CN107410829B - Method for improving emulsification stability of polysaccharide/protein compound - Google Patents
Method for improving emulsification stability of polysaccharide/protein compound Download PDFInfo
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Abstract
The invention discloses a method for improving the emulsification stability of a polysaccharide/protein compound, which solves the problem that the stability of the existing polysaccharide/protein compound needs to be improved. Within a certain pH range, polysaccharides and proteins can form intramolecular complexes which have very excellent emulsifying activity but are sensitive to pH, limiting their range of use. The invention takes polysaccharide/protein compound as an emulsifier, and adopts an emulsification-solvent volatilization method to prepare the polysaccharide/protein compound and fatty acid shell-core structure compound particles. The solvent volatilization method of the invention leads the polysaccharide/protein compound on the fatty acid particle interface to generate interface aggregation, leads the fatty acid particle to generate collapse and shrink, and leads the interface layer to thicken, thus effectively improving the pH stability of the polysaccharide/protein compound, leading the polysaccharide/protein compound to have good gastrointestinal transport characteristics and improving the application value of the polysaccharide/protein electrostatic compound.
Description
Technical Field
The invention relates to a method for improving the emulsification stability of a polysaccharide/protein compound, in particular to a method for preparing a polysaccharide/protein compound and fatty acid shell-core structure compound particle by an emulsification-solvent volatilization method.
Background
Polysaccharides and proteins are the most commonly used emulsifiers in food products and are one of the important factors affecting the physicochemical stability of emulsions. In the oil-in-water type emulsion, protein can be adsorbed on the surface of oil drops to form an interfacial film with certain viscoelasticity, so that emulsion layering caused by aggregation or flocculation of emulsion drops is prevented; while polysaccharides increase the viscosity of the continuous phase, improving emulsion stability by impeding the motion of the emulsion droplets. Therefore, polysaccharide-protein interaction to shape and improve the stability of the polysaccharide-protein interaction is widely applied to food science and biomedicine, and the formed non-covalent electrostatic compound has important biological significance and is easy to use in product formulas, thereby attracting wide attention.
Electrostatic forces are the most dominant driving force for protein and polysaccharide interactions, and at pH values below the isoelectric point of the protein, the protein carries a net positive charge and can form complexes with anionic polysaccharides. Research shows that protein and polysaccharide are combined under the electrostatic action, so that a protein interface layer is protected; the high molecular weight and high hydrophilicity of the polysaccharide enable space repulsion among the emulsion droplets to prevent the coalescence of the emulsion droplets; however, the interaction between protein and polysaccharide is influenced by many factors, such as pH, ionic strength, mixing ratio, etc. For example, soluble intramolecular complexes, soluble intermolecular complexes, insoluble intermolecular complexes, etc. may be formed depending on the mixing ratio of the protein and the polysaccharide.
In the prior art, polysaccharide/protein complexes are researched more, such as hydrogel particles with similar size and functionality to low-calorie starch particles are prepared by utilizing the electrostatic interaction between gelatin and pectin; as in the probiotic microencapsulation technique, the use of polysaccharide-protein complexes improves the activity of probiotics under different stresses; for example, the lycopene micelle is prepared by utilizing the soybean protein isolate/sodium alginate copolymer, so that the problems of poor solubility and stability of the lycopene and the like are solved. The polysaccharide/protein compound has both excellent emulsification activity of protein and space stability of polysaccharide, and effectively improves the stability of food emulsion, but the polysaccharide/protein intramolecular compound is sensitive to pH, and when the pH of an emulsion system changes, the intramolecular compound can be dissociated or precipitated due to agglomeration, so that the stability of the emulsion is reduced, and the application of the polysaccharide/protein intramolecular compound is restricted.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a method for preparing a polysaccharide/protein compound and fatty acid shell-core structure compound particle by using a polysaccharide/protein intramolecular compound as an emulsifier and adopting an emulsification-solvent volatilization method, so as to solve the problem of unstable pH of the existing polysaccharide/protein compound.
A method for improving the emulsification stability of a polysaccharide/protein complex, which is used for preparing a polysaccharide/protein complex and fatty acid shell-core structure complex particle by an emulsification-solvent volatilization method to improve the pH stability of the polysaccharide/protein complex, wherein the emulsification-solvent volatilization method comprises the following steps:
(1) weighing polysaccharide and protein, dissolving in pure water, placing in a roller mixer, mixing at room temperature for 12h to dissolve completely, mixing, adjusting pH to 4.0-4.4, and stirring for 1h to obtain polysaccharide/protein complex with a mass ratio of polysaccharide to protein of 1-2: 2-1.
(2) Preparing 100mg/mL fatty acid ethanol solution, and stirring for 1 h;
(3) slowly dropwise adding the fatty acid ethanol solution obtained in the step (2) into the polysaccharide/protein compound aqueous solution obtained in the step (1) subjected to high-speed shearing and stirring, performing rotary evaporation at 45 ℃ and under 0.1Mpa, and quickly removing ethanol to obtain a fatty acid particle dispersion liquid, wherein the high-speed shearing rotation speed is 20000 rpm/min;
(4) and (4) freeze-drying the fatty acid particle dispersion liquid prepared in the step (3) to obtain the polysaccharide/protein compound and fatty acid shell-core structure compound particles, wherein when the final concentration of the fatty acid particles is 2%, the final concentrations of the polysaccharide/protein intramolecