CN111388420B - Preparation method and application of sodium caseinate-polyglycerol fatty acid ester compound - Google Patents

Preparation method and application of sodium caseinate-polyglycerol fatty acid ester compound Download PDF

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CN111388420B
CN111388420B CN202010215488.5A CN202010215488A CN111388420B CN 111388420 B CN111388420 B CN 111388420B CN 202010215488 A CN202010215488 A CN 202010215488A CN 111388420 B CN111388420 B CN 111388420B
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sodium caseinate
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water
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CN111388420A (en
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贺军波
曹蕾
黄双双
韩立娟
张维农
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Wuhan Polytechnic University
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Abstract

The invention discloses a preparation method and application of a sodium caseinate-polyglycerol fatty acid ester compound, and relates to the technical field of food processing. The preparation method of the sodium caseinate-polyglycerol fatty acid ester compound comprises the following steps: mixing sodium caseinate, polyglycerol fatty acid ester and water, and stirring to form sodium caseinate-polyglycerol fatty acid ester complex. The invention changes the surface hydrophilicity of the casein sodium emulsion by the interaction of the polyglycerol fatty acid ester and the casein sodium, thereby enhancing the stability of the casein sodium emulsion.

Description

Preparation method and application of sodium caseinate-polyglycerol fatty acid ester compound
Technical Field
The invention relates to the technical field of food processing, and particularly relates to a preparation method and application of a sodium caseinate-polyglycerol fatty acid ester compound.
Background
The casein sodium is the sodium salt of the highest protein content in the milk, has wide source, low price, safety and no toxicity, and is an important food raw material. The sodium caseinate has certain water solubility and amphiphilic property, can be adsorbed to an oil-water interface to form a stable emulsion, however, the sodium caseinate emulsion is greatly influenced by factors such as pH, ionic strength, temperature and the like, so that the sodium caseinate emulsion cannot be stored for a long time, and the application of the sodium caseinate is limited.
Disclosure of Invention
The invention mainly aims to provide a preparation method and application of a sodium caseinate-polyglycerol fatty acid ester compound, and aims to solve the problem of poor stability of a sodium caseinate emulsion.
In order to achieve the above object, the present invention provides a method for preparing a sodium caseinate-polyglycerin fatty acid ester complex, comprising the following steps:
mixing sodium caseinate, polyglycerol fatty acid ester and water, and stirring to form sodium caseinate-polyglycerol fatty acid ester complex.
Optionally, the mass ratio of the sodium caseinate to the polyglycerol fatty acid ester is 1: 0.5 to 4.
Optionally, the polyglyceryl fatty acid ester comprises one of decaglyceryl monooleate and hexaglyceryl monooleate.
Optionally, the step of mixing and stirring sodium caseinate, polyglycerol fatty acid ester and water to form a sodium caseinate-polyglycerol fatty acid ester complex comprises:
dissolving sodium caseinate in water and adjusting the pH value to 6-7 to obtain a sodium caseinate solution;
dissolving polyglycerol fatty acid ester in water and adjusting the pH value to 6-7 to obtain a polyglycerol fatty acid ester solution;
mixing the sodium caseinate solution and the polyglycerol fatty acid ester solution and stirring until a sodium caseinate-polyglycerol fatty acid ester complex is formed.
Optionally, in the step of dissolving sodium caseinate in water and adjusting the pH to 6-7 to obtain a sodium caseinate solution, the concentration of the sodium caseinate solution is 30-50 mg/mL.
Optionally, in the step of dissolving the polyglycerin fatty acid ester in water and adjusting the pH to 6 to 7 to obtain a polyglycerin fatty acid ester solution, the concentration of the polyglycerin fatty acid ester solution is 20 to 160 mg/mL.
Optionally, the step of mixing and stirring the sodium caseinate solution and the polyglyceryl fatty acid ester solution to form a sodium caseinate-polyglyceryl fatty acid ester complex is performed at 40-100 ℃.
Optionally, the sodium caseinate solution and the polyglycerol fatty acid ester solution are mixed and stirred to form a sodium caseinate-polyglycerol fatty acid ester compound, and the stirring time is 0.8-1.2 hours.
