon, the argil and the organic membrane filtration technology in the refining process, fishy smell can be effectively removed, the obtained essential oil as a cosmetic raw material has the advantages of high purity and good quality, and the essential oil is easy to accept by consumers, wide in market application and good in prospect.
Drawings
FIG. 1 chromatogram of the product obtained in example 1;
FIG. 2 is a chromatogram of the product obtained in example 2.
Detailed Description
The following are specific embodiments of the present invention and the accompanying drawings, which further describe the technical solutions of the present invention, but the present invention is not limited to these embodiments.
Example 1
(1) Pretreating crocodile oil adipose tissues: mixing crocodile fat and water according to a ratio of 1:1, and chopping into paste;
(2) ultra-high pressure auxiliary enzymolysis: placing the mixed solution in an ultrahigh pressure container, extracting the alligator oil by an ultrahigh pressure auxiliary enzymolysis method under the conditions of 200MPa, 60 ℃ and 4 hours, wherein the selected enzyme is a compound enzyme (keratinase: lipase: 1), after the enzymolysis is finished, boosting pressure, inactivating the enzyme and inactivating the enzyme for 25 minutes under the conditions of 500MPa, and separating meat residue, oil and water out-of-phase from the enzymolysis solution to obtain a crude product of the alligator oil;
(3) decoloring and deodorizing: introducing steam into the crude oil for 30min by using a steam generator, wherein the steam flow rate is 60m/s, the rotation speed is 150r/min, condensing, vacuumizing and removing fishy smell, and then performing oil-water separation; adding activated carbon and clay into the crude oil for decolorization and deodorization, and specifically comprising the following steps: adding 2% active carbon, keeping the temperature for 30min, and filtering; adding 2% of argil, keeping the temperature for 30min, centrifuging, filtering and taking supernatant; simultaneously adding 2% of active carbon and argil (1:1), keeping the temperature for 30min, centrifuging (12000rpm, 15min), filtering and taking the supernatant;
(4) removing impurities and bacteria: adopting organic membrane (pore diameter of 0.22 μm) filtration method to effectively remove foreign matters in refining process and sterilize to obtain essential oil.
The results of this example are: by adopting an ultrahigh pressure auxiliary composite enzymolysis method and combining a steam distillation method, the enzymolysis efficiency is 79 percent, the efficiency is higher, a large amount of active ingredients such as unsaturated fatty acid and the like are reserved, and the obtained product is transparent, free of fishy smell and good in quality.
Example 2
(1) Pretreating crocodile oil adipose tissues: mixing crocodile fat and water according to a ratio of 1:1, and chopping into paste;
(2) ultra-high pressure auxiliary enzymolysis: placing the mixed solution in an ultrahigh pressure container, extracting the alligator oil by an ultrahigh pressure auxiliary enzymolysis method under the conditions of 250MPa, 55 ℃ and 5h, wherein the selected enzyme is a compound enzyme (keratinase: lipase: 1.5: 1), boosting pressure after enzymolysis is finished, inactivating the enzyme, and inactivating the enzyme for 30min under the conditions of 450MPa, and separating meat residues, oil and water out-of-phase from the enzymolysis solution to obtain a crude product of the alligator oil;
(3) decoloring and deodorizing: introducing steam into the crude oil for 30min by using a steam generator, wherein the steam flow rate is 70m/s, the rotation speed is 200r/min, condensing and vacuumizing to remove fishy smell, and then performing oil-water separation; adding activated carbon and clay into the crude oil for decolorization and deodorization, and specifically comprising the following steps: adding 2.5% active carbon, keeping the temperature for 30min, and filtering; adding 2.5% of argil, keeping the temperature for 30min, centrifuging, filtering and taking a supernatant; simultaneously adding 2.5% of active carbon and argil (1:1), keeping the temperature for 30min, centrifuging (12000rpm, 15min), filtering and taking the supernatant;
(4) removing impurities and bacteria: adopting organic membrane (pore diameter of 0.22 μm) filtration method to effectively remove foreign matters in refining process and sterilize to obtain essential oil.
The results of this example are: by adopting an ultrahigh pressure auxiliary composite enzymolysis method and combining a steam distillation method, the enzymolysis efficiency is 77.4%, the efficiency is higher, a large amount of active ingredients such as unsaturated fatty acid and the like are reserved, and the obtained product is transparent, free of fishy smell and good in quality.
