CN112515169A - Flaxseed oil, and preparation method of compound emulsion and high internal phase emulsion thereof - Google Patents
Flaxseed oil, and preparation method of compound emulsion and high internal phase emulsion thereof Download PDFInfo
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- CN112515169A CN112515169A CN202011327345.XA CN202011327345A CN112515169A CN 112515169 A CN112515169 A CN 112515169A CN 202011327345 A CN202011327345 A CN 202011327345A CN 112515169 A CN112515169 A CN 112515169A
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- emulsion
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- linseed oil
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Images
Classifications
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/115—Fatty acids or derivatives thereof; Fats or oils
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
- A23D9/00—Other edible oils or fats, e.g. shortenings, cooking oils
- A23D9/007—Other edible oils or fats, e.g. shortenings, cooking oils characterised by ingredients other than fatty acid triglycerides
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
- A23D9/00—Other edible oils or fats, e.g. shortenings, cooking oils
- A23D9/02—Other edible oils or fats, e.g. shortenings, cooking oils characterised by the production or working-up
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- A—HUMAN NECESSITIES
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- A23D9/00—Other edible oils or fats, e.g. shortenings, cooking oils
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- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
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- A23L29/045—Organic compounds containing nitrogen as heteroatom
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
- A23L29/30—Foods or foodstuffs containing additives; Preparation or treatment thereof containing carbohydrate syrups; containing sugars; containing sugar alcohols, e.g. xylitol; containing starch hydrolysates, e.g. dextrin
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
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- A23L3/3454—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
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- A23L3/3481—Organic compounds containing oxygen
- A23L3/3499—Organic compounds containing oxygen with doubly-bound oxygen
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
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- A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
- A23L3/3454—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
- A23L3/3463—Organic compounds; Microorganisms; Enzymes
- A23L3/3562—Sugars; Derivatives thereof
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23P—SHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
- A23P10/00—Shaping or working of foodstuffs characterised by the products
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
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Abstract
The invention discloses linseed oil, a compound emulsion thereof, a high internal phase emulsion and a preparation method thereof. The preparation method of the linseed oil and the compound emulsion thereof comprises the following steps: polysaccharide and protein are used as emulsification wall materials, and oil or a compound of the oil and fat-soluble components is used as a core material; adding a polysaccharide solution and a protein solution into grease or the compound, and performing high-speed shearing or ultrasonic emulsification to obtain a coarse emulsion; and (3) homogenizing the crude emulsion under high pressure, and adjusting the pH of the system to 3-4 to obtain the product. Centrifuging the emulsion to obtain the high internal phase emulsion. The linseed oil, the compound emulsion and the high internal phase emulsion prepared by the invention can keep better stability in the process treatments of wider pH range, higher ionic strength, sterilization and the like. The linseed oil and the compound emulsion thereof and the high internal phase emulsion prepared by the invention have good storage stability, and the complex formed by the polysaccharide and the protein can prevent the demulsification phenomenon and better protect the linseed oil and the compound thereof.
Description
Technical Field
The invention belongs to the field of grease processing, and particularly relates to linseed oil and a preparation method of a compound emulsion and a high internal phase emulsion thereof.
Background
The content of unsaturated fatty acid in linseed oil is up to more than 90%, wherein the content of alpha-linolenic acid is the highest (some varieties exceed 54%), the alpha-linolenic acid is n-3 series essential fatty acid for human body, can be converted into EPA and DHA in vivo, and has physiological functions of promoting the growth and development of fetus and baby brain, enhancing memory, improving immunity, improving and maintaining vision, preventing cerebral thrombosis and myocardial infarction, and the like. As a good n-3 series unsaturated fatty acid raw material, the linseed oil is easy to oxidize due to the high content of the unsaturated fatty acid, so that bad flavor and even harmful substances are generated, and the shelf life of the linseed oil is influenced.
The highly unsaturated fatty acids of linseed oil are easily lost during traditional cooking, which severely limits the use of linseed oil in diet and food processing formulations. The direct eating of linseed oil has great challenge on the traditional dietary habits of residents in China. The emulsion has a soft and smooth taste, and the linseed oil is prepared into the stable emulsion, so that on one hand, the specific functional components in the oil are greatly reserved, and on the other hand, the emulsion is suitable for the traditional dietary habits of residents in China, thereby solving the problem of efficiently supplementing the n-3 series unsaturated fatty acid. The high viscosity emulsion can replace salad sauce in fruit and vegetable salad, and has n-3 fatty acid strengthening effect in daily diet, and the low viscosity emulsion can be used as beverage for daily carrying and drinking.
