CN106800969B - Process for extracting fish oil from internal organs of cuttlefish by segmented compound enzymolysis method - Google Patents

Process for extracting fish oil from internal organs of cuttlefish by segmented compound enzymolysis method Download PDF

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CN106800969B
CN106800969B CN201710050057.6A CN201710050057A CN106800969B CN 106800969 B CN106800969 B CN 106800969B CN 201710050057 A CN201710050057 A CN 201710050057A CN 106800969 B CN106800969 B CN 106800969B
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enzymolysis
cuttlefish
alkaline
fish oil
weight ratio
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CN106800969A (en
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刘文穗
陈郴永
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Shishi City Huabao Marine Biopharmaceutical Co ltd
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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
    • 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

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  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
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Abstract

The invention discloses a process for extracting fish oil from cuttlefish viscera by a segmented compound enzymolysis method, which comprises the following specific steps: the method has the advantages that raw material treatment, primary enzymolysis, secondary enzymolysis and oil-water separation are carried out, the extraction rate of the cuttlefish oil can be effectively improved, the damage to main functional components of the fish oil can be reduced as low as possible, the quality of the cuttlefish oil is improved, meanwhile, no chemical solvent is used in the whole extraction process, the solvent recovery and the environmental pollution are avoided, the energy is saved, the environment is protected, the safety is realized, and on the other hand, the extraction rate of the cuttlefish oil is higher due to the adoption of the segmented composite enzymolysis and the special stable catalyst technology thereof, and the economic benefit of an enterprise is further improved.