Example 3
(1) Pretreating crocodile oil adipose tissues: mixing crocodile fat and water according to a ratio of 1:1, and chopping into paste;
(2) ultra-high pressure auxiliary enzymolysis: placing the mixed solution in an ultrahigh pressure container, extracting the alligator oil by an ultrahigh pressure auxiliary enzymolysis method under the conditions of 280MPa, 65 ℃ and 4h, wherein the selected enzyme is a compound enzyme (keratinase: lipase: 2: 1), after the enzymolysis is finished, boosting pressure, inactivating the enzyme and inactivating the enzyme for 25min under the conditions of 500MPa, and separating meat residue, oil and water out-of-phase from the enzymolysis solution to obtain a crude product of the alligator oil;
(3) decoloring and deodorizing: introducing steam into the crude oil for 30min by using a steam generator, wherein the steam flow rate is 50m/s, the rotating speed is 120r/min, condensing and vacuumizing to remove fishy smell, and then performing oil-water separation; adding activated carbon and clay into the crude oil for decolorization and deodorization, and specifically comprising the following steps: adding 1.5% active carbon, keeping the temperature for 30min, and filtering; adding 1.5% of argil, keeping the temperature for 30min, centrifuging, filtering and taking the supernatant; simultaneously adding 1.5% of active carbon and argil (1:1), keeping the temperature for 30min, centrifuging (12000rpm, 15min), filtering and taking the supernatant;
(4) removing impurities and bacteria: adopting organic membrane (pore diameter of 0.22 μm) filtration method to effectively remove foreign matters in refining process and sterilize to obtain essential oil.
The results of this example are: by adopting an ultrahigh pressure auxiliary composite enzymolysis method and combining a steam distillation method, the enzymolysis efficiency is 76.2 percent, the efficiency is higher, a large amount of active ingredients such as unsaturated fatty acid and the like are reserved, and the obtained product is transparent, free of fishy smell and good in quality.
Comparative example 1
(1) Pretreating crocodile oil adipose tissues: mixing crocodile fat and water according to a ratio of 1:1, and chopping into paste;
(2) enzymolysis: placing the mixed solution in an enzyme container, extracting the crocodile oil by an enzymolysis method, wherein the enzymolysis condition is 60 ℃, 4 hours, the selected enzyme is a compound enzyme (keratinase: lipase ═ 1:1), after the enzymolysis is finished, heating up, inactivating the enzyme and inactivating the enzyme, the condition is 85 ℃, 25 minutes, and separating meat residue, oil and water out-of-phase from the enzymolysis solution to obtain a crude crocodile oil;
(3) decoloring and deodorizing: introducing steam into the crude oil for 30min by using a steam generator, wherein the steam flow rate is 60m/s, the rotation speed is 150r/min, condensing, vacuumizing and removing fishy smell, and then performing oil-water separation; adding activated carbon and clay into the crude oil for decolorization and deodorization, and specifically comprising the following steps: adding 2% active carbon, keeping the temperature for 30min, and filtering; adding 2% of argil, keeping the temperature for 30min, centrifuging, filtering and taking supernatant; simultaneously adding 2% of active carbon and argil (1:1), keeping the temperature for 30min, centrifuging (12000rpm, 15min), filtering and taking the supernatant;
(4) removing impurities and bacteria: adopting organic membrane (pore diameter of 0.22 μm) filtration method to effectively remove foreign matters in refining process and sterilize to obtain essential oil.
The results of this comparative example are: by a composite enzymolysis method and a steam distillation method, the enzymolysis efficiency is 62 percent, the efficiency is lower, partial unsaturated fatty acid and other active ingredients are damaged, and the obtained product is transparent, free of fishy smell and general in quality.
Comparative example 2
(1) Pretreating crocodile oil adipose tissues: mixing crocodile fat and water according to a ratio of 1:1, and chopping into paste;
(2) ultra-high pressure auxiliary enzymolysis: placing the mixed solution in an ultrahigh pressure container, extracting the alligator oil by an ultrahigh pressure auxiliary enzymolysis method under the conditions of 200MPa, 60 ℃ and 4 hours, wherein the selected enzyme is a compound enzyme (keratinase: lipase: 1), after the enzymolysis is finished, boosting pressure, inactivating the enzyme and inactivating the enzyme for 25 minutes under the conditions of 500MPa, and separating meat residue, oil and water out-of-phase from the enzymolysis solution to obtain a crude product of the alligator oil;
(3) decoloring and deodorizing: adding activated carbon and clay into the crude oil for decolorization and deodorization, and specifically comprising the following steps: adding 2% active carbon, keeping the temperature for 30min, and filtering; adding 2% of argil, keeping the temperature for 30min, centrifuging, filtering and taking supernatant; simultaneously adding 2% of active carbon and argil (1:1), keeping the temperature for 30min, centrifuging (12000rpm, 15min), filtering and taking the supernatant;
(4) removing impurities and bacteria: adopting organic membrane (pore diameter of 0.22 μm) filtration method to effectively remove foreign matters in refining process and sterilize to obtain essential oil.
The results of this example are: by adopting an ultrahigh pressure auxiliary complex enzymolysis method, the enzymolysis efficiency is 78.2%, the efficiency is higher, a large amount of unsaturated fatty acid and other active ingredients are reserved, and the obtained product is yellowish in color, has little fishy smell and is general in quality.