In the emulsion wall material, polysaccharide and protein attract great attention due to their natural safety characteristics, and common natural polysaccharides include sodium alginate, chitosan, acacia, carrageenan and the like, and natural proteins include whey protein, bovine serum albumin, casein and the like. However, the thickness of the interfacial film is very thin, and it is very susceptible to environmental influences, such as acid, alkali, heat, etc., resulting in instability of the emulsion system. For the stabilization of emulsion systems, large amounts of synthetic emulsifiers are often added, and the safety of the emulsifiers is now a concern for some scholars.
Disclosure of Invention
In order to solve the problems, the invention provides a grease and a preparation method of a compound emulsion and a high internal phase emulsion thereof. The invention selects polysaccharide with negative electricity to be mixed with protein solution, grease or compound thereof to prepare emulsion. Then according to the characteristics of the protein, the charge is changed from negative electricity to positive point around the isoelectric point, and polysaccharide and protein complexes are formed by adjusting the pH value of the emulsion, so that the instability of the emulsion is avoided.
The preparation method of the grease and the compound emulsion thereof provided by the invention comprises the following steps:
1) preparation of wall material and core material
Polysaccharide and protein are used as emulsification wall materials, and oil or a compound of the oil and fat-soluble components is used as a core material;
preparing a polysaccharide solution, wherein the polysaccharide is negatively charged;
preparing a protein solution, wherein the protein is negatively charged protein;
2) preparation of the crude solution
Adding the polysaccharide solution and the protein solution into the grease or the compound, and performing high-speed shearing or ultrasonic emulsification to obtain a coarse emulsion;
3) preparation of the emulsion
And (3) homogenizing the crude emulsion at high pressure, and adjusting the pH of the system to 3-4 by adopting 10% acetic acid solution or citric acid solution under the condition of continuously stirring after the high-pressure homogenization is finished to obtain the final emulsion.
In step 1) of the above method, the polysaccharide solution may have a mass concentration of 0.5 to 10% (preferably 1 to 3%) of polysaccharide, and the polysaccharide solution exhibits negative electricity. The polysaccharide is selected from one or two of carrageenan and chondroitin sulfate;
in step 1) of the above method, the protein solution may have a protein concentration of 0.3 to 10% (preferably 1 to 3%) by mass, and the protein solution exhibits negative electricity. The protein is selected from one or more of whey protein, bovine serum albumin, casein and egg albumin.
In the step 1), the oil may be at least one selected from linseed oil, peony seed oil, grape seed oil, rose seed oil, coconut oil, camellia oil, peanut oil, germ oil, walnut oil, sesame oil, sunflower seed oil, canola oil, olive oil, tomato seed oil, rapeseed oil, deep sea fish oil, cumin oil, capsicum seed oil, garlic oil and ginger oil. Or dissolving the fat-soluble component in the oil to form a compound of the oil and the fat-soluble component; the fat-soluble component can be curcumin, lycopene, lutein, fat-soluble vitamins, etc.
In the step 2) of the method, the mass ratio of the polysaccharide in the polysaccharide solution to the protein in the protein solution is (1.5-9) to 1, and specifically can be 1.5:1, 7:3, 8:2 or 9: 1.
Further, the volume ratio of the polysaccharide solution, the protein solution, the oil or the compound can be (10-20) mL: (10-20) mL: (10-15) mL.
In the step 2) of the method, the high-speed shearing is carried out by adopting a high-speed shearing machine, and the high-speed shearing condition is that the high-speed shearing is carried out for 1-3min at 5000-20000 rpm;
in step 2), the ultrasonic emulsification conditions are as follows: immersing an ultrasonic probe into the mixture, and carrying out ultrasonic treatment for 1-3min under the conditions of 300-450W; wherein, the ultrasound is carried out for 2-10s (specifically 5s), and the ultrasound is stopped for 1-3s (specifically 2 s).
In the step 3), homogenizing under high pressure by using a high-pressure homogenizer;
the high-pressure homogenization comprises primary homogenization and secondary homogenization;
the pressure of the primary homogenizing can be 250-350 bar, and specifically can be 250bar, 300bar or 350 bar;
the pressure of the secondary homogenization can be 40-80 bar, specifically 50bar and 80 bar.