In addition, the invention also provides an application of the sodium caseinate-polyglyceryl fatty acid ester compound in stabilizing an oil-in-water emulsion, wherein the sodium caseinate-polyglyceryl fatty acid ester compound is prepared by the preparation method of the sodium caseinate-polyglyceryl fatty acid ester compound.
In addition, the invention also provides an application of the sodium caseinate-polyglyceryl fatty acid ester compound in delivery of drugs and/or food nutrients, wherein the sodium caseinate-polyglyceryl fatty acid ester compound is prepared by the preparation method of the sodium caseinate-polyglyceryl fatty acid ester compound.
According to the technical scheme provided by the invention, the polyglycerol fatty acid ester with high hydrophilicity is compounded with the sodium caseinate to obtain the stable sodium caseinate-polyglycerol fatty acid ester compound, and the polyglycerol fatty acid ester and the sodium caseinate interact to change the surface hydrophilicity of the sodium caseinate emulsion, so that the stability of the sodium caseinate emulsion is enhanced.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other related drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a graph showing the appearance of aqueous dispersions of sodium caseinate-polyglycerin fatty acid ester complexes prepared in examples 1 to 5;
FIG. 2 is a graph showing the change in fluorescence intensity of aqueous dispersions of sodium caseinate-polyglycerin fatty acid ester complexes prepared in examples 1 to 5;
FIG. 3 is a graph showing the appearance effect of the products of example 9, comparative example 3 and comparative example 4;
FIG. 4 is a confocal microscope photomicrograph of the aqueous dispersion of sodium caseinate-polyglycerin fatty acid ester complex prepared in example 9;
FIG. 5 is a confocal laser scanning confocal micrograph of the sodium caseinate oil-in-water emulsion of comparative example 3;
FIG. 6 is a confocal laser scanning microscope photograph of an aqueous dispersion of the sodium caseinate-polyglycerin fatty acid ester complex prepared in example 4.
The implementation, functional features and advantages of the objects of the present invention will be further explained with reference to the accompanying drawings.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. It is to be understood that the described embodiments are merely a few embodiments of the invention, and not all embodiments.
It should be noted that those whose specific conditions are not specified in the examples were performed according to the conventional conditions or the conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially. In addition, the meaning of "and/or" appearing throughout includes three juxtapositions, exemplified by "A and/or B" including either A or B or both A and B. In addition, technical solutions between various embodiments may be combined with each other, but must be realized by a person skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination should not be considered to exist, and is not within the protection scope of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The sodium caseinate has certain water solubility and amphiphilic property, can be adsorbed to an oil-water interface to form a stable emulsion, however, the sodium caseinate emulsion is greatly influenced by factors such as pH, ionic strength, temperature and the like, so that the sodium caseinate emulsion cannot be stored for a long time, and the application of the sodium caseinate is limited.
In view of the above, the invention provides a preparation method of a sodium caseinate-polyglyceryl fatty acid ester complex, which comprises the following steps:
and step S100, mixing and stirring the casein sodium, the polyglycerol fatty acid ester and the water to form the sodium casein-polyglycerol fatty acid ester compound.
The polyglycerol fatty acid ester is a novel emulsifier which is natural in source, good in biodegradability and high in safety, is a nonionic emulsifier which is synthesized by polyglycerol and fatty acid ester and has excellent properties, has various performances such as good emulsification, dispersion and stability, and can be purchased on the market. In the embodiment, sodium caseinate, polyglycerol fatty acid ester and water are mixed, and the lipophilic of fatty acid and sodium caseinate are subjected to intermolecular interaction to form the aqueous dispersion of the sodium caseinate-polyglycerol fatty acid ester compound. In addition, the preparation method provided by the invention has the advantages of simple process, common required instruments and equipment, easy operation, low energy consumption, high repeatability and easy industrial production when put into production.
Wherein the mass ratio of the casein sodium to the polyglycerol fatty acid ester is 1: 0.5-4, within the range, the sodium caseinate and the polyglycerol fatty acid ester can fully act with each other, and the interference of a stable spatial structure due to excessive polyglycerol fatty acid ester can be avoided, so that the stability of the emulsion is reduced.
In addition, the types of polyglycerin fatty acid esters are various and are influenced by the polymerization degree and fatty acid type of polyglycerin, the hydrophilic-lipophilic balance (HLB) values of different polyglycerin fatty acid esters are greatly different, and the hexa-polyglycerin mono fatty acid ester and deca-polyglycerin mono fatty acid ester have a high HLB value (HLB is more than or equal to 10) and have strong hydrophilicity. In this embodiment, the polyglycerin fatty acid ester may include one of decaglyceryl monooleate and hexaglyceryl monooleate, and decaglyceryl monooleate is preferable.
Specifically, there are various mixing modes of casein sodium, polyglycerol fatty acid ester and water, and casein sodium and polyglycerol fatty acid ester can be added into water; or dissolving sodium caseinate in water, and adding polyglycerol fatty acid ester; the polyglycerol fatty acid ester can be dissolved in water, and sodium caseinate can be added. As a preferred embodiment of the present invention, step S100 may be implemented as follows:
and step S10, dissolving the casein sodium in water and adjusting the pH value to 6-7 to obtain a casein sodium solution.
Wherein the concentration of the casein sodium solution is 30-50 mg/mL, preferably 40 mg/mL.
And step S20, dissolving the polyglycerin fatty acid ester in water and adjusting the pH to 6-7 to obtain a polyglycerin fatty acid ester solution.
Wherein the concentration of the polyglycerin fatty acid ester solution is 20 to 160 mg/mL.
And step S30, mixing and stirring the sodium caseinate solution and the polyglycerol fatty acid ester solution until a sodium caseinate-polyglycerol fatty acid ester compound is formed.
In the embodiment, the sodium caseinate and the polyglycerol fatty acid ester are respectively dissolved in water, the pH value is adjusted to 6-7, and then the sodium caseinate and the polyglycerol fatty acid ester are mixed to form a compound under a neutral condition.
In order to promote the interaction between the sodium caseinate and the polyglycerin fatty acid ester, the step S30 is performed at 40 to 100 ℃, and preferably at 80 ℃.
In addition, the mixing and stirring time can be controlled, and in the embodiment, after the casein sodium solution and the polyglycerol fatty acid ester solution are mixed, the mixture is stirred for 0.8 to 1.2 hours.
In addition, the sodium caseinate-polyglycerin fatty acid ester compound prepared by the preparation method of the sodium caseinate-polyglycerin fatty acid ester compound has high stability in a dispersion liquid formed in water, so the invention also provides an application of the sodium caseinate-polyglycerin fatty acid ester compound in stabilizing an oil-in-water emulsion. Specifically, the sodium caseinate-polyglycerol fatty acid ester complex can be mixed with water to form a dispersion, and then an oil phase is added to the dispersion, so that a uniform and stable oil-in-water nanoemulsion can be formed.
In addition, the invention also provides application of the casein sodium-polyglycerol fatty acid ester compound in delivering medicaments and/or food nutrients. Specifically, the sodium caseinate-polyglycerin fatty acid ester complex can be used as a carrier for delivering drugs and/or food nutrients, and the drugs and/or food nutrients are loaded on the sodium caseinate-polyglycerin fatty acid ester complex or wrapped in the sodium caseinate-polyglycerin fatty acid ester complex and then transported to a target site.
The technical solutions of the present invention are further described in detail below with reference to specific examples and drawings, it should be understood that the following examples are merely illustrative of the present invention and are not intended to limit the present invention.
Example 1
Weighing 1.2g of sodium caseinate, dissolving in 30mL of distilled water to obtain a sodium caseinate solution with the concentration of 40mg/mL, and adjusting the pH to 7.0; 0.6g of decaglycerol monooleate was additionally weighed out and dissolved in 30mL of distilled water to obtain a decaglycerol monooleate solution having a concentration of 20mg/mL, and the pH was adjusted to 7.0. Respectively mixing 1mL of casein sodium solution and 1mL of decaglycerol monooleate solution, and then stirring and reacting at 80 ℃ for 1 hour to obtain the aqueous dispersion of the casein sodium-decaglycerol monooleate complex (wherein the mass ratio of the casein sodium to the decaglycerol monooleate is 2: 1).
Effect verification: the aqueous dispersion of the sodium caseinate-decaglycerol monooleate complex of example 1 was left for 90 days without any particle aggregation and precipitation, indicating that the system had good stability.
Example 2
Weighing 1.2g of sodium caseinate, dissolving in 30mL of distilled water to obtain a sodium caseinate solution with the concentration of 40mg/mL, and adjusting the pH to 7.0; separately, 1.2g of decaglycerol monooleate was dissolved in 30mL of distilled water to obtain a decaglycerol monooleate solution having a concentration of 40mg/mL, and the pH was adjusted to 7.0. Respectively mixing 1mL of sodium caseinate solution and 1mL of decaglycerol monooleate solution, and then stirring and reacting at 80 ℃ for 1 hour to obtain the aqueous dispersion of the sodium caseinate-decaglycerol monooleate complex (wherein the mass ratio of sodium caseinate to decaglycerol monooleate is 1: 1).
Effect verification: the aqueous dispersion of the sodium caseinate-decaglycerol monooleate complex of example 2 was left for 90 days without any particle aggregation and precipitation, indicating that the system had good stability.
Example 3
Weighing 1.2g of sodium caseinate, dissolving in 30mL of distilled water to obtain a sodium caseinate solution with the concentration of 40mg/mL, and adjusting the pH to 7.0; in addition, 2.4g of decaglycerol monooleate was weighed out and dissolved in 30mL of distilled water to obtain a decaglycerol monooleate solution having a concentration of 80mg/mL, and the pH was adjusted to 7.0. Respectively mixing 1mL of sodium caseinate solution and 1mL of decaglycerol monooleate solution, and then stirring and reacting at 80 ℃ for 1 hour to obtain the aqueous dispersion of the sodium caseinate-decaglycerol monooleate complex (wherein the mass ratio of sodium caseinate to decaglycerol monooleate is 1: 2).
Effect verification: the aqueous dispersion of the sodium caseinate-decaglycerol monooleate complex of example 3 was left for 90 days without any particle aggregation and precipitation, indicating that the system had good stability.
Example 4
Weighing 1.2g of sodium caseinate, dissolving in 30mL of distilled water to obtain a sodium caseinate solution with the concentration of 40mg/mL, and adjusting the pH to 7.0; 3.6g of decaglycerol monooleate was further weighed out and dissolved in 30mL of distilled water to obtain a decaglycerol monooleate solution having a concentration of 120mg/mL, and the pH was adjusted to 7.0. Respectively mixing 1mL of sodium caseinate solution and 1mL of decaglycerol monooleate solution, and then stirring and reacting at 80 ℃ for 1 hour to obtain the aqueous dispersion of the sodium caseinate-decaglycerol monooleate complex (wherein the mass ratio of sodium caseinate to decaglycerol monooleate is 1: 3).
Effect verification: the aqueous dispersion of the sodium caseinate-decaglycerol monooleate complex of example 4 was left for 90 days without any particle aggregation and precipitation, indicating that the system had good stability.
Example 5
Weighing 1.2g of sodium caseinate, dissolving in 30mL of distilled water to obtain a sodium caseinate solution with the concentration of 40mg/mL, and adjusting the pH to 7.0; separately, 4.8g of decaglycerol monooleate was dissolved in 30mL of distilled water to give a 160mg/mL decaglycerol monooleate solution, and the pH was adjusted to 7.0. Respectively mixing 1mL of sodium caseinate solution and 1mL of decaglycerol monooleate solution, and then stirring and reacting at 80 ℃ for 1 hour to obtain the aqueous dispersion of the sodium caseinate-decaglycerol monooleate complex (wherein the mass ratio of sodium caseinate to decaglycerol monooleate is 1: 4).
Effect verification: the aqueous dispersion of the sodium caseinate-decaglycerol monooleate complex of example 5 was left for 90 days without any particle aggregation and precipitation, indicating that the system had good stability.
Example 6
Weighing 0.9g of sodium caseinate, dissolving in 30mL of distilled water to obtain a sodium caseinate solution with the concentration of 30mg/mL, and adjusting the pH to 6.8; 3.6g of hexaglycerol monooleate was further weighed out and dissolved in 30mL of distilled water to obtain a solution of hexaglycerol monooleate at a concentration of 120mg/mL, and the pH was adjusted to 6.8. Respectively mixing 1mL of sodium caseinate solution and 1mL of hexaglycerol monooleate solution, and then stirring and reacting at 90 ℃ for 1.1 hours to obtain an aqueous dispersion of a sodium caseinate-hexaglycerol monooleate complex (wherein the mass ratio of sodium caseinate to hexaglycerol monooleate is 1: 4).
Effect verification: the aqueous dispersion of the sodium caseinate-hexaglycerol monooleate complex of example 6 was left for 90 days without any particle aggregation and precipitation, indicating that the system had good stability.
Example 7
Weighing 1.5g of sodium caseinate, dissolving in 30mL of distilled water to obtain a sodium caseinate solution with the concentration of 50mg/mL, and adjusting the pH to 6.0; separately, 1.2g of hexaglycerol monooleate was dissolved in 30mL of distilled water to obtain a solution of hexaglycerol monooleate at a concentration of 40mg/mL, and the pH was adjusted to 6.0. Respectively mixing 1mL of sodium caseinate solution and 1mL of hexaglycerol monooleate solution, and then stirring and reacting at 100 ℃ for 0.8 hour to obtain an aqueous dispersion of a sodium caseinate-hexaglycerol monooleate complex (wherein the mass ratio of sodium caseinate to hexaglycerol monooleate is 1: 1).
Effect verification: the aqueous dispersion of the sodium caseinate-hexaglycerol monooleate complex of example 7 was left for 90 days without any particle aggregation and precipitation, indicating that the system had good stability.
Example 8
Weighing 1.2g of sodium caseinate, dissolving in 30mL of distilled water to obtain a sodium caseinate solution with the concentration of 40mg/mL, and adjusting the pH to 7.0; separately, 4.8g of hexaglycerol monooleate was weighed out and dissolved in 30mL of distilled water to obtain a solution of hexaglycerol monooleate having a concentration of 160mg/mL, and the pH was adjusted to 6.5. Respectively mixing 1mL of sodium caseinate solution and 1mL of hexaglycerol monooleate solution, and then stirring and reacting at 40 ℃ for 1.2 hours to obtain an aqueous dispersion of a sodium caseinate-hexaglycerol monooleate complex (wherein the mass ratio of sodium caseinate to hexaglycerol monooleate is 1: 4).
Effect verification: the aqueous dispersion of the sodium caseinate-hexaglycerol monooleate complex of example 8 was left for 90 days without particle aggregation and precipitation, indicating that the system had good stability.
Example 9
This example is an application example of the aqueous dispersion of the sodium caseinate-decaglycerol monooleate complex obtained in example 2:
adding water to the aqueous dispersion of sodium caseinate-decaglycerol monooleate complex until the final concentration of sodium caseinate reaches 5 mg/mL;
0.4g of soybean oil is weighed and added into the diluted aqueous dispersion of the sodium caseinate-decaglycerol monooleate complex, and then uniform oil-in-water nano emulsion is formed by adopting high-pressure homogenization treatment.
Effect verification: the oil-in-water nanoemulsion of example 9 was not layered after standing for 90 days, indicating that a sodium caseinate-polyglycerin fatty acid ester complex is excellent in emulsifiability.
Example 10
This example is an application example of the aqueous dispersion of the sodium caseinate-decaglycerol monooleate complex obtained in example 2:
adding water to the aqueous dispersion of sodium caseinate-decaglycerol monooleate complex until the final concentration of sodium caseinate reaches 5 mg/mL;
0.2g of vitamin E is weighed and added into the diluted aqueous dispersion of the sodium caseinate-decaglycerol monooleate complex, and then uniform vitamin E nano emulsion is formed by adopting high-pressure homogenization treatment.
Effect verification: the vitamin E nanoemulsion of example 10 showed no delamination after standing for 90 days, indicating that the sodium caseinate-polyglycerol fatty acid ester complex has good stability when used to deliver food nutrients.
Comparative example 1
The procedure was the same as in example 2 except that decaglycerol monooleate was changed to decaglycerol monostearate as compared with example 2.
Effect verification: significant delamination was observed after 7 days of storage of the sample of comparative example 1, indicating poor stability of the system.
Comparative example 2
The procedure was the same as in example 2 except that decaglycerol monooleate was changed to triglycerol monooleate, compared with example 2.
Effect verification: the sample of comparative example 3 was left for 7 days and was found to have particles aggregated and precipitated, indicating that the system was not stable.
Comparative example 3
This comparative example is the first comparative example of example 9: 0.4g of soybean oil was weighed and added to 8mL of 10mg/mL sodium caseinate solution, and then, a sample solution was formed by high pressure homogenization treatment.
Effect verification: the sample solution of comparative example 3 immediately after the end of the treatment showed demixing and failed to form a homogeneous emulsion, indicating that sodium caseinate alone is less emulsifying than the sodium caseinate-decaglycerol monooleate complex.
Comparative example 4
This comparative example is a second comparative example of example 9: 0.4g of soybean oil was weighed and added to 8mL of a 10mg/mL decaglycerol monooleate solution, and then, a sample solution was formed by high-pressure homogenization treatment.
Effect verification: the sample liquid of comparative example 4 immediately after the end of the treatment showed demixing and failed to form a uniform emulsion, indicating that decaglycerol monooleate alone is less emulsifying than the sodium caseinate-decaglycerol monooleate complex.
Performance detection
Pretreatment: the aqueous dispersions of the sodium caseinate-polyglycerin fatty acid ester complexes prepared in examples 1 to 5 were diluted with water, respectively, so that the final concentration of sodium caseinate in the diluted aqueous dispersions of the sodium caseinate-polyglycerin fatty acid ester complexes was 5mg/mL for use.
First, the appearance of the diluted aqueous dispersion of the sodium caseinate-polyglycerin fatty acid ester complex was observed, and as shown in fig. 1, it was found that the aqueous dispersion of the diluted sodium caseinate-polyglycerin fatty acid ester complex according to each example exhibited good uniformity and dispersibility, and the transparency of the dispersion gradually decreased as the content of the polyglycerin fatty acid ester increased.
(II) identification
The change of fluorescence intensity of the diluted aqueous dispersion of the sodium caseinate-polyglycerin fatty acid ester complex was measured using a fluorescence spectrometer, as shown in fig. 2. As can be seen from FIG. 2, the fluorescence intensity of sodium caseinate is decreased with the increase of the content of polyglyceryl fatty acid ester, which indicates that the polyglyceryl fatty acid ester forms a complex with sodium caseinate and changes the spatial structure of sodium caseinate.
(III) particle size, polydispersity index (PDI) and zeta-potential of the diluted aqueous dispersions of sodium caseinate-polyglycerin fatty acid ester complexes according to examples 1 to 5 and the oil-in-water nano-emulsions prepared in example 9 were measured
The detection method comprises the following steps: diluting 100 μ L of sample with distilled water by 80 times, placing into a cuvette, placing the cuvette in a Malvern nanometer particle size analyzer, and setting conditions of room temperature 25 deg.C, water as disperse phase, and preparation time of 60 s. The particle diameter, PDI and zeta potential of the sample were measured in triplicate under these conditions, and the average of the results of the triplicate measurements was taken as the particle diameter, PDI and zeta potential of the sample for measurement and reported in Table 1 below. Wherein, the dilution by 80 times means that the volume ratio of the emulsion to the distilled water is 1: 80; the relative standard deviation between the three measurements should be less than 10% to ensure good reproducibility of the measurements.
TABLE 1 particle size, PDI and zeta potential data for the examples
Figure BDA0002423783320000101
Figure BDA0002423783320000111
As can be seen from table 1 above, the average particle size of the samples prepared in each example can reach nanometer level, the PDI value is very low, and the dispersibility of each sample is excellent, and the stability of the formed sodium caseinate-polyglycerol fatty acid ester complex in water dispersion and oil-in-water emulsion is good.
(IV) stability testing under different pH conditions
The detection method comprises the following steps: the aqueous dispersions of sodium caseinate-polyglycerin fatty acid ester complexes prepared in examples 1 to 5 were placed in buffer solutions having pH of 2, 3, 4, 5, 6, 7, respectively, and then the particle size and PDI were measured, and the results are shown in table 2.
TABLE 2 comparison of stability at different pH
Figure BDA0002423783320000112
Figure BDA0002423783320000121
As can be seen from Table 2 above, the aqueous dispersions of sodium caseinate-polyglycerin fatty acid ester complexes prepared in the examples showed good stability except for the pH of 4. The isoelectric point of sodium caseinate is known to be 4.6, and the stability of sodium caseinate emulsion at pH 5 is poor, while the stability of the aqueous dispersion of the sodium caseinate-polyglycerol fatty acid ester compound prepared by the invention at pH 5 is good, which shows that the interaction between sodium caseinate and polyglycerol fatty acid ester affects the isoelectric point of sodium caseinate, and the stability at pH 5 is better.
(V) stability testing at different salt concentrations
The detection method comprises the following steps: the diluted aqueous dispersions of the sodium caseinate-polyglycerin fatty acid ester complexes corresponding to examples 1 to 5 were placed in 0.05, 0.1, 0.15, 0.3mol/L NaCl solutions, respectively, and then the particle size and PDI were measured, with the results shown in table 3.
TABLE 3 comparison of the stability at different salt concentrations
Figure BDA0002423783320000122
As can be seen from Table 3 above, the aqueous dispersions of sodium caseinate-polyglycerin fatty acid ester complexes prepared in the examples still showed good stability at high salt concentrations. The stability of the sodium caseinate-polyglycerol fatty acid ester compound prepared by the preparation method is not influenced by the salt concentration.
(VI) stability testing under simulated gastrointestinal fluid conditions
Detection method of stability test under simulated gastric fluid conditions:
the diluted aqueous dispersions of the sodium caseinate-polyglycerin fatty acid ester complexes corresponding to examples 1 to 5 were placed in simulated gastric fluid and shaken in a 130r/min water bath at 37 ℃ for 120min (simulating gastric motility in vivo), and the particle size and PDI were measured, with the results shown in table 4.
The preparation method of the simulated gastric juice comprises the following steps: taking 3.84mL of hydrochloric acid, adding 800mL of water and 10g of pepsin, shaking up, and adding water to dilute into 1000mL to obtain the finished product.
The detection method of the stability test under the simulated intestinal fluid condition comprises the following steps:
the diluted aqueous dispersions of the sodium caseinate-polyglycerin fatty acid ester complexes corresponding to examples 1 to 5 were placed in simulated intestinal fluid, and then shaken in a water bath at 37 ℃ and 45r/min for 240min (simulated intestinal motility in vivo), and the particle size and PDI were measured, and the results are shown in table 4.
The preparation method of the simulated intestinal fluid comprises the following steps: taking 6.8g of monopotassium phosphate, adding 500mL of water for dissolving, and adjusting the pH value to 6.8 by using 0.1mol/L sodium hydroxide solution; dissolving pancreatin 10g in water, mixing the two solutions, and diluting to 1000 mL.
TABLE 4 stability comparison under simulated gastrointestinal fluid conditions
Figure BDA0002423783320000131
As can be seen from the above Table 4, the aqueous dispersion of the sodium caseinate-polyglycerin fatty acid ester complex prepared in each example can maintain high stability in simulated gastric juice environment, and large particles appear in the system in simulated intestinal environment, and PDI is increased, which indicates that the aqueous dispersion of the sodium caseinate-polyglycerin fatty acid ester complex is unstable, thus indicating that the aqueous dispersion of the sodium caseinate-polyglycerin fatty acid ester complex can be used for constructing a targeted intestinal delivery system.
(VII) the appearance of the products of example 9, comparative example 3 and comparative example 4 was visually observed as shown in FIG. 3.
Referring to fig. 3, the effect of the products of example 9, comparative example 3 and comparative example 4 is shown from left to right. The sodium caseinate-decaglycerol monooleate complex of example 9 exhibited a good, stable oil-in-water emulsion, whereas both the sodium caseinate oil-in-water emulsion of comparative example 3 and the decaglycerol monooleate oil-in-water emulsion of comparative example 4 exhibited oil phase stratification (the horizontal line marked in the figure is the stratification of the water and oil phases, wherein the upper layer is the oil phase), indicating that the sodium caseinate-decaglycerol monooleate complex has a significantly better ability to emulsify and stabilize the oil phase than the sodium caseinate and decaglycerol monooleate of the individual components.
(eighth) the products of example 9, comparative example 3 and comparative example 4 were observed using a laser scanning confocal microscope, as shown in fig. 4 to 6.
Referring to fig. 4, in the aqueous dispersion of sodium caseinate-decaglycerol monooleate complex of example 9, the soybean oil was uniformly dispersed in the stable oil-in-water emulsion of sodium caseinate-decaglycerol monooleate complex, which had good physical stability; referring to fig. 5 and 6, in the sodium caseinate oil-in-water emulsion of comparative example 3 and the decaglycerol monooleate oil-in-water emulsion of comparative example 4, large oil droplet aggregates appeared, the oil phase was prone to oxgall ripening, and aggregation occurred between oil droplets. The sodium caseinate-decaglycerol monooleate complex is proved to have obviously better capability of stabilizing the oil phase than the sodium caseinate and decaglycerol monooleate which are single components.
The above is only a preferred embodiment of the present invention, and it is not intended to limit the scope of the invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention shall be included in the scope of the present invention.

Claims (6)

1. The preparation method of the sodium caseinate-polyglycerol fatty acid ester compound is characterized by comprising the following steps:
dissolving sodium caseinate in water to obtain a sodium caseinate solution with the concentration of 30-50 mg/mL;
dissolving polyglycerol fatty acid ester in water to obtain a polyglycerol fatty acid ester solution with the concentration of 20-160 mg/mL;
mixing and stirring the sodium caseinate solution and the polyglycerol fatty acid ester solution at 40-100 ℃ to obtain a sodium caseinate-polyglycerol fatty acid ester compound, wherein the sodium caseinate-polyglycerol fatty acid ester compound can form a stable dispersion in water;
wherein the mass ratio of the casein sodium to the polyglycerol fatty acid ester is 1: 0.5-4, wherein the polyglyceryl fatty acid ester is one of decapolyglyceryl monooleate and hexapolyglyceryl monooleate.
2. The method for preparing a sodium caseinate-polyglycerin fatty acid ester complex as claimed in claim 1, wherein the step of dissolving sodium caseinate in water to obtain a sodium caseinate solution with a concentration of 30-50 mg/mL comprises: dissolving sodium caseinate in water and adjusting the pH value to 6-7 to obtain a sodium caseinate solution with the concentration of 30-50 mg/mL.
3. The method for preparing a sodium caseinate-polyglycerin fatty acid ester complex as set forth in claim 1, wherein the step of dissolving the polyglycerin fatty acid ester in water to obtain a polyglycerin fatty acid ester solution having a concentration of 20 to 160mg/mL comprises: dissolving polyglycerol fatty acid ester in water, and adjusting the pH value to 6-7 to obtain a polyglycerol fatty acid ester solution with the concentration of 20-160 mg/mL.
4. The method for preparing a sodium caseinate-polyglycerin fatty acid ester complex as set forth in claim 1, wherein the mixing time of the sodium caseinate solution and the polyglycerin fatty acid ester solution is 0.8 to 1.2 hours in the step of forming the sodium caseinate-polyglycerin fatty acid ester complex.
5. Use of a sodium caseinate-polyglyceryl fatty acid ester complex in the stabilization of an oil-in-water emulsion, wherein the sodium caseinate-polyglyceryl fatty acid ester complex is prepared by the process for the preparation of a sodium caseinate-polyglyceryl fatty acid ester complex as claimed in any of the claims 1 to 4.
6. Use of a sodium caseinate-polyglyceryl fatty acid ester complex in the preparation of a carrier for the delivery of pharmaceutical and/or food nutrients, wherein the sodium caseinate-polyglyceryl fatty acid ester complex is prepared by the method of preparation of a sodium caseinate-polyglyceryl fatty acid ester complex as claimed in any one of claims 1 to 4.
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