CN117137121A - Preparation method of stable emulsion taking fish skin gelatin and pectin as composite carriers - Google Patents
Preparation method of stable emulsion taking fish skin gelatin and pectin as composite carriers Download PDFInfo
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- CN117137121A CN117137121A CN202310978500.1A CN202310978500A CN117137121A CN 117137121 A CN117137121 A CN 117137121A CN 202310978500 A CN202310978500 A CN 202310978500A CN 117137121 A CN117137121 A CN 117137121A
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- skin gelatin
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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
- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
- A23L29/10—Foods or foodstuffs containing additives; Preparation or treatment thereof containing emulsifiers
-
- 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
- A23L29/03—Organic compounds
- A23L29/035—Organic compounds containing oxygen as heteroatom
-
- 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
- A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
- A23L29/206—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
- A23L29/231—Pectin; Derivatives thereof
-
- 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
-
- 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
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Nutrition Science (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Dispersion Chemistry (AREA)
- Mycology (AREA)
- Jellies, Jams, And Syrups (AREA)
Abstract
The invention discloses a carrier stabilized by using fish skin gelatin and pectin as composite emulsifying agents and a preparation method of emulsion, and belongs to the technical field of emulsion preparation. The method of the invention comprises the following steps: s1, preparation of a water phase: respectively dissolving fish skin gelatin and pectin in deionized water to fully dissolve, fully mixing the two, and regulating pH to prepare water phase; s2, preparing an oil phase: adding fat-soluble active substances into corn oil to fully dissolve the active substances, and preparing an oil phase for later use; s3, mixing the oil phase and the water phase, dispersing at high speed, homogenizing, and obtaining the emulsion which is stabilized by taking the fishskin gelatin and the pectin as the composite emulsifier. The invention adopts fish skin gelatin and pectin as composite emulsifying agent, corn oil as oil phase and fat-soluble active substance as embedding material, and the fish skin gelatin and pectin can be encapsulated by emulsion. The invention has simple operation, and the prepared emulsion has good emulsifying activity, emulsifying stability, storage stability and higher capability of protecting active substances.
Description
Technical Field
The invention belongs to the technical field of emulsion preparation, and particularly relates to a preparation method of stable emulsion taking fish skin gelatin and pectin as composite carriers.
Background
The fat-soluble active substances include fat-soluble vitamins, polyunsaturated fatty acids, polyphenols, etc. The fat-soluble active substance has biological activities such as antioxidation and anti-inflammatory which are beneficial to human health, but its application in the food field is limited due to its poor water solubility. The effective means for solving the problem is to embed the fat-soluble active substance by using an oil-in-water (O/W) emulsion, and the oil-in-water emulsion conveying system can well protect the fat-soluble active substance and greatly improve the utilization degree of the organism.
Oil-in-water (O/W) emulsion has wide application, and is suitable for being used as an additive of liquid beverage due to the advantages of good stability, weak light scattering effect and the like. In addition, the emulsion is used as a carrier system for carrying medicines and active ingredients, and has wide application prospect in the fields of nutritional foods, functional foods and the like. Fishskin gelatin is a marine protein of high molecular weight and positive charge, which has a high emulsifying capacity due to its high protein content, and can act as an emulsifier to construct an emulsion delivery system. The fish skin is a main raw material for extracting the fish skin gelatin because of being rich in collagen, and can not involve mad cow disease infection of mammal-derived gelatin. The fishskin gelatin also has excellent properties such as film forming property, gel property, dispersion stability and the like, has high self-nutrition value and is easy to dissolve in water, and can be widely applied to industries such as food, medicines and the like. The polysaccharide is also an emulsifier, and the protein and the polysaccharide are combined through intermolecular forces to prepare emulsion as a composite emulsifier, so that the emulsion emulsifying activity and stability of the emulsion can be improved, the protein is easier to adsorb at an interface, the stability of an emulsion system can be better improved compared with a single emulsifier, and the optimal conveying of active ingredients is realized. Pectin is an anionic polysaccharide rich in D-galacturonic acid and rhamnogalacturonyl, and is mainly derived from a large amount of residue waste meal generated in the processing of apples, oranges and beets. Pectin is widely used in the food industry as a functional food ingredient to provide food nutrition and improve its flavor and texture, as well as to increase system viscosity, improve emulsion stability, etc. The fishskin gelatin-pectin is used as a composite carrier, so that the emulsion stability and the embedding rate of fat-soluble active substances can be improved to a certain extent.