Description

Process for extracting fish oil from internal organs of cuttlefish by segmented compound enzymolysis method
Technical Field
The invention relates to the technical field of deep processing of marine aquatic products, in particular to a process for extracting fish oil from cuttlefish viscera by a segmented compound enzymolysis method.
Background
The deep sea fish oil is rich in polyunsaturated fatty acids such as EPA, DHA, omega-3 acid and the like, has various physiological activities such as enhancing nervous system function, benefiting intelligence, strengthening brain, preventing senile dementia, inhibiting platelet aggregation, reducing thrombosis, preventing cardiovascular and cerebrovascular diseases, resisting inflammation and cancer, enhancing autoimmunity, protecting eyesight and the like, and is increasing in the number of commodities based on the nutrition and medicinal value of the fish oil, and the extraction and development of the fish oil become hot spots for developing and utilizing food resources.
The production method of the fish oil mainly comprises a squeezing method, a light alkali hydrolysis method, a solvent method, a water method, an enzymolysis method and the like, wherein the squeezing method is mainly used for byproducts of fish meal processing plants, the extraction rate of the fish oil is generally low, and the quality is poor; the alkali concentration of the dilute alkali hydrolysis method is not easy to control, the hydrolysis is incomplete when the alkali concentration is too low, the fish oil saponification is caused when the alkali concentration is too high, the extraction rate of the oil is reduced, the sodium salt content of the wastewater generated in the extraction process is high, the wastewater cannot be further utilized, and new waste is formed; the solvent method adopts an organic solvent to extract fat in the raw materials, and the extracted fish oil may have solvent residue and is limited in application; the enzymatic extraction condition is mild, the damage to the functional components of the fish oil is low, the quality of the produced fish oil is high, and meanwhile, the protease hydrolysis can be fully utilized to produce the enzymatic hydrolysate.
The cuttlefish is one of four seas in China and plays a very important role in production, cuttlefish oil extracted from internal organs of the cuttlefish has been sold as a feed additive in Zhejiang, Shandong, Fujian and the like, and researches show that the liver of the cuttlefish contains rich polyunsaturated fatty acids [1,2] and is an important source of substances such as DHA, EPA, squalene and the like. How to fully extract the cuttlefish oil, reduce the damage of the functional components of the fish oil as low as possible and improve the quality of the cuttlefish oil is of great significance to the fish product deep processing and scientific research enterprises in the field.
Disclosure of Invention
The invention discloses a process for extracting fish oil from cuttlefish viscera by a segmented compound enzymatic hydrolysis method, which mainly aims to overcome the defects and shortcomings in the prior art, and provides an extraction process of the cuttlefish oil.
The technical scheme adopted by the invention is as follows:
a process for extracting fish oil from cuttlefish viscera by a segmented compound enzymolysis method comprises the following specific steps:
(1) raw material treatment: removing ink sacs and impurities from the viscera of the cuttlefish, cleaning the viscera, and grinding the viscera of the cuttlefish into pulp by using a colloid mill to obtain uniform pulp;
(2) primary enzymolysis: adding the obtained homogenate into an enzymolysis tank, and homogenizing according to the following steps: water = 1: adding water in a weight ratio of 1.5-2.5, adjusting the pH value to 8.5-9.5 by using alkali, adding an alkaline complex enzyme accounting for 0.4-0.6 wt% of the homogenate material into an enzymolysis tank, adding a special stabilizing catalyst A accounting for 1/5 wt% of the alkaline complex enzyme, heating, controlling the temperature of the mixed material liquid to be 40-50 ℃, and then stirring for 1.5-2 hours under heat preservation to obtain a primary enzymolysis liquid;
(3) secondary enzymolysis: adjusting the pH of the primary enzymolysis liquid obtained in the step (2) to 4.5-5.5 by using acid, adding acidic mixed enzyme accounting for 0.2-0.4% of the weight of the enzymolysis liquid for enzymolysis, adding a special stable catalyst B accounting for 1/10 of the weight of the enzyme, firstly heating and controlling the temperature of the liquid at 50-60 ℃, preserving the heat for 1.5-2 hours, then heating to 90-95 ℃, and preserving the heat for 15-20min to obtain a secondary enzymolysis liquid;
(4) oil-water separation: and (4) filtering and deslagging the secondary enzymolysis liquid obtained in the step (3), and then separating and processing by using a high-speed centrifuge to obtain the refined fish oil.
Further, the alkaline complex enzyme in the step 2 comprises alkaline marine protease and alkaline lipase, and the weight ratio of the alkaline marine protease to the alkaline lipase is 1: 0.3 to 0.5.
Furthermore, the weight ratio of the alkaline marine protease to the alkaline lipase in the alkaline complex enzyme is 1: 0.5.
further, the special stable catalyst A in the step 2 is CaCl2And N-acetylglucosamine, wherein the weight ratio of the two is 1: 0.5 to 1.0.
Further, the CaCl2The weight ratio of the N-acetylglucosamine to the mixture is 1: 0.8.