In the step 3) of the method, the charges of the protein are changed from negative charges to positive charges near the isoelectric point (pH is 3-4), and the protein and the polysaccharide form a complex, so that the instability of the emulsion is avoided.
The grease and the compound emulsion thereof prepared by the method also belong to the protection scope of the invention.
The invention also provides a preparation method of the grease and the compound high internal phase emulsion thereof.
The preparation method of the grease and the compound high internal phase emulsion thereof provided by the invention comprises the following steps: and centrifuging the prepared grease and the compound emulsion thereof to obtain the linseed oil and the compound high internal phase emulsion thereof.
In the above method, the centrifugation conditions are as follows: centrifuging at 1000-; or centrifuging at 5000g for 5 min; or centrifuged at 15000g for 2 min.
The grease prepared by the method and the compound high internal phase emulsion thereof also belong to the protection scope of the invention.
Compared with the prior art, the invention has the following beneficial effects:
1. the emulsifying wall material adopted by the invention is protein and polysaccharide which are natural food-grade materials, and does not contain emulsifying agents such as Tween, Span and the like.
2. The linseed oil and the compound emulsion thereof prepared by the invention have the advantages of small particle size, good dispersibility and high physical stability. The linseed oil and the compound high internal phase emulsion thereof have a pasty structure and higher physical stability.
3. The linseed oil, the compound emulsion and the high internal phase emulsion prepared by the method can keep better stability in the process treatments of wider pH range, higher ionic strength, sterilization and the like.
4. The linseed oil and the compound emulsion thereof and the high internal phase emulsion prepared by the invention have good storage stability, and the complex formed by the polysaccharide and the protein can prevent the demulsification phenomenon and better protect the linseed oil and the compound thereof.
Drawings
FIG. 1 shows the effect of the mass ratio of carrageenan to egg white protein on the potential value.
Detailed Description
The present invention will be further illustrated with reference to the following specific examples, but the present invention is not limited to the following examples. The method is a conventional method unless otherwise specified. The starting materials are commercially available from the open literature unless otherwise specified.
Example 1 preparation of linseed oil emulsions and high internal phase emulsions
1) Preparation of wall material and core material
Carrageenin and egg white protein are used as emulsification wall materials, and linseed oil is used as a core material;
preparing a carrageenan aqueous solution with the mass concentration of 0.6%, wherein the solution presents negative electricity;
preparing an egg white protein aqueous solution with the mass concentration of 0.4%, wherein the solution presents negative electricity.
2) Preparation of the crude emulsion
Adding 100mL of carrageenan aqueous solution prepared in the step 1) and 100mL of egg white protein aqueous solution into 100mL of linseed oil (wherein the mass ratio of the carrageenan to the egg white protein is 6: 4). Shearing the mixture at 10000rpm for 2min by a high-speed shearing machine to obtain a crude emulsion.
3) Preparation of the emulsion
And (3) carrying out secondary homogenization on the coarse emulsion by using a high-pressure homogenizer, wherein the primary homogenization pressure is 350bar, and the secondary homogenization pressure is 50 bar. After homogenization, the pH is adjusted to 3-4 with 10% acetic acid solution under continuous stirring to obtain the final emulsion (i.e. linseed oil emulsion).
4) Preparation of high internal phase emulsions
The final emulsion prepared was centrifuged at 10000g for 5min to give a high internal phase emulsion which exhibited a cream like structure.
The mean particle size of the linseed oil emulsion prepared in this example was 105.3 ± 2.9 nm.
The storage stability of the linseed oil emulsion prepared in this example was tested as follows:
the linolenic acid content of the linseed oil emulsion prepared in the embodiment is respectively reduced by 2.26% and 15.9% after being stored for 20 days at 4 ℃ and 25 ℃; the linolenic acid content of the linseed oil is respectively reduced by 7.8 percent and 26.7 percent after the linseed oil is respectively stored for 20 days at the temperature of 4 ℃ and 25 ℃, and the obvious difference between the linolenic acid content and the linolenic acid content (P <0.05) is shown, so that the linseed oil emulsion disclosed by the invention can play a better role in protecting the linolenic acid compared with a linseed oil pure oil system.