The fatty acid components of the alligator oil prepared in the examples and the comparative examples are detected, and the specific results are shown in table 1:
TABLE 1
The table shows that the content of fatty acid in the crocodile oil extracted by the ultrahigh pressure auxiliary enzymolysis is obviously higher than that of the crocodile oil extracted by the common enzymolysis, particularly the content of unsaturated fatty acid such as ARA, EPA and DHA which are beneficial to human bodies is obviously improved, the extraction efficiency of the crocodile oil is improved by the ultrahigh pressure auxiliary enzymolysis, a large amount of nutrient components such as unsaturated fatty acid can be reserved, and the subsequent high-quality product development is facilitated.
The concentrations in table 1 are calculated by the instrument according to figures 1 and 2.
The above is not relevant and is applicable to the prior art.
While certain specific embodiments of the present invention have been described in detail by way of illustration, it will be understood by those skilled in the art that the foregoing is illustrative only and is not limiting of the scope of the invention, as various modifications or additions may be made to the specific embodiments described and substituted in a similar manner by those skilled in the art without departing from the scope of the invention as defined in the appending claims. It should be understood by those skilled in the art that any modifications, equivalents, improvements and the like made to the above embodiments in accordance with the technical spirit of the present invention are included in the scope of the present invention.
Claims (10)
1. A method for extracting refined alligator oil is characterized by comprising the following steps: the method comprises the following steps:
(1) pretreating crocodile oil adipose tissues: mixing crocodile fat and water in proportion and chopping into paste;
(2) ultra-high pressure auxiliary enzymolysis: placing minced alligator fat in an ultrahigh pressure container, extracting alligator oil by using an ultrahigh pressure auxiliary complex enzymolysis method, then boosting pressure, inactivating enzyme, and separating meat residue, oil and water out-of-phase from enzymolysis liquid to obtain crude alligator oil;
(3) decoloring and deodorizing: removing fishy smell of the crocodile oil crude product obtained in the step (2) by adopting a steam distillation method, performing oil-water separation to obtain crude oil, and adding activated carbon and carclazyte into the crude oil to decolor and remove fishy smell;
(4) removing impurities and bacteria: removing foreign matters in the crude oil obtained in the step (3) and sterilizing to obtain the essential oil.
2. A process for extracting refined alligator oil as claimed in claim 1, wherein: the specific steps of the step (3) are as follows: introducing steam into the crude alligator oil obtained in the step (2) by using a steam generator for 20-50min, and then carrying out oil-water separation; then adding a certain amount of activated carbon and argil, preserving the heat for 20-40min, and filtering; adding argil, keeping the temperature for 20-40min, centrifuging, filtering and taking the supernatant; adding active carbon and clay, maintaining the temperature for 20-40min, centrifuging, filtering, and collecting supernatant.
3. A process for extracting refined alligator oil as claimed in claim 2, wherein: in the step (2): the steam distillation method conditions are that the steam flow rate is 50-70m/s, the rotating speed is 100-200r/min, and the time is 20-50 min.
4. A process for extracting refined alligator oil as claimed in claim 3, wherein: the adding amount of the first activated carbon is 1-3% of the mass of the crude oil, the adding amount of the clay is 1-3% of the mass of the crude oil, the total adding amount of the second activated carbon and the clay is 1-3% of the mass of the crude oil, the temperature is 50-65 ℃, the centrifugation condition is 12000rpm and 15 min.
5. A process for extracting refined alligator oil as claimed in claim 2, wherein: the mass ratio of the activated carbon to the clay is 1: 1.
6. A process for extracting refined alligator oil as claimed in claim 1, wherein: in the step (1): the ratio of crocodile fat to water is between 1:0.5 and 1: 2.
7. A process for extracting refined alligator oil as claimed in claim 1, wherein: the ultrahigh pressure auxiliary enzymolysis condition in the step (2) is 150-300MPa, 50-65 ℃ and 3-5h, and the selected enzymes are lipase and keratinase.
8. A process for extracting refined alligator oil as claimed in claim 1, wherein: the conditions of enzyme inactivation and inactivation after the enzymolysis in the step (2) are 450-600MPa and 15-30 min.
9. A process for extracting refined alligator oil as claimed in claim 1, wherein: and (4) removing impurities and bacteria, and filtering the crude oil obtained in the step (3) by using an organic membrane.
10. A process for extracting refined alligator oil according to claim 9, wherein: the organic membrane is an organic membrane with a pore diameter of 0.22 mu m.
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| CN114317115A (en) * | 2021-12-09 | 2022-04-12 | 河南天源药物研究有限公司 | Extraction of essential oil from sweet wormwood herb and extraction process thereof |
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