further, the acid mixed enzyme in the step 3 comprises acid marine protease and acid lipase, and the weight ratio of the acid marine protease to the acid lipase is 1: 0.3 to 0.5.
Further, the weight ratio of the acidic marine protease to the acidic lipase is 1: 0.3.
further, the special stable catalyst B in the step (3) is CaCl2And a chitosan oligosaccharide mixture, wherein the weight ratio of the chitosan oligosaccharide mixture to the chitosan oligosaccharide mixture is 1: 1.5 to 2.0.
Further, the CaCl2The weight ratio of the chitosan oligosaccharide to the chitosan oligosaccharide mixture is 1: 1.5.
an oil product comprising the fish oil prepared by the preparation process of any one of claims 1 to 9.
As can be seen from the above description of the present invention, compared with the prior art, the present invention has the following advantages:
1. the method for extracting the cuttlefish oil is innovative, the cuttlefish oil is extracted by the segmented compound enzymolysis method, and the structure of the main effective components of the cuttlefish oil is not damaged because high-temperature cooking is not adopted in the extraction process, so that the quality of the cuttlefish oil is improved.
2, the invention avoids solvent recovery and environmental pollution because no chemical solvent is used in the whole process of extracting the fish oil, and is energy-saving, environment-friendly and safe.
3. The invention adopts the technology of segmented composite enzymolysis and special stable catalyst thereof, so that the extraction rate of the cuttlefish oil is higher, and the economic benefit of enterprises is further improved.
Detailed Description
Example one
A process for extracting fish oil from cuttlefish viscera by a segmented compound enzymolysis method comprises the following specific steps:
(1) raw material treatment: removing ink sacs and impurities from the viscera of the cuttlefish, cleaning the viscera, and grinding the viscera of the cuttlefish into pulp by using a colloid mill to obtain uniform pulp;
(2) primary enzymolysis: adding the obtained homogenate into an enzymolysis tank, and homogenizing according to the following steps: water = 1: adding water according to the weight ratio of 2.0, then adjusting the pH value to 8.5 by using alkali, then adding an alkaline complex enzyme accounting for 0.4 percent of the weight of the homogenate material into the enzymolysis tank, adding a special stabilizing catalyst A accounting for 1/5 percent of the weight of the alkaline complex enzyme, heating, controlling the temperature of the mixed material liquid to be 40-50 ℃, and then stirring for 1.5-2 hours under heat preservation to obtain a primary enzymolysis liquid;
(3) secondary enzymolysis: regulating the pH of the primary enzymolysis liquid obtained in the step (2) to 4.5 by using acid, then adding acidic mixed enzyme accounting for 0.2 percent of the weight of the enzymolysis liquid for enzymolysis, then adding a special stable catalyst B accounting for 1/10 percent of the weight of the enzyme, firstly heating and controlling the temperature of the liquid at 50-60 ℃, preserving heat for 1.5-2 hours, then heating to 90-95 ℃, and preserving heat for 15-20 minutes to obtain secondary enzymolysis liquid;
(4) oil-water separation: and (4) filtering and deslagging the secondary enzymolysis liquid obtained in the step (3), and then separating and processing by using a high-speed centrifuge to obtain the refined fish oil.
Further, the alkaline complex enzyme in the step 2 comprises alkaline marine protease and alkaline lipase, and the weight ratio of the alkaline marine protease to the alkaline lipase is 1: 0.3.
further, the special stable catalyst A in the step 2 is CaCl2And N-acetylglucosamine, wherein the weight ratio of the two is 1: 0.5.
further, the acid mixed enzyme in the step 3 comprises acid marine protease and acid lipase, and the weight ratio of the acid marine protease to the acid lipase is 1: 0.3.
further, the special stable catalyst B in the step (3) is CaCl2And a chitosan oligosaccharide mixture, wherein the weight ratio of the chitosan oligosaccharide mixture to the chitosan oligosaccharide mixture is 1: 1.5.
example two
A process for extracting fish oil from cuttlefish viscera by a segmented compound enzymolysis method comprises the following specific steps:
(1) raw material treatment: removing ink sacs and impurities from the viscera of the cuttlefish, cleaning the viscera, and grinding the viscera of the cuttlefish into pulp by using a colloid mill to obtain uniform pulp;
(2) primary enzymolysis: adding the obtained homogenate into an enzymolysis tank, and homogenizing according to the following steps: water = 1: 2.5, adding water, then adjusting the pH to 9.5 by using alkali, then adding an alkaline complex enzyme accounting for 0.6 percent of the weight of the homogenate material into the enzymolysis tank, then adding a special stabilizing catalyst A accounting for 1/5 percent of the weight of the alkaline complex enzyme, heating, controlling the temperature of the mixed material liquid to be 40-50 ℃, and then stirring for 1.5-2 hours under heat preservation to obtain a primary enzymolysis liquid;
(3) secondary enzymolysis: regulating the pH of the primary enzymolysis liquid obtained in the step (2) to 5.5 by using acid, then adding acidic mixed enzyme accounting for 0.4 percent of the weight of the enzymolysis liquid for enzymolysis, then adding a special stable catalyst B accounting for 1/10 percent of the weight of the enzyme, firstly heating and controlling the temperature of the liquid at 50-60 ℃, preserving heat for 1.5-2 hours, then heating to 90-95 ℃, and preserving heat for 15-20 minutes to obtain secondary enzymolysis liquid;
(4) oil-water separation: and (4) filtering and deslagging the secondary enzymolysis liquid obtained in the step (3), and then separating and processing by using a high-speed centrifuge to obtain the refined fish oil.
Further, the alkaline complex enzyme in the step 2 comprises alkaline marine protease and alkaline lipase, and the weight ratio of the alkaline marine protease to the alkaline lipase is 1: 0.5.
Further, the special stable catalyst A in the step 2 is CaCl2And N-acetylglucosamine, wherein the weight ratio of the two is 1: 1.0.
Further, the acid mixed enzyme in the step 3 comprises acid marine protease and acid lipase, and the weight ratio of the acid marine protease to the acid lipase is 1: 0.5.
Further, the special stable catalyst B in the step (3) is CaCl2And a chitosan oligosaccharide mixture, wherein the weight ratio of the chitosan oligosaccharide mixture to the chitosan oligosaccharide mixture is 1: 2.0.
EXAMPLE III
A process for extracting fish oil from cuttlefish viscera by a segmented compound enzymolysis method comprises the following specific steps:
(1) raw material treatment: removing ink sacs and impurities from the viscera of the cuttlefish, cleaning the viscera, and grinding the viscera of the cuttlefish into pulp by using a colloid mill to obtain uniform pulp;
(2) primary enzymolysis: adding the obtained homogenate into an enzymolysis tank, and homogenizing according to the following steps: water = 1: 2.5, adding water, then adjusting the pH to 9.5 by using alkali, then adding an alkaline complex enzyme accounting for 0.5 percent of the weight of the homogenate material into the enzymolysis tank, then adding a special stabilizing catalyst A accounting for 1/5 percent of the weight of the alkaline complex enzyme, heating, controlling the temperature of the mixed material liquid to be 40-50 ℃, and then stirring for 1.5-2 hours under heat preservation to obtain a primary enzymolysis liquid;
(3) secondary enzymolysis: regulating the pH of the primary enzymolysis liquid obtained in the step (2) to 5.5 by using acid, then adding acidic mixed enzyme accounting for 0.3 percent of the weight of the enzymolysis liquid for enzymolysis, then adding a special stable catalyst B accounting for 1/10 percent of the weight of the enzyme, firstly heating and controlling the temperature of the liquid at 50-60 ℃, preserving heat for 1.5-2 hours, then heating to 90-95 ℃, and preserving heat for 15-20 minutes to obtain secondary enzymolysis liquid;
(4) oil-water separation: and (4) filtering and deslagging the secondary enzymolysis liquid obtained in the step (3), and then separating and processing by using a high-speed centrifuge to obtain the refined fish oil.
Further, the alkaline complex enzyme in the step 2 comprises alkaline marine protease and alkaline lipase, and the weight ratio of the alkaline marine protease to the alkaline lipase is 1: 0.4.
further, the special stable catalyst A in the step 2 is CaCl2And N-acetylglucosamine, wherein the weight ratio of the two is 1: 0.8.
further, the acid mixed enzyme in the step 3 comprises acid marine protease and acid lipase, and the weight ratio of the acid marine protease to the acid lipase is 1: 0.4.
further, the special stable catalyst B in the step (3) is CaCl2And a chitosan oligosaccharide mixture, wherein the weight ratio of the chitosan oligosaccharide mixture to the chitosan oligosaccharide mixture is 1: 1.8.
the fish oil products of the above examples were tested and the properties of the fish oil, the total content of DHA, EPA and omega-3 acids in each example are shown in table 1:
table 1: comparison of Fish oil Performance, DHA, EPA and Total omega-3 acid content in the examples
Performance testing Example 1 Example 2 Example 3
Appearance of the product Orange yellow, clear and transparent Orange yellow, clear and transparent Orange yellow, clear and transparent
Smell(s) Has no fishy smell of fish oil and no sour taste Has no fishy smell of fish oil and no sour taste Has no fishy smell of fish oil and no sour taste
Acid value 6.5 5.8 6.2
EPA content% 17.9 18.6 18.2
DHA content% 8.9 9.8 9.3
Total omega-3 fatty acids (Glycerol type) 33.7 34.5 33.9
Due to the adoption of the segmented composite enzymolysis and the special stable catalyst technology, the extraction rate is higher, and the extraction rate of each implementation is shown in the table 2:
Figure DEST_PATH_IMAGE001
the method for extracting the cuttlefish oil is innovative, the cuttlefish oil is extracted by the segmented compound enzymolysis method, and the structure of the main effective components of the cuttlefish oil is not damaged because high-temperature cooking is not adopted in the extraction process, so that the quality of the cuttlefish oil is improved. Meanwhile, no chemical solvent is used in the whole process of extracting the fish oil, so that solvent recovery and environmental pollution are avoided, and the method is energy-saving, environment-friendly and safe. On the other hand, the invention adopts the technology of the segmented composite enzymolysis and the special stable catalyst thereof, so that the extraction rate of the cuttlefish oil is higher, and the economic benefit of enterprises is further improved.
The above description is only an embodiment of the present invention, but the design concept of the present invention is not limited thereto, and any insubstantial modifications of the present invention using this concept shall fall within the scope of infringing the present invention.

Claims (6)

1. A process for extracting fish oil from cuttlefish viscera by a segmented compound enzymolysis method is characterized by comprising the following steps: the process comprises the following specific steps:
(1) raw material treatment: removing ink sacs and impurities from the viscera of the cuttlefish, cleaning the viscera, and grinding the viscera of the cuttlefish into pulp by using a colloid mill to obtain uniform pulp;
(2) primary enzymolysis: adding the obtained homogenate into an enzymolysis tank, and homogenizing according to the following steps: water = 1: adding water in a weight ratio of 1.5-2.5, adjusting the pH value to 8.5-9.5 by using alkali, adding an alkaline complex enzyme accounting for 0.4-0.6 wt% of the homogenate material into an enzymolysis tank, adding a special stabilizing catalyst A accounting for 1/5 wt% of the alkaline complex enzyme, heating, controlling the temperature of the mixed material liquid to be 40-50 ℃, and then stirring for 1.5-2 hours under heat preservation to obtain a primary enzymolysis liquid;
(3) secondary enzymolysis: adjusting the pH of the primary enzymolysis liquid obtained in the step (2) to 4.5-5.5 by using acid, adding acidic mixed enzyme accounting for 0.2-0.4% of the weight of the enzymolysis liquid for enzymolysis, adding a special stable catalyst B accounting for 1/10 of the weight of the enzyme, firstly heating and controlling the temperature of the liquid at 50-60 ℃, preserving the heat for 1.5-2 hours, then heating to 90-95 ℃, and preserving the heat for 15-20min to obtain a secondary enzymolysis liquid;
(4) oil-water separation: filtering and deslagging the secondary enzymolysis liquid obtained in the step (3), and then separating and processing by using a high-speed centrifuge to obtain refined fish oil;
the special stable catalyst A in the step (2) is CaCl2With N-acetylglucosamine, bothThe weight ratio of (1): 0.5 to 1.0;
the alkaline complex enzyme in the step (2) comprises alkaline marine protease and alkaline lipase, and the weight ratio of the alkaline marine protease to the alkaline lipase is 1: 0.3 to 0.5;
the acid mixed enzyme in the step (3) comprises acid marine protease and acid lipase, and the weight ratio of the acid marine protease to the acid lipase is 1: 0.3 to 0.5;
the special stable catalyst B in the step (3) is CaCl2And a chitosan oligosaccharide mixture, wherein the weight ratio of the chitosan oligosaccharide mixture to the chitosan oligosaccharide mixture is 1: 1.5 to 2.0.
2. The process for extracting fish oil from cuttlefish viscera by the segmented complex enzymolysis method according to claim 1, which is characterized in that: the weight ratio of the alkaline marine protease to the alkaline lipase in the alkaline complex enzyme is 1: 0.5.
3. the process for extracting fish oil from cuttlefish viscera by the segmented complex enzymolysis method according to claim 1, which is characterized in that: the CaCl is2The weight ratio of the N-acetylglucosamine to the mixture is 1: 0.8.
4. the process for extracting fish oil from cuttlefish viscera by the segmented complex enzymolysis method according to claim 1, which is characterized in that: the weight ratio of the acidic marine protease to the acidic lipase is 1: 0.3.
5. the process for extracting fish oil from cuttlefish viscera by the segmented complex enzymolysis method according to claim 1, which is characterized in that: the CaCl is2The weight ratio of the chitosan oligosaccharide to the chitosan oligosaccharide mixture is 1: 1.5.
6. an oil product comprising the fish oil prepared by the preparation process of any one of claims 1 to 5.
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103060410A (en) * 2012-12-29 2013-04-24 青岛安芙兰生物科技有限公司 Method for extracting biological active peptide from sea aquatic product
CN103060076A (en) * 2012-11-02 2013-04-24 浙江省海洋开发研究院 Method for preparing fish oil by virtue of leftovers of tuna
CN103725403A (en) * 2013-12-06 2014-04-16 山东好当家海洋发展股份有限公司 Method for extracting engraulis japonicus oil by two-enzyme method

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103060076A (en) * 2012-11-02 2013-04-24 浙江省海洋开发研究院 Method for preparing fish oil by virtue of leftovers of tuna
CN103060410A (en) * 2012-12-29 2013-04-24 青岛安芙兰生物科技有限公司 Method for extracting biological active peptide from sea aquatic product
CN103725403A (en) * 2013-12-06 2014-04-16 山东好当家海洋发展股份有限公司 Method for extracting engraulis japonicus oil by two-enzyme method

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