The tests for the ability of the linseed oil emulsion and the high internal phase emulsion prepared in this example to resist environmental changes were as follows:
the linseed oil emulsion and the high internal phase emulsion prepared in the embodiment and the linseed oil emulsion prepared in the comparative example (the preparation method is the same as the embodiment, except that the pH value is not adjusted in the step 3) have the stability under the experiments of different pH conditions (3-9), different ionic strength conditions (0.1-0.5 mol/L sodium chloride solution and calcium chloride solution), sterilization (sterilization at 121 ℃ for 15min in an autoclave) and freezing-unfreezing (freezing at-20 ℃ for 24h, and then standing at room temperature for 12h as a cycle, and 3 times of cycle), and the experimental results show that: in the comparative example, the protein-polysaccharide emulsion was still susceptible to pH due to the fact that the emulsifier contained protein, and an unstable phenomenon occurred in the vicinity of the isoelectric point. The linseed oil emulsion and the high internal phase emulsion prepared by the invention are near the isoelectric point (pH 3-4), the charges of the protein are converted from negative charges to positive charges to form a complex with the polysaccharide, the instability of the emulsion is avoided, the linseed oil emulsion has stronger capability of resisting environmental change, and better stability can be maintained in the process treatments of wider pH range, larger ionic strength, sterilization, freeze thawing and the like.
Example 2 preparation of linseed oil emulsion and high internal phase emulsion
1) Preparation of wall material and core material
Chondroitin sulfate and lactalbumin are used as an emulsifying wall material, and linseed oil is used as a core material;
preparing 0.7% chondroitin sulfate aqueous solution with negative electricity;
preparing a 0.3% whey protein aqueous solution, wherein the solution is negatively charged.
2) Preparation of the crude emulsion
Adding 100mL of the chondroitin sulfate aqueous solution prepared in the step 1) and 100mL of the whey protein aqueous solution into 100mL of linseed oil (wherein the mass ratio of the chondroitin sulfate to the whey protein is 7: 3). The mixture was sheared at high speed of 15000rpm for 1.5min using a high speed shear to give a crude emulsion.
3) Preparation of the emulsion
And (3) carrying out secondary homogenization on the coarse emulsion by using a high-pressure homogenizer, wherein the primary homogenization pressure is 300bar, and the secondary homogenization pressure is 60 bar. After homogenization, the pH is adjusted to 3-4 with 10% citric acid solution under continuous stirring to obtain the final emulsion (i.e. linseed oil emulsion).
4) Preparation of high internal phase emulsions
The final emulsion prepared was centrifuged at 5000g for 5min to give a high internal phase emulsion which exhibited a cream structure.
The mean particle size of the linseed oil emulsion prepared in this example was 107.5 ± 3.2 nm.
The storage stability of the linseed oil emulsion prepared in this example was tested as follows:
the linolenic acid content of the linseed oil emulsion prepared in the embodiment is respectively reduced by 2.22% and 16.81% after being stored for 20 days at 4 ℃ and 25 ℃; and the linolenic acid content of the linseed oil is respectively reduced by 7.8 percent and 26.7 percent after the linseed oil is respectively stored for 20 days at the temperature of 4 ℃ and 25 ℃, and the obvious difference between the linolenic acid content and the linolenic acid content (P <0.05) is shown, so that the linseed oil emulsion phase can play a better role in protecting the linolenic acid compared with a linseed oil pure oil system.
The tests for the ability of the linseed oil emulsion and the high internal phase emulsion prepared in this example to resist environmental changes were as follows:
the linseed oil emulsion and the high internal phase emulsion prepared in the embodiment and the linseed oil emulsion prepared in the comparative example (the preparation method is the same as the embodiment, except that the pH value is not adjusted in the step 3) have the stability under the experiments of different pH conditions (3-9), different ionic strength conditions (0.1-0.5 mol/L sodium chloride solution and calcium chloride solution), sterilization (sterilization at 121 ℃ for 15min in an autoclave) and freezing-unfreezing (freezing at-20 ℃ for 24h, and then standing at room temperature for 12h as a cycle, and 3 times of cycle), and the experimental results show that: in the comparative example, the protein-polysaccharide emulsion was still susceptible to pH due to the fact that the emulsifier contained protein, and an unstable phenomenon occurred in the vicinity of the isoelectric point. The linseed oil emulsion and the high internal phase emulsion prepared by the invention are near the isoelectric point (pH 3-4), the charges of the protein are converted from negative charges to positive charges to form a complex with the polysaccharide, the instability of the emulsion is avoided, the linseed oil emulsion has stronger capability of resisting environmental change, and better stability can be maintained in the process treatments of wider pH range, larger ionic strength, sterilization, freeze thawing and the like.
Example 3 preparation of linseed oil emulsion and high internal phase emulsion
1) Preparation of wall material and core material
Carrageenin and egg white protein are used as emulsification wall materials, and linseed oil is used as a core material;
preparing a carrageenan aqueous solution with the mass concentration of 1.2%, wherein the solution presents negative electricity;
preparing an egg white protein aqueous solution with the mass concentration of 0.8%, wherein the solution presents negative electricity.
2) Preparation of the crude emulsion
Adding 100mL of carrageenan aqueous solution prepared in the step 1) and 100mL of egg white protein aqueous solution into 150mL of linseed oil (wherein the mass ratio of the carrageenan to the egg white protein is 6: 4). The mixture was sheared at 20000rpm for 1min using a high speed shear to give a crude emulsion.
3) Preparation of the emulsion
And (3) carrying out secondary homogenization on the coarse emulsion by using a high-pressure homogenizer, wherein the primary homogenization pressure is 300bar, and the secondary homogenization pressure is 80 bar. After homogenization, the pH is adjusted to 3-4 with 10% acetic acid solution under continuous stirring to obtain the final emulsion (i.e. linseed oil emulsion).
4) Preparation of high internal phase emulsions
The final emulsion prepared was centrifuged at 15000g for 2min to give a high internal phase emulsion which assumed a cream structure.
The mean particle size of the linseed oil emulsion prepared in this example was 101.5 ± 1.6 nm.
The storage stability of the linseed oil emulsion prepared in this example was tested as follows:
the linolenic acid content of the linseed oil emulsion prepared in the embodiment is respectively reduced by 2.11% and 11.36% after being stored for 20 days at 4 ℃ and 25 ℃; and the linolenic acid content of the linseed oil is respectively reduced by 7.8 percent and 26.7 percent after the linseed oil is respectively stored for 20 days at the temperature of 4 ℃ and 25 ℃, and the obvious difference between the linolenic acid content and the linolenic acid content (P <0.05) is shown, so that the linseed oil emulsion phase can play a better role in protecting the linolenic acid compared with a linseed oil pure oil system.
Example 4 preparation of linseed oil emulsions and high internal phase emulsions
1) Preparation of wall material and core material
Carrageenin and egg white protein are used as emulsification wall materials, and linseed oil is used as a core material;
preparing a carrageenan aqueous solution with the mass concentration of 3%, wherein the solution presents negative electricity;
preparing an egg white protein aqueous solution with the mass concentration of 2%, wherein the solution presents negative electricity.
2) Preparation of the crude emulsion
Taking 100mL of carrageenan aqueous solution prepared in the step 1) and 100mL of egg white protein aqueous solution, adding 100mL of linseed oil (wherein the mass ratio of carrageenan to egg white protein is 6:4) for ultrasonic emulsification, wherein the ultrasonic emulsification conditions are as follows: immersing an ultrasonic probe into the mixture, and carrying out ultrasonic treatment for 2min under the condition of 450W; wherein, the ultrasound is carried out for 5s, and the operation is stopped for 2 s.
3) Preparation of the emulsion
And (3) carrying out secondary homogenization on the coarse emulsion by using a high-pressure homogenizer, wherein the primary homogenization pressure is 250bar, and the secondary homogenization pressure is 80 bar. After homogenization, the pH is adjusted to 3-4 with 10% acetic acid solution under continuous stirring to obtain the final emulsion (i.e. linseed oil emulsion).
4) Preparation of high internal phase emulsions
The final emulsion prepared was centrifuged at 15000g for 2min to give a high internal phase emulsion which assumed a cream structure.
The mean particle size of the linseed oil emulsion prepared in this example was 93.5 ± 2.3 nm.
The storage stability of the linseed oil emulsion prepared in this example was tested as follows:
the linolenic acid content of the linseed oil emulsion prepared in the embodiment is respectively reduced by 4.89% and 19.63% after being stored for 20 days at 4 ℃ and 25 ℃; and the linolenic acid content of the linseed oil is respectively reduced by 7.8 percent and 26.7 percent after the linseed oil is respectively stored for 20 days at the temperature of 4 ℃ and 25 ℃, and the obvious difference between the linolenic acid content and the linolenic acid content (P <0.05) is shown, so that the linseed oil emulsion phase can play a better role in protecting the linolenic acid compared with a linseed oil pure oil system.
Example 5 preparation of linseed oil emulsion and high internal phase emulsion
1) Preparation of wall material and core material
Carrageenin and egg white protein are used as emulsification wall materials, and linseed oil is used as a core material;
preparing a carrageenan aqueous solution with the mass concentration of 1.4%, wherein the solution presents negative electricity;
preparing an egg white protein aqueous solution with the mass concentration of 0.6%, wherein the solution presents negative electricity.
2) Preparation of the crude emulsion
Taking 100mL of carrageenan aqueous solution prepared in the step 1) and 100mL of egg white protein aqueous solution, adding 150mL of linseed oil (wherein the mass ratio of carrageenan to egg white protein is 7:3) for ultrasonic emulsification, wherein the ultrasonic emulsification conditions are as follows: immersing an ultrasonic probe into the mixture, and carrying out ultrasonic treatment for 3min under the condition of 400W; wherein, the ultrasound is carried out for 5s, and the operation is stopped for 2 s.
3) Preparation of the emulsion
And (3) carrying out secondary homogenization on the coarse emulsion by using a high-pressure homogenizer, wherein the primary homogenization pressure is 350bar, and the secondary homogenization pressure is 50 bar. After homogenization, the pH is adjusted to 3-4 with 10% acetic acid solution under continuous stirring to obtain the final emulsion (i.e. linseed oil emulsion).
4) Preparation of high internal phase emulsions
The final emulsion prepared was centrifuged at 10000g for 2min to give a high internal phase emulsion which exhibited a cream like structure.
The mean particle size of the linseed oil emulsion prepared in this example was 91.5 ± 3.1 nm.
The storage stability of the linseed oil emulsion prepared in this example was tested as follows:
the linolenic acid content of the linseed oil emulsion prepared in the embodiment is respectively reduced by 4.26% and 18.52% after being stored for 20 days at 4 ℃ and 25 ℃; and the linolenic acid content of the linseed oil is respectively reduced by 7.8 percent and 26.7 percent after the linseed oil is respectively stored for 20 days at the temperature of 4 ℃ and 25 ℃, and the obvious difference between the linolenic acid content and the linolenic acid content (P <0.05) is shown, so that the linseed oil emulsion phase can play a better role in protecting the linolenic acid compared with a linseed oil pure oil system.
Example 6 preparation of linseed oil emulsion and high internal phase emulsion
1) Preparation of wall material and core material
Chondroitin sulfate and lactalbumin are used as an emulsifying wall material, and linseed oil is used as a core material;
preparing a 1.8% chondroitin sulfate aqueous solution with a mass concentration, wherein the solution presents negative electricity;
preparing a whey protein aqueous solution with the mass concentration of 1.2%, wherein the solution presents negative electricity.
2) Preparation of the crude emulsion
Adding 100mL of the chondroitin sulfate aqueous solution prepared in the step 1) and 100mL of the whey protein aqueous solution into 150mL of linseed oil (wherein the mass ratio of the chondroitin sulfate to the whey protein is 6: 4). The mixture was sheared at high speed of 15000rpm for 1.5min using a high speed shear to give a crude emulsion.
3) Preparation of the emulsion
And (3) carrying out secondary homogenization on the coarse emulsion by using a high-pressure homogenizer, wherein the primary homogenization pressure is 350bar, and the secondary homogenization pressure is 50 bar. After homogenization, the pH is adjusted to 3-4 with 10% citric acid solution under continuous stirring to obtain the final emulsion (i.e. linseed oil emulsion).
4) Preparation of high internal phase emulsions
The final emulsion prepared was centrifuged at 15000g for 2min to give a high internal phase emulsion which assumed a cream structure.
The mean particle size of the linseed oil emulsion prepared in this example was 103.2 ± 2.9 nm.
The storage stability of the linseed oil emulsion prepared in this example was tested as follows:
the linolenic acid content of the linseed oil emulsion prepared in the embodiment is respectively reduced by 2.35% and 15.72% after being stored for 20 days at 4 ℃ and 25 ℃; and the linolenic acid content of the linseed oil is respectively reduced by 7.8 percent and 26.7 percent after the linseed oil is respectively stored for 20 days at the temperature of 4 ℃ and 25 ℃, and the obvious difference between the linolenic acid content and the linolenic acid content (P <0.05) is shown, so that the linseed oil emulsion phase can play a better role in protecting the linolenic acid compared with a linseed oil pure oil system.
Example 7 examination of the ratio of carrageenan to egg white protein
Compounding carrageenan and egg white protein in different proportions to prepare a linseed oil emulsion; the mass ratios of carrageenan and egg white protein in example 1 are respectively replaced by 1:9, 2:8, 3:7, 4:6, 5:5, 6:4, 7:3, 8:2 and 9:1, and the other preparation methods are the same as example 1.
The results are shown in FIG. 1. As shown in figure 1, the preferred mass ratio of the carrageenan to the egg white protein is (1.5-9):1, and the optimal mass ratio is 6: 4.
Claims (10)
1. A preparation method of grease or compound emulsion thereof comprises the following steps:
1) preparation of wall material and core material
Polysaccharide and protein are used as emulsification wall materials, and grease or a compound of the grease and a fat-soluble component is used as a core material;
preparing a polysaccharide solution, wherein the polysaccharide is negatively charged;
preparing a protein solution, wherein the protein is negatively charged protein;
2) preparation of the crude solution
Adding the polysaccharide solution and the protein solution into the grease or the compound, and performing high-speed shearing or ultrasonic emulsification to obtain a coarse emulsion;
3) preparation of the emulsion
And (3) homogenizing the crude emulsion at high pressure, and adjusting the pH of the system to 3-4 by adopting acid under the condition of continuously stirring after the high-pressure homogenization is finished to obtain the grease or the compound emulsion thereof.
2. The method of claim 1, wherein: in the step 1), the mass concentration of the polysaccharide in the polysaccharide solution is 0.5-10%;
the polysaccharide is selected from one or two of carrageenan and chondroitin sulfate.
3. The production method according to claim 1 or 2, characterized in that: in the step 1), the mass concentration of the protein in the protein solution is 0.3-10%;
the protein is selected from one or more of whey protein, bovine serum albumin, casein and egg white protein.
4. The production method according to any one of claims 1 to 3, characterized in that: in the step 1), the oil is at least one selected from linseed oil, peony seed oil, grape seed oil, rose seed oil, coconut oil, camellia oil, peanut oil, germ oil, walnut oil, sesame oil, sunflower seed oil, canola oil, olive oil, tomato seed oil, rapeseed oil, deep sea fish oil, cumin oil, capsicum seed oil, garlic oil and ginger oil.
5. The production method according to any one of claims 1 to 4, characterized in that: in the step 2), the mass ratio of the polysaccharide in the polysaccharide solution to the protein in the protein solution is (1.5-9) to 1;
the volume ratio of the polysaccharide solution, the protein solution, the grease or the compound is (10-20) mL: (10-20) mL: (10-15) mL;
the high-speed shearing is carried out by adopting a high-speed shearing machine, and the high-speed shearing condition is that the high-speed shearing is carried out for 1-3min at 5000-20000 rpm;
the conditions of the ultrasonic emulsification are as follows: immersing an ultrasonic probe into the mixture, and carrying out ultrasonic treatment for 1-3min under the conditions of 300-450W; wherein, the ultrasonic treatment is carried out for 2-10s, and the ultrasonic treatment is stopped for 1-3 s.
6. The production method according to any one of claims 1 to 5, characterized in that: in the step 3), the high-pressure homogenization comprises primary homogenization and secondary homogenization;
the pressure of the primary homogenizing is 250-350 bar; the pressure of the secondary homogenization is 40-80 bar;
the acid is 10% acetic acid solution or citric acid solution.
7. An emulsion of a fat or oil or a combination thereof prepared by the method of any one of claims 1 to 6.
8. A preparation method of a high internal phase emulsion of grease or a compound thereof comprises the following steps: centrifuging the grease or the compound emulsion thereof according to claim 7 to obtain the grease or the compound high internal phase emulsion thereof.
9. The method of claim 8, wherein: the centrifugation conditions were: centrifugation was carried out at 1000-15000g for 1-5 min.
10. A linseed oil or a compound high internal phase emulsion thereof produced by the method of claim 8 or 9.
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