CN113208097B - Fish skin gelatin emulsion stabilized by sodium alginate and corn starch and preparation method thereof - Google Patents
Fish skin gelatin emulsion stabilized by sodium alginate and corn starch and preparation method thereof Download PDFInfo
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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
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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
- A23L2/00—Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
- A23L2/52—Adding ingredients
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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
- A23L2/00—Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
- A23L2/52—Adding ingredients
- A23L2/62—Clouding agents; Agents to improve the cloud-stability
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- 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
- A23L2/00—Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
- A23L2/52—Adding ingredients
- A23L2/66—Proteins
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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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- 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
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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
- A23L29/20—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
- A23L29/256—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin from seaweeds, e.g. alginates, agar or carrageenan
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- A—HUMAN NECESSITIES
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- 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
- A23L29/275—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of animal origin, e.g. chitin
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Abstract
A fish skin gelatin emulsion stabilized by sodium alginate and corn starch and a preparation method thereof belong to the technical field of emulsion preparation. Firstly, mixing sodium alginate and corn starch, dissolving the mixture in deionized water, carrying out water bath reaction, and cooling to room temperature to obtain a biopolymer stabilizer; then, the fish Pi Ming is peptized in a stabilizer to prepare a water phase, and fat-soluble active substances are added into the corn oil to serve as an oil phase; mixing the water phase and the oil phase, and then dispersing at high speed and homogenizing at high pressure to obtain the fishskin gelatin emulsion with stable sodium alginate and corn starch. Compared with the emulsion prepared by using the fishskin gelatin under the same condition, the emulsion prepared by the invention is an oil-in-water delivery system with low cost, safety, convenience, higher BITC embedding rate and bioavailability and better storage stability, and has great potential in developing products such as health-care food, functional beverage and the like.
Description
Technical Field
The invention belongs to the technical field of emulsion preparation, and particularly relates to a fish skin gelatin emulsion stabilized by sodium alginate and corn starch and a preparation method thereof.
Background
Fat-soluble active substances such as n-3 polyunsaturated fatty acid, fat-soluble vitamins, plant sterols and the like have high utilization value, but most of the fat-soluble active substances have the defects of poor water solubility, easiness in oxidative degradation, low bioavailability and the like, so that the application of the fat-soluble active substances in the food field is greatly limited. How to introduce fat-soluble active substances into food systems becomes a key element in the development of new functional foods. Embedding the fat-soluble active substances by adopting an O/W type emulsion system can effectively protect the fat-soluble active substances, and can improve the bioavailability of the fat-soluble active substances by changing the composition and structure of the emulsion.
An O/W emulsion is a heterogeneous liquid dispersion in which one liquid is dispersed in the form of droplets (dispersed phase, i.e., oil phase) in another liquid that is immiscible therewith (continuous phase, i.e., aqueous phase). At this time, the interfacial area is increased sharply, the free energy of the system is increased, a thermodynamically unstable system is formed, and a surfactant must be added to reduce the free energy of the system. The protein is a macromolecular surfactant, contains hydrophilic and lipophilic groups, can be adsorbed on an interface and is directionally arranged to form an interface adsorption layer, so that the system energy is reduced, and the stability of a dispersion system is improved. The fishskin gelatin is high-quality marine protein with relatively high molecular weight, is obtained by hydrolyzing collagen of aquatic fishes, is a byproduct in the fishery processing process, is abundant and economic in raw material acquisition, and has extremely high utilization value. Meanwhile, the fishskin gelatin has high surface activity, can form positively charged droplets, and is widely used as an emulsifier in the food industry. Polysaccharides are also a common emulsifier whose emulsion can be stably present under various environmental conditions. The combination of protein and polysaccharide can increase emulsion stability and bioavailability of fat-soluble actives compared to emulsions stabilized with protein alone. Sodium alginate is a natural anionic linear polysaccharide extracted from brown algae or gulfweed, has thickening, emulsifying and gelling properties, and is widely applied to the food, medicine and pharmaceutical industries. The sodium alginate has pH responsiveness, the molecular skeleton is contracted in an acidic environment, the pore diameter is reduced, the molecular skeleton is opened in a neutral or alkaline environment, and the molecular structure is stretched to enlarge the surface pore diameter, so that the release process of the carried substance can be controlled, and the bioavailability of the carrier substance is improved. Corn starch is a processed product of corn, the surface of the corn is easy to be subjected to physicochemical modification, the miscibility between the water phase and the oil phase is facilitated, the stability of emulsion is improved, and the corn starch serving as a stabilizer is widely applied to the field of food.
Disclosure of Invention
The invention provides a preparation method of a fish skin gelatin emulsion stabilized by sodium alginate and corn starch by using cold water fish skin gelatin as an emulsifier. According to the invention, the fishskin gelatin is used as an emulsifier, sodium alginate and corn starch are used as stabilizers, corn oil is used as an oil phase carrier, and the fishskin gelatin emulsion which is stabilized by sodium alginate and corn starch and can embed fat-soluble active substances is obtained. Compared with the emulsion prepared by using the fishskin gelatin under the same condition, the emulsion prepared by the invention has better stability and higher embedding rate and bioavailability of the fat-soluble active substances.
The invention relates to a preparation method of a fish skin gelatin emulsion with stable sodium alginate and corn starch, which comprises the following steps:
s1, preparing a biopolymer stabilizer: mixing sodium alginate and corn starch, dissolving the mixture in deionized water, wherein the mass concentration of the sodium alginate is 0.125-0.25%, the mass concentration of the corn starch is 0.1-0.3%, carrying out water bath reaction at 85-95 ℃, and then cooling to room temperature to obtain a biopolymer stabilizer;
s2, preparing a water phase: dissolving fish Pi Ming in the biopolymer stabilizer prepared in the step S1 to prepare an aqueous phase;
s3, preparing an oil phase: weighing corn oil, and adding fat-soluble active substances (such as benzyl isothiocyanate) into the corn oil as an oil phase, wherein the mass concentration of the fat-soluble active substances is 0-5 mg/mL; the fat-soluble active substances are added into the corn oil and used as an oil phase, so that the stability of the emulsion of the product is not affected;
s4, mixing water phase and oil phase: mixing the oil phase prepared in the step S3 with the water phase prepared in the step S2, wherein the volume of the oil phase is 8-15% of that of the water phase, and then dispersing at a high speed;
s5, homogenizing: homogenizing the product obtained in the step S4 under high pressure to obtain the fish skin gelatin emulsion with stable sodium alginate and corn starch.
Further, in the step S1, the water bath reaction time is 15-30 min;
further, in the biopolymer stabilizer in the step S2, the mass concentration of the fishskin gelatin is 1% -3%;
further, the high-speed dispersion condition in the step S4 is 10000-15000 r/min for 2-3 min;
further, the oil phase in step S4 has the best effect when the volume of the oil phase is 10% of that of the water phase;
further, the conditions of high pressure homogenization in step S5 are 10000 to 12000psi (psi: pounds per square foot) for 5 to 7 times.
The beneficial effects of the invention are as follows:
the invention adopts fish-derived protein as the emulsifier, which can effectively solve the problems of infectious disease (mad cow disease) infection, religious belief and the like related to other mammal-derived gelatin. The biopolymers of sodium alginate and corn starch can play respective roles as stabilizers: corn starch is mixed and dissolved in an oil-water interface, so that the stability of the emulsion is improved, the pH response characteristic of sodium alginate inhibits the degradation of the fat-soluble active substances embedded in the emulsion in the digestion process, and the bioavailability of the fat-soluble active substances is improved. The corn oil is used as an oil phase carrier, and the raw materials are easy to obtain, safe and convenient. The preparation method is simple and easy to implement, and compared with the pure fish skin gelatin, the emulsion prepared by the method has high absolute value of electric potential, and the cold field scanning electron microscope shows that the emulsion has uniform structure distribution. Taking fat-soluble active substance Benzyl Isothiocyanate (BITC) as an example, compared with emulsion prepared by using fishskin gelatin under the same condition, the emulsion prepared by the invention has the advantages of low cost, safety, convenience, higher BITC embedding rate and bioavailability, better storage stability and great potential in developing products such as health food, functional beverage and the like.
The invention uses fish skin gelatin as an emulsifier and biological polymers of sodium alginate and corn starch as a stabilizer to obtain stable emulsion; the stabilizing effect of the corn starch in the storage process and the protecting effect of the sodium alginate on the emulsion in the digestion process are exerted, and compared with the pure fishskin gelatin emulsion, the stability of the emulsion and the embedding rate and the retention rate of fat-soluble active substances are improved, so that the product has higher efficacy value. The emulsion prepared by the invention has small average particle size, high absolute value of electromotive potential and even spatial structure distribution as shown by a cold field scanning electron microscope image, has better stability, and can be used as an effective embedding system of fat-soluble active substances to be applied to the field of foods.
Drawings
FIG. 1 is a graph showing the particle size change between the emulsion products prepared in examples 1-4 of the present invention and the emulsion of the control group of pure fish skin gelatin after storage at 4℃for 0-14 days;
FIG. 2 is a graph showing the potential change between the emulsions of the products prepared in examples 1 to 4 of the present invention and the emulsion of the control group of pure fish skin gelatin (g) stored at 4℃for 0 to 14 days;
FIG. 3 is the appearance of the product emulsions prepared in examples 1 to 4 of the present invention and the pure fish skin gelatin control emulsion (comparative example 1) stored at 4℃for day 0;
FIG. 4 is the appearance of the product emulsions prepared in examples 1 to 4 of the present invention and the simple fishskin gelatin control emulsion (comparative example 1) stored at 4℃for day 1;
FIG. 5 shows the appearance of the emulsions of the products prepared in examples 1 to 4 of the present invention and the emulsion of the control group of pure fish skin gelatin (comparative example 1) stored at 4℃for 4 days;
FIG. 6 is the appearance of the product emulsions prepared in examples 1 to 4 of the present invention and the pure fish skin gelatin control emulsion (comparative example 1) stored at 4℃for 7 days;
FIG. 7 is a view showing the appearance of the emulsion products prepared in examples 1 to 4 of the present invention and the emulsion of the control group of pure fish skin gelatin (comparative example 1) stored at 4℃for 14 days;
FIG. 8 is a cold field scanning electron microscope image (the inset is a partial enlarged view) of the emulsion of the control group of pure fish skin gelatin of the present invention;
FIG. 9 is a cold field scanning electron microscope image (the inset is a partial enlarged view) of the product emulsion prepared in example 1 of the present invention;
FIG. 10 is a cold field scanning electron microscope image (the inset is a partial enlarged view) of the product emulsion prepared in example 2 of the present invention;
FIG. 11 is a cold field scanning electron microscope image (the inset is a partial enlarged view) of the product emulsion prepared in example 3 of the present invention;
FIG. 12 is a cold field scanning electron microscope image (insert is a partial enlarged view) of the product emulsion prepared in example 4 of the present invention.
FIG. 13 is a graph showing the embedding rate of BITC of the product emulsions prepared in examples 5-8 of the present invention and the emulsion of the pure fish skin gelatin control group;
FIG. 14 is a graph showing the retention of BITC after simulated digestion of the product emulsions prepared in examples 5-8 of the present invention versus the pure fish skin gelatin control emulsion.
Detailed Description
The test methods used in the following examples are conventional methods unless otherwise specified. Materials, reagents and the like used in the examples described below are commercially available unless otherwise specified.
Comparative example 1: control group of pure fishskin gelatin
S1, weighing fish skin gelatin, dissolving in deionized water, and preparing into a water-phase gelatin solution with the mass concentration of the fish skin gelatin of 1 percent for later use;
s2, oil phase preparation: weighing corn oil; dissolving benzyl isothiocyanate in corn oil, and sufficiently shaking to prepare an oil phase with the mass concentration of 5mg/mL of benzyl isothiocyanate for later use;
s3, adding the oil phase obtained in the step S2 into the aqueous phase gelatin solution prepared in the step S1, wherein the volume of the oil phase is 10% of that of the aqueous phase gelatin solution, and then dispersing at a high speed of 10000r/min for 3min;
and S4, homogenizing the product of the step S3 at 12000psi high pressure for 6 times to obtain the emulsion of the pure fish skin gelatin control group.
Example 1
S1, mixing sodium alginate and corn starch, dissolving the mixture in deionized water, wherein the mass concentration of the sodium alginate is 0.125%, the mass concentration of the corn starch is 0.1%, heating to 90 ℃ for water bath reaction for 20min, and cooling to room temperature to obtain a stabilizer;
s2, weighing the fishskin gelatin, dissolving the fishskin gelatin in the stabilizer prepared in the step S1, and preparing an aqueous-phase gelatin solution with the mass concentration of the fishskin gelatin of 1% for later use;
s3, oil phase preparation: weighing corn oil as an oil phase;
s4, adding the oil phase obtained in the step S3 into the aqueous phase gelatin solution prepared in the step S2, wherein the volume of the oil phase is 10% of that of the aqueous phase gelatin solution, and then dispersing at a high speed of 12000r/min for 3min;
and S5, homogenizing the product obtained in the step S4 at 12000psi for 5 times to obtain the fishskin gelatin emulsion stabilized by sodium alginate and corn starch.
Example 2
S1, mixing sodium alginate and corn starch, dissolving the mixture in deionized water, wherein the mass concentration of the sodium alginate is 0.15%, the mass concentration of the corn starch is 0.2%, heating to 90 ℃ for water bath reaction for 20min, and cooling to room temperature to obtain a stabilizer;
s2, weighing the fishskin gelatin, dissolving the fishskin gelatin in the stabilizer prepared in the step S1, and preparing an aqueous-phase gelatin solution with the mass concentration of the fishskin gelatin of 1% for later use;
s3, oil phase preparation: weighing corn oil as an oil phase;
s4, adding the oil phase obtained in the step S3 into the aqueous phase gelatin solution prepared in the step S2, wherein the volume of the oil phase is 10% of that of the aqueous phase gelatin solution, and then dispersing at a high speed of 10000r/min for 3min;
and S5, homogenizing the product obtained in the step S4 at 12000psi for 6 times to obtain the fishskin gelatin emulsion stabilized by sodium alginate and corn starch.
Example 3
S1, mixing sodium alginate and corn starch, dissolving the mixture in deionized water, wherein the mass concentration of the sodium alginate is 0.2% and the mass concentration of the corn starch is 0.3%, heating to 90 ℃ for water bath reaction for 20min, and cooling to room temperature to obtain a stabilizer;
s2, weighing the fishskin gelatin, dissolving the fishskin gelatin in the stabilizer prepared in the step S1, and preparing an aqueous-phase gelatin solution with the mass concentration of the fishskin gelatin of 1% for later use;
s3, oil phase preparation: weighing corn oil as an oil phase;
s4, adding the oil phase obtained in the step S3 into the aqueous phase gelatin solution prepared in the step S2, wherein the volume of the oil phase is 10% of that of the aqueous phase gelatin solution, and then dispersing at a high speed of 15000r/min for 2min;
and S5, homogenizing the product obtained in the step S4 at 12000psi for 5 times to obtain the fishskin gelatin emulsion stabilized by sodium alginate and corn starch.
Example 4
S1, mixing sodium alginate and corn starch, dissolving the mixture in deionized water, wherein the mass concentration of the sodium alginate is 0.25% and the mass concentration of the corn starch is 0.1%, heating to 90 ℃ for water bath reaction for 20min, and cooling to room temperature to obtain a stabilizer;
s2, weighing the fishskin gelatin, dissolving the fishskin gelatin in the stabilizer prepared in the step S1, and preparing an aqueous-phase gelatin solution with the mass concentration of the fishskin gelatin of 1% for later use;
s3, oil phase preparation: weighing corn oil as an oil phase;
s4, adding the oil phase obtained in the step S3 into the aqueous phase gelatin solution prepared in the step S2, wherein the volume of the oil phase is 10% of that of the aqueous phase gelatin solution, and then dispersing for 3min at a high speed of 13000 r/min;
and S5, homogenizing the product obtained in the step S4 at 12000psi for 7 times to obtain the fishskin gelatin emulsion stabilized by sodium alginate and corn starch.
Example 5
S1, mixing sodium alginate and corn starch, dissolving the mixture in deionized water, wherein the mass concentration of the sodium alginate is 0.125%, the mass concentration of the corn starch is 0.1%, heating to 90 ℃ for water bath reaction for 20min, and cooling to room temperature to obtain a stabilizer;
s2, weighing the fishskin gelatin, dissolving the fishskin gelatin in the stabilizer prepared in the step S1, and preparing an aqueous-phase gelatin solution with the mass concentration of the fishskin gelatin of 1% for later use;
s3, oil phase preparation: weighing corn oil; dissolving benzyl isothiocyanate in corn oil, and sufficiently shaking to prepare an oil phase with the mass concentration of 5mg/mL of benzyl isothiocyanate for later use;
s4, adding the oil phase obtained in the step S3 into the aqueous phase gelatin solution prepared in the step S2, wherein the volume of the oil phase is 10% of that of the aqueous phase gelatin solution, and then dispersing at a high speed of 14000r/min for 2min;
and S5, homogenizing the product obtained in the step S4 at 12000psi for 7 times to obtain the fishskin gelatin emulsion stabilized by sodium alginate and corn starch.
Example 6
S1, mixing sodium alginate and corn starch, dissolving the mixture in deionized water, wherein the mass concentration of the sodium alginate is 0.15%, the mass concentration of the corn starch is 0.2%, heating to 90 ℃ for water bath reaction for 20min, and cooling to room temperature to obtain a stabilizer;
s2, weighing the fishskin gelatin, dissolving the fishskin gelatin in the stabilizer prepared in the step S1, and preparing an aqueous-phase gelatin solution with the mass concentration of the fishskin gelatin of 1% for later use;
s3, oil phase preparation: weighing corn oil; dissolving benzyl isothiocyanate in corn oil, and sufficiently shaking to prepare an oil phase with the mass concentration of 5mg/mL of benzyl isothiocyanate for later use;
s4, adding the oil phase obtained in the step S3 into the aqueous phase gelatin solution prepared in the step S2, wherein the volume of the oil phase is 10% of that of the aqueous phase gelatin solution, and then dispersing at a high speed of 11000r/min for 3min;
and S5, homogenizing the product obtained in the step S4 at 12000psi for 7 times to obtain the fishskin gelatin emulsion stabilized by sodium alginate and corn starch.
Example 7
S1, mixing sodium alginate and corn starch, dissolving the mixture in deionized water, wherein the mass concentration of the sodium alginate is 0.2% and the mass concentration of the corn starch is 0.3%, heating to 90 ℃ for water bath reaction for 20min, and cooling to room temperature to obtain a stabilizer;
s2, weighing the fishskin gelatin, dissolving the fishskin gelatin in the stabilizer prepared in the step S1, and preparing an aqueous-phase gelatin solution with the mass concentration of the fishskin gelatin of 1% for later use;
s3, oil phase preparation: weighing corn oil; dissolving benzyl isothiocyanate in corn oil, and sufficiently shaking to prepare an oil phase with the mass concentration of 5mg/mL of benzyl isothiocyanate for later use;
s4, adding the oil phase obtained in the step S3 into the aqueous phase gelatin solution prepared in the step S2, wherein the volume of the oil phase is 10% of that of the aqueous phase gelatin solution, and then dispersing at a high speed of 14000r/min for 3min;
and S5, homogenizing the product obtained in the step S4 at 12000psi for 7 times to obtain the fishskin gelatin emulsion stabilized by sodium alginate and corn starch.
Example 8
S1, mixing sodium alginate and corn starch, dissolving the mixture in deionized water, wherein the mass concentration of the sodium alginate is 0.25% and the mass concentration of the corn starch is 0.1%, heating to 90 ℃ for water bath reaction for 20min, and cooling to room temperature to obtain a stabilizer;
s2, weighing the fishskin gelatin, dissolving the fishskin gelatin in the stabilizer prepared in the step S1, and preparing an aqueous-phase gelatin solution with the mass concentration of the fishskin gelatin of 1% for later use;
s3, oil phase preparation: weighing corn oil; dissolving benzyl isothiocyanate in corn oil, and sufficiently shaking to prepare an oil phase with the mass concentration of 5mg/mL of benzyl isothiocyanate for later use;
s4, adding the oil phase obtained in the step S3 into the aqueous phase gelatin solution prepared in the step S2, wherein the volume of the oil phase is 10% of that of the aqueous phase gelatin solution, and then dispersing at a high speed of 12000r/min for 3min;
and S5, homogenizing the product obtained in the step S4 at 12000psi for 7 times to obtain the fishskin gelatin emulsion stabilized by sodium alginate and corn starch.
Particle size and electrokinetic potential measurements were performed on the product emulsion prepared according to the invention: the product emulsions prepared in examples 1 to 4 were diluted 100 times (stored at 4℃for 0 day, 1 day, 4 days, 7 days and 14 days, respectively), and then subjected to measurement of average particle size, particle size distribution and electromotive potential using a nanoparticle analyzer. The different letters in the data represent significant differences (p < 0.05). Specific analysis and theoretical basis include:
(1) The average grain diameter of the emulsion is nano-scale, and the emulsion is uniformly and stably distributed.
(2) The higher the absolute value of the electromotive force, the more stable the system.
The cold field scanning electron microscope determination is carried out on the product emulsion prepared by the invention: after freezing the sample in liquid nitrogen, sublimation was carried out for 20min at-80 ℃. And then observing the microstructure of the product emulsion by adopting a cold field scanning electron microscope. Specific analysis and theoretical basis include:
(1) The more uniform the emulsion structure of the cold field scanning electron microscope image is, the more stable the system is.
(2) The closer the emulsion structure is connected in the cold field scanning electron microscope, the more stable the system is.
The oil-in-water emulsion system is commonly used for embedding fat-soluble active substances, and BITC is taken as an example for measuring the embedding rate of BITC in the product emulsion prepared by the invention: taking a proper amount of the product emulsion prepared in examples 5-8, extracting the BITC embedded in the emulsion with 1mL of n-hexane and 1mL of methanol, analyzing the BITC content by high performance liquid chromatography, and calculating the embedding rate (%) of the BITC in the emulsion according to a standard curve of the BITC concentration, wherein the embedding rate (%) = of the peak area of the BITC in the emulsion/the peak area of the BITC in the standard substance.
BITC retention determination was performed after digestion of the product emulsion prepared in accordance with the present invention using BITC as an example: the product emulsions prepared in examples 5 to 8 were taken in appropriate amounts for in vitro simulated digestion. The specific steps of in vitro simulated digestion are as follows: an in vitro simulated gastrointestinal tract (GIT) model was constructed consisting of a simulated digestive tract of 3 stages of oral cavity, stomach, small intestine, to simulate the digestive process of an emulsion in vivo. Throughout the digestion, the temperature of all solutions and dispersions was maintained at 37 ℃, and the pH of the samples was adjusted with 1M NaOH or HCl solution.
Simulation of oral digestion phase: mixing 20mL of the emulsion sample preheated at 37 ℃ with 20mL of artificial saliva, adjusting the pH to 6.8, and shaking at a constant temperature of 100rpm/min at 37 ℃ for 10min to simulate oral digestion;
simulation of gastric digestion phase: first, simulated Gastric Fluid (SGF) was prepared by dissolving 2g NaCl with 7mL HCl in 1L distilled water. 20mL of orally digested liquid preheated to 37℃was mixed with 20mL of SGF containing pepsin (3.2 mg/mL) and the pH was adjusted to 2.5. Shaking at constant temperature of 37℃and 100rpm/min for 2 hours to simulate gastric digestion;
simulation of small intestine digestion phase: first, 5.5g CaCl was added 2 A Simulated Intestinal Fluid (SIF) was prepared by dissolving 32.9g NaCl in 1L distilled water. 30mL of the digested liquid was taken in a 100mL beaker, stirred at a constant speed of 100rpm/min in a magnetic stirrer heated at a constant temperature of 37℃and the pH was adjusted to 7.0. To the sample, 1.5mL of SIF and 3.5mL of bile salt (53.6 mg/mL) were added, and the pH was again adjusted to 7.0. Finally, 2.5mL of lipase solution (24 mg/mL) was added to the system, and the pH of the system was maintained at 7.0 by dropping 0.02M NaOH solution into the sample over 2 hours to simulate small intestine digestion.
Taking 1mL of digestive juice after the small intestine digestion stage, extracting BITC in the emulsion by using 1mL of n-hexane and 1mL of methanol, measuring the BITC content by adopting high performance liquid chromatography, and calculating the retention (%) of BITC in the emulsion according to a standard curve of BITC concentration, wherein the retention (%) = the peak area of BITC in the small intestine digestive juice/the peak area of BITC in a standard substance.
The test results are shown in fig. 1-14, and different letters in the data represent significant differences (p < 0.05).
In fig. 1, all samples showed little change in particle size in 14 days of storage, and the simple fish skin gelatin control group showed slightly larger change in particle size than the example group.
In fig. 2, all samples showed no significant change in potential during 14 days of storage, and the absolute value of the potential of the example group was greater than that of the control group of pure fish skin gelatin.
In FIGS. 3 to 7, all samples were stable in storage for 14 days without flocculation.
Fig. 8 to 12 are cold field scanning electron microscope diagrams of a control group and examples 1 to 4 in sequence, and as the concentration of sodium alginate increases, it can be clearly observed that sodium alginate filaments are interwoven on a fish skin gelatin branch structure, so that the stability of the system is increased.
Fig. 13 shows the results of the entrapment rate for all samples, with sodium alginate concentrations of 0.25% and entrapment rates of up to 95.45%, much higher than 68.88% for the control group. Compared with a pure fish skin gelatin control group, the embedding rate of the example group is obviously improved, which indicates that the encapsulation rate of the emulsion is improved by adding sodium alginate and corn starch.
Fig. 14 shows the results of bioavailability of all samples, with sodium alginate concentration of 0.25% and entrapment rate of 90.49% at the highest, far above 80.12% for the control. Illustrating that the examples of the present invention provide better protection of the entrapped fat-soluble active substances during digestion.
Compared with the pure fishskin gelatin emulsion, the emulsion prepared by the invention has higher absolute value of electric potential, and the emulsion structure of the cold field scanning electron microscope image is even and compact. The slightly increased particle size shows that the sodium alginate and the fish skin gelatin are fully compounded at the oil-water interface, and play a role in protecting the digestion process of the emulsion system. Compared with the pure fishskin gelatin emulsion, the embedding rate and the bioavailability of BITC are higher, namely the fishskin gelatin emulsion with stable sodium alginate and corn starch prepared by the invention can be used as a conveying system to improve the utilization rate of embedding substances. The sodium alginate and corn starch stabilized fish skin gelatin emulsion prepared in example 4 has extremely high stability.
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 (4)
1. A preparation method of a fish skin gelatin emulsion with stable sodium alginate and corn starch comprises the following steps:
s1, preparing a biopolymer stabilizer: mixing sodium alginate and corn starch, dissolving the mixture in deionized water, wherein the mass concentration of the sodium alginate is 0.125-0.25%, the mass concentration of the corn starch is 0.1-0.3%, carrying out water bath reaction for 15-30 min at 85-95 ℃, and then cooling to room temperature to obtain a biopolymer stabilizer;
s2, preparing a water phase: dissolving fish Pi Ming in the biopolymer stabilizer prepared in the step S1, wherein the mass concentration of fish skin gelatin in the biopolymer stabilizer is 1% -3%, and preparing into a water phase;
s3, preparing an oil phase: weighing corn oil, and adding fat-soluble active substances into the corn oil as an oil phase, wherein the mass concentration of the fat-soluble active substances is 5mg/mL;
s4, mixing water phase and oil phase: mixing the oil phase prepared in the step S3 with the water phase prepared in the step S2, wherein the volume of the oil phase is 8-15% of that of the water phase, and then dispersing at a high speed for 2-3 min under the condition of 10000-15000 r/min;
s5, homogenizing: homogenizing the product obtained in the step S4 under high pressure for 5-7 times under the condition of 10000-12000 psi to obtain the fishskin gelatin emulsion with stable sodium alginate and corn starch.
2. The method for preparing the sodium alginate and corn starch stabilized fishskin gelatin emulsion as claimed in claim 1, wherein: the fat-soluble active substance in step S3 is benzyl isothiocyanate.
3. The method for preparing the sodium alginate and corn starch stabilized fishskin gelatin emulsion as claimed in claim 1, wherein: the volume of the oil phase in step S4 is 10% of the water phase.
4. A fish skin gelatin emulsion stabilized by sodium alginate and corn starch is characterized in that: is prepared by the method of any one of claims 1-3.
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