Disclosure of Invention
Technical problems: the invention takes fish skin gelatin as an emulsifying agent and pectin as a stabilizing agent to embed fat-soluble active substances, thus obtaining a stable emulsion which can embed fat-soluble active substances by utilizing molecular acting force between the fish skin gelatin and the pectin to prepare a composite carrier. Compared with the emulsion prepared by the simple fishskin gelatin under the same condition, the emulsion prepared by the invention has better stability and higher embedding rate of the fat-soluble active substances.
The technical scheme is as follows:
the first aim of the invention is to provide a preparation method of a stabilized emulsion taking fish skin gelatin and pectin as composite carriers, which comprises the following steps:
s1, preparation of a water phase: mixing fish skin gelatin solution, pectin solution and a certain amount of water to obtain water phase; wherein the mass ratio of the fish skin gelatin to the pectin in the water phase is 16:1-1:6;
s2, preparing an oil phase: dissolving fat-soluble active substances in corn oil to prepare an oil phase; the mass concentration of the fat-soluble active substances in the oil phase is 2-8 mg/mL;
s3, mixing: mixing the water phase prepared in the step S1 with the oil phase prepared in the step S2, performing high-speed dispersion treatment on the mixture with the volume ratio of the oil phase to the water phase being 1:4-1:15, and homogenizing to obtain the emulsion with the fish skin gelatin and pectin as the composite emulsifier.
In one embodiment of the present invention, in S1, the mass concentration of the fish skin gelatin solution is 1% to 6%.
In one embodiment of the present invention, in S1, the mass concentration of the pectin solution is 1% to 6%.
In one embodiment of the present invention, in S1, the final concentration of the fish skin gelatin in the aqueous phase is 0.5% to 3%.
In one embodiment of the present invention, in S1, the mass ratio of the fish skin gelatin to the pectin in the aqueous phase is more preferably 8:1 to 2:1. Specifically, 8:1, 4:1 and 2:1 are selected.
As an embodiment of the present invention, in S1, adjusting the pH of the aqueous phase to 7 is further included.
In one embodiment of the present invention, the edible oil in the step S2 is corn oil, and the fat-soluble active substance is benzyl isothiocyanate.
As one embodiment of the present invention, the volume ratio of the oil phase to the water phase in the step S3 is 1:10.
As an embodiment of the present invention, the step S3 is high-speed dispersion: 8000-15000 r/min for 1-4 min.
As an embodiment of the present invention, in the step S3, the steps of homogenizing: homogenizing at 8000-14000 psi for 4-8 times.
The invention provides a stable emulsion taking fish skin gelatin and pectin as composite carriers based on the preparation method.
The invention also provides application of the stable emulsion taking the fish skin gelatin and pectin as composite carriers in the field of foods.
The beneficial effects of the invention are as follows:
(1) Under the background of national ocean and national construction, the utilization value of the protein from the aquatic product is fully excavated to become the future development trend, and the emulsion conveying system becomes a research hot spot for improving the bioavailability of the functional active substances. The fish skin gelatin selected by the invention is derived from aquatic fish collagen, has good surface activity and emulsifying property, is a better substitute product of gelatin of mammal (such as pigs, cattle and the like), but the stability of emulsion constructed by single protein is easily affected by environment. Pectin has functional properties such as gelability, emulsifying property, dispersion stability, etc., but its emulsifying ability is limited by its own components (degree of methyl esterification, protein residues, neutral sugar side chains and molecular weight). The composite carrier is prepared by utilizing the interaction of the fish skin gelatin and the pectin, and the composite carrier is used as a composite emulsifier to remarkably improve the emulsifying property and the stability of the emulsion. The emulsion constructed by compounding the fishskin gelatin and pectin has good application prospect. Can be applied to the fields of nutritional food, functional food and the like.
(2) According to the invention, the turbidity of the fish skin gelatin and pectin is smaller at the pH value of 7 (shown in figure 1), a soluble compound is generated, the system is stable, the interfacial stability of the fish skin gelatin and pectin composite carrier is improved at the compounding ratio of 8:1, 4:1 and 2:1 (figures 2-7), and the emulsification activity index and the emulsification stability index of the composite carrier are obviously higher than those of a pure fish skin gelatin solution at 3 compounding ratios (figures 8-9). The average particle size, zeta potential, appearance structure, oil droplet distribution and benzyl isothiocyanate retention of the fish skin gelatin and pectin composite emulsion stored at 4 ℃ for 14 days were determined. The results show that the fish skin gelatin and pectin composite emulsion with the compounding ratio of 8:1, 4:1 and 2:1 has no obvious layering during storage (fig. 12-16), the average particle size is smaller (fig. 10), the Zeta potential change range is smaller in the whole storage process (fig. 11), the emulsion oil drops are uniformly distributed (fig. 17-22) through observation of a fluorescence microscope, the retention rate of benzyl isothiocyanate is higher, and the retention rate is obviously higher than that of a (p < 0.05) pure fish skin gelatin emulsion (43.80 +/-1.33%) (fig. 23), so that the fish skin gelatin and pectin composite emulsion has good storage stability and higher active substance (benzyl isothiocyanate) protective capability under the 3 compounding ratios.
Drawings
FIG. 1 is a graph showing turbidity at various pH values of solutions prepared in examples 1 to 5 according to the present invention;
FIG. 2 is a graph of the measurement of the control group contact angle of the present invention;
FIG. 3 is a graph of the contact angle measurement of example 1 of the present invention;
FIG. 4 is a graph of the contact angle measurement of example 2 of the present invention;
FIG. 5 is a graph of the contact angle measurement of example 3 of the present invention;
FIG. 6 is a graph of the contact angle measurement of example 4 of the present invention;
FIG. 7 is a graph of the contact angle measurement of example 5 of the present invention;
FIG. 8 is a graph showing the emulsion activity of the solutions prepared in examples 1 to 5 of the present invention and the simple fishskin gelatin solution;
FIG. 9 is a graph showing the emulsion stability of the solutions prepared in examples 1 to 5 of the present invention and the simple fishskin gelatin solution;
FIG. 10 is a graph showing the particle size change of the product emulsions prepared in examples 1 to 5 of the present invention and the pure fish skin gelatin control emulsion stored at 4℃for 0, 1, 4, 7, and 14 days;
FIG. 11 is a graph showing the potential change of the product emulsions prepared in examples 1 to 5 of the present invention and the simple fish skin gelatin control emulsion stored at 4℃for 0, 1, 4, 7, and 14 days;
FIG. 12 is a physical diagram of the product emulsions prepared in examples 1 to 5 of the present invention and the pure fish skin gelatin control emulsion stored at 4℃for 0 days;
FIG. 13 is a physical diagram of the product emulsions prepared in examples 1 to 5 of the present invention and a pure fish skin gelatin control emulsion stored at 4℃for 1 day;
FIG. 14 is a physical diagram of the product emulsions prepared in examples 1 to 5 of the present invention and a pure fish skin gelatin control emulsion stored at 4℃for 4 days;
FIG. 15 is a physical diagram of the product emulsions prepared in examples 1 to 5 of the present invention and a pure fish skin gelatin control emulsion stored at 4℃for 7 days;
FIG. 16 is a physical diagram of the product emulsions prepared in examples 1 to 5 of the present invention and a pure fish skin gelatin control emulsion stored at 4℃for 14 days;
FIG. 17 is a fluorescence microscope image of an emulsion prepared in the control of the present invention stored at 4℃for 0 days;
FIG. 18 is a fluorescence microscope image of the emulsion prepared in example 1 of the present invention stored at 4℃for 0 days;
FIG. 19 is a fluorescence microscope image of the emulsion prepared in example 2 of the present invention stored at 4℃for 0 days;
FIG. 20 is a fluorescence microscope image of the emulsion prepared in example 3 of the present invention stored at 4℃for 0 days;
FIG. 21 is a fluorescence microscope image of the emulsion prepared in example 4 of the present invention stored at 4℃for 0 days;
FIG. 22 is a fluorescence microscope image of the emulsion prepared in example 5 of the present invention stored at 4℃for 0 days;
FIG. 23 is a graph showing the entrapment rate of benzyl isothiocyanate in the emulsion of the product prepared in examples 1 to 5 of the present invention and in the emulsion of the control group of pure fish skin gelatin.
Detailed Description
Materials, reagents and the like used in the examples described below are commercially available unless otherwise specified.
Comparative example 1 (simple fishskin gelatin control group)
S1, diluting a fish skin gelatin solution prepared in the earlier stage to enable the mass concentration of the fish skin gelatin solution to be 1%, and stirring the fish skin gelatin solution for 1h by using a magnetic stirrer at normal temperature;
s2, preparing an oil phase: dissolving benzyl isothiocyanate into edible oil to prepare benzyl isothiocyanate-corn oil solution with the mass concentration of 2 mg/mL;
s3, mixing the oil phase prepared in the step S2 with the fishskin gelatin solution prepared in the step S1 according to the volume ratio of 1:10, and dispersing at a high speed of 10000r/min for 2min;
s4, homogenizing at high pressure for 6 times at 12000psi to obtain the emulsion of the pure fish skin gelatin control group.
Example 1
S1, preparing a fish skin gelatin solution with the mass concentration of 2%, and fully stirring for 1h by a magnetic stirrer at normal temperature until the fish skin gelatin solution is completely dissolved. Preparing pectin solution with the mass concentration of 4%, and stirring in a water bath at 60 ℃ until the pectin solution is thoroughly dissolved; the fishskin gelatin, the pectin solution and deionized water are uniformly mixed according to a certain proportion to prepare the fishskin gelatin with the final concentration of 1 percent and the pectin with the final concentration of 0.125 percent, and the pH value of the system is regulated to 7.
S2, preparing an oil phase: dissolving benzyl isothiocyanate into edible oil to prepare benzyl isothiocyanate-corn oil solution with the mass concentration of 3 mg/mL;
s3, mixing the oil phase prepared in the step S2 with the fishskin gelatin solution prepared in the step S1 according to the volume ratio of 1:10, and performing high-speed dispersion at 8000r/min for 2min;
s4, homogenizing at high pressure for 6 times at 8000psi to obtain emulsion with fish skin gelatin and pectin as composite carrier.
Example 2
S1, preparing a fish skin gelatin solution with the mass concentration of 2%, and fully stirring for 1h by a magnetic stirrer at normal temperature until the fish skin gelatin solution is completely dissolved. Preparing pectin solution with the mass concentration of 4%, and stirring in a water bath at 60 ℃ until the pectin solution is thoroughly dissolved; the fishskin gelatin, the pectin solution and deionized water are uniformly mixed according to a certain proportion to prepare the fishskin gelatin with the final concentration of 1 percent and the pectin with the final concentration of 0.25 percent, and the pH value of the system is regulated to 7.
S2, preparing an oil phase: dissolving benzyl isothiocyanate into edible oil to prepare benzyl isothiocyanate-corn oil solution with the mass concentration of 8mg/mL;
s3, mixing the oil phase prepared in the step S2 with the fishskin gelatin solution prepared in the step S1 according to the volume ratio of 1:10, and dispersing at a high speed of 14000r/min for 1min;
s4, homogenizing at high pressure for 4 times at 12000psi to obtain emulsion with fish skin gelatin and pectin as composite carrier.
Example 3
S1, preparing a fish skin gelatin solution with the mass concentration of 2%, and fully stirring for 1h by a magnetic stirrer at normal temperature until the fish skin gelatin solution is completely dissolved. Preparing pectin solution with the mass concentration of 4%, and stirring in a water bath at 60 ℃ until the pectin solution is thoroughly dissolved; the fishskin gelatin, the pectin solution and deionized water are uniformly mixed according to a certain proportion to prepare the fishskin gelatin with the final concentration of 1 percent and the pectin with the final concentration of 0.5 percent, and the pH value of the system is regulated to 7.
S2, preparing an oil phase: dissolving benzyl isothiocyanate into edible oil to prepare benzyl isothiocyanate-corn oil solution with the mass concentration of 5 mg/mL;
s3, mixing the oil phase prepared in the step S2 with the fishskin gelatin solution prepared in the step S1 according to the volume ratio of 1:10, and dispersing at a high speed of 12000r/min for 4min;
s4, homogenizing at high pressure for 8 times at 14000psi to obtain emulsion with fish skin gelatin and pectin as composite carrier.
Example 4
S1, preparing a fish skin gelatin solution with the mass concentration of 2%, and fully stirring for 1h by a magnetic stirrer at normal temperature until the fish skin gelatin solution is completely dissolved. Preparing pectin solution with the mass concentration of 4%, and stirring in a water bath at 60 ℃ until the pectin solution is thoroughly dissolved; the fishskin gelatin, the pectin solution and deionized water are uniformly mixed according to a certain proportion to prepare the fishskin gelatin with the final concentration of 1 percent and the pectin with the final concentration of 1 percent, and the pH value of the system is regulated to 7.
S2, preparing an oil phase: dissolving benzyl isothiocyanate into edible oil to prepare benzyl isothiocyanate-corn oil solution with the mass concentration of 4 mg/mL;
s3, mixing the oil phase prepared in the step S2 with the fishskin gelatin solution prepared in the step S1 according to the volume ratio of 1:10, and dispersing at a high speed of 13000r/min for 1min;
s4, homogenizing at high pressure for 5 times at 10000psi to obtain emulsion taking fish skin gelatin and pectin as composite carriers.
Example 5
S1, preparing a fish skin gelatin solution with the mass concentration of 2%, and fully stirring for 1h by a magnetic stirrer at normal temperature until the fish skin gelatin solution is completely dissolved. Preparing pectin solution with the mass concentration of 4%, and stirring in a water bath at 60 ℃ until the pectin solution is thoroughly dissolved; the fishskin gelatin, the pectin solution and deionized water are uniformly mixed according to a certain proportion to prepare the fishskin gelatin with the final concentration of 1 percent and the pectin with the final concentration of 2 percent, and the pH value of the system is regulated to 7.
S2, preparing an oil phase: dissolving benzyl isothiocyanate into edible oil to prepare benzyl isothiocyanate-corn oil solution with the mass concentration of 7 mg/mL;
s3, mixing the oil phase prepared in the step S2 with the fishskin gelatin solution prepared in the step S1 according to the volume ratio of 1:10, and dispersing at a high speed of 11000r/min for 3min;
s4, homogenizing at high pressure for 7 times at 12000psi to obtain emulsion with fish skin gelatin and pectin as composite carrier.
The testing method comprises the following steps:
turbidity determination of composite systems: the pH values of the solutions prepared in examples 1 to 5 were adjusted with 1mol/L HCl solution and 1mol/L NaOH solution so that the pH value change interval was 2 to 9. The sample was placed in a sample cell with a 1cm optical path, and turbidity of the sample was measured at 600nm using an ultraviolet spectrophotometer. Turbidity (T) definition is calculated by the formula: t= -ln (I/I 0 ) Wherein I is transmitted light intensity, I 0 Is the intensity of the incident light. The specific analysis theory basis is as follows: the complex system has four key pH inflection points: pH value c For soluble complex formation, pH φ1 Is formed into insoluble complex and has pH value opt To achieve maximum turbidity and pH φ2 Is insoluble complex dissociation, wherein the pH is c The corresponding emulsion has low turbidity and stable system.
Determination of contact Angle of Complex System: preparing a circular sample piece with the thickness of 1-2mm from fish skin gelatin and fish skin gelatin-pectin freeze-dried powder samples with different concentrations in a tabletting groove, immersing different sample pieces in corn oil, taking out after full oil bath, placing on a glass slide, slowly dripping ultrapure water on the sample piece after oil bath by adopting a sitting drip method, and quantifying by shooting the included angle between the liquid drop and a plane. The specific analysis theory basis is as follows: the contact angle is a critical value with amphipathy when 90 degrees, the oil-water interface tends to be hydrophobic when the contact angle is larger than the critical value, otherwise, the contact angle tends to be hydrophilic, and the state of the prepared oil-in-water emulsion is the most stable when the contact angle tends to be the critical value.
Determination of emulsion Activity and emulsion stability: respectively taking 30mL of 0.2% (w/v) pure fish skin gelatin control group and solutions prepared in examples 1-5 with different compounding ratios, regulating the pH value of a compound system to 7 by using 1mol/L HCl or 1mol/L NaOH solution, adding 10mL of corn oil into the compound system, performing coarse dispersion on the compound system by using a high-speed dispersion homogenizer, performing high-speed dispersion for 1min at 10000rpm to obtain coarse emulsion of examples 1-5, immediately sucking 50 mu L of emulsion from the bottom of a beaker, adding 0.1% (w/v) sodium dodecyl sulfate solution to dilute 100 times, vibrating to fully mix, and measuring absorbance A of the obtained sample at 500nm 0 . Standing the crude emulsion for 10min, sucking 50 μl of emulsion from the bottom of the beaker again, repeating the above experimental steps, and measuring absorbance of sample A 10 . The emulsification activity index is characterized by EA; the emulsion stability index is characterized by ES, ea=ea= (2×2.303×dil×a 0 )/(c×φ×10000)，ES＝(A 0 ×10)/(A 0 -A 10 ) Wherein dil is the dilution factor (100), c is the initial concentration of protein (g/mL), phi is the fraction of oil used to form the emulsion (0.25), A 0 And A 10 The initial absorbance of the diluted emulsion and the absorbance at 10min, respectively. The different letters in the data represent significant differences (p<0.05). Specific analysis theoretical basis includes:
(1) The greater the emulsifying activity, the more stable the emulsion system.
(1) The greater the emulsion stability, the more stable the emulsion system.
Emulsion particle size and potential determination: and diluting a proper amount of the product emulsion prepared in the examples 1-5 and pure fish skin gelatin control group emulsion (respectively storing for 0 day, 1 day, 4 days, 7 days and 14 days at 4 ℃) by 100 times, and detecting the average particle size and Zeta potential by adopting a nano particle size meter. Different capital letters in the data represent the same day of storage significance differences for different emulsions, and different lowercase letters represent the same day of storage significance differences (p<0.05). Specific analysis and theoretical basis include:
(1) The smaller the average particle size of the emulsion, the more stable the system.
(2) The larger the absolute value of the emulsion potential, the more stable the system.
Emulsion appearance structure observation: and taking a proper amount of the product emulsion prepared in the examples 1-5 and pure fish skin gelatin control group emulsion (respectively storing for 0 day, 1 day, 4 days, 7 days and 14 days at 4 ℃) to observe the appearance structure. The specific analysis basis is as follows: the appearance and the shape of the emulsion are not obviously changed, and the more stable the system is.
Emulsion oil drop distribution observation:taking a proper amount of the product emulsion prepared in examples 1-5 and pure fish skin gelatin control group emulsion (respectively stored for 0 day at 4 ℃), using fish skin gelatin and pectin with fluorescein isothiocyanate marked as wall materials and corn oil with nile red marked as core materials, uniformly mixing dye and emulsion samples in a ratio of 1:25, taking 5 mu L of dyed samples on a glass slide, and obtaining images of the samples through a fluorescence microscope. The specific analysis basis is as follows: the more uniform the oil droplet distribution in the fluorescence microscopy image, the more stable the system.
Benzyl isothiocyanate retention assay: taking a proper amount of the product emulsion prepared in examples 1-5 and storing the emulsion of the pure fish skin gelatin control group at 4 ℃ for 0 day and 14 daysExtracting benzyl isothiocyanate from the emulsion by using normal hexane and methanol, analyzing the content of the benzyl isothiocyanate by adopting high performance liquid chromatography, and calculating the retention rate of the benzyl isothiocyanate in the emulsion according to the positive correlation between the concentration of the benzyl isothiocyanate in the solution and the peak content, wherein the retention rate (%) = the peak area of the benzyl isothiocyanate in the emulsion/the peak area of the benzyl isothiocyanate in the standard substance. Different capital letters in the data represent the difference in significance of the same emulsion for different days of storage, and different lowercase letters represent the difference in significance of the same emulsion for the same days of storage (p<0.05). The specific analysis and theoretical basis are: the higher the embedding rate of the emulsion, the more stable the system.
Analysis of results:
according to the invention, by adopting pure fishskin gelatin as a carrier and adopting fishskin gelatin-pectin composite carriers with different proportions to construct emulsion and embedding benzyl isothiocyanate, the research shows that:
the optimal pH value of the fish skin gelatin and pectin composite carrier under different pH values is analyzed by turbidity. The turbidity of the fish skin gelatin and pectin is smaller at pH 7 (figure 1), a soluble compound appears and has a co-dissolution trend, and the system is stable. The contact angle results show that the addition of pectin can change the oil-water interface adsorption capacity of the system, the amphipathy of the compound system with the compound ratio of 8:1, 4:1 and 2:1 is stronger, the interface stability of the compound system can be improved, and the stability of the prepared oil-in-water emulsion is further improved (figures 2-7). The emulsifying activity and the emulsifying stability are used as indexes to explore the emulsifying performance of the composite carrier of the fishskin gelatin and the pectin. The compound systems with the compounding ratios of 8:1, 4:1 and 2:1 have higher emulsification activity indexes and higher emulsification stability indexes (figures 8-9), and are obviously higher than that of the pure fishskin gelatin solution.
The average particle size, zeta potential, appearance structure and benzyl isothiocyanate retention of the fish skin gelatin and pectin composite emulsion stored at 4℃for 14 days were determined. The results show that the fish skin gelatin and pectin composite emulsion with the compounding ratio of 8:1, 4:1 and 2:1 have no obvious layering during storage (fig. 12-16), after the fish skin gelatin and pectin composite emulsion is stored for 14 days under the condition of 4 ℃, the average particle size of the fish skin gelatin and pectin composite emulsion with the compounding ratio of 8:1, 4:1 and 2:1 is smaller, respectively, 312.73 +/-2.41 nm, 345.2 +/-2.33 nm and 433.33 +/-1.12 nm, the compounding ratio of the fish skin gelatin and pectin composite emulsion is obviously lower than that of (P < 0.05) 1:1 (725.03 +/-10.19 nm) and 1:2 (2309+/-164.68 nm) (fig. 10), the Zeta potential has smaller variation amplitude during the whole storage process (fig. 11), the fish skin gelatin and pectin composite emulsion with the compounding ratio of 8:1, 4:1 and 2:1 are uniformly distributed (fig. 17-22) after the fish skin gelatin composite emulsion is stored for 0 days under the condition of observing 4 ℃, and the three composite emulsion with the compounding ratio of 8:1, 4:1 and 2:1 are respectively, the benzyl isothiocyanate composite emulsion with the three composite emulsion having good storage ratios of (P < 0:1 > +/-0.35.35.35%, 58+/-1.9% -35.44%) and the three composite emulsion having better storage stability of the three composite emulsion (P < 0:1, 58%) (58:0.35:0.35%) (35:0.35:0.35%) and 35.37%) and 35.0.0.0.44% of the composite emulsion).
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should be covered by the protection scope of the present invention by making equivalents and modifications to the technical solution and the inventive concept thereof.
Claims (10)
1. The preparation method of the stable emulsion taking the fishskin gelatin and pectin as the composite carrier is characterized by comprising the following steps:
s1, preparation of a water phase: mixing fish skin gelatin solution, pectin solution and a certain amount of water to obtain water phase; wherein the mass ratio of the fish skin gelatin to the pectin in the water phase is 16:1-1:6;
s2, preparing an oil phase: dissolving fat-soluble active substances in corn oil to prepare an oil phase; the mass concentration of the fat-soluble active substances in the oil phase is 2-8 mg/mL;
s3, mixing: mixing the water phase prepared in the step S1 with the oil phase prepared in the step S2, performing high-speed dispersion treatment on the mixture with the volume ratio of the oil phase to the water phase being 1:4-1:15, and homogenizing to obtain the emulsion with the fish skin gelatin and pectin as the composite emulsifier.
2. The method according to claim 1, wherein in S1, the mass concentration of the fish skin gelatin solution is 1% -6%.
3. The method according to claim 1, wherein in S1, the mass concentration of the pectin solution is 1% to 6%.
4. The method according to claim 1, wherein in S1 the final concentration of fish skin gelatin in the aqueous phase is 0.5% to 3%.
5. The method according to claim 1, wherein in S1 the mass ratio of fish skin gelatin to pectin in the aqueous phase is further preferably 8:1 to 2:1.
6. The method of claim 1, wherein S1 further comprises adjusting the pH of the aqueous phase to 7.
7. The method according to claim 1, wherein the edible oil in step S2 is corn oil and the fat-soluble active substance is benzyl isothiocyanate.
8. The method according to any one of claims 1 to 7, wherein the volume ratio of oil phase to water phase in step S3 is 1:10; the high-speed dispersing condition is 8000-15000 r/min for 1-4 min; homogenizing under 8000-14000 psi for 4-8 times.
9. A stabilized emulsion prepared by the method of any one of claims 1-8, wherein the stabilized emulsion is a composite carrier of fish skin gelatin and pectin.
10. Use of a stabilized emulsion of fish skin gelatin and pectin as a composite carrier as claimed in claim 9 in the food sector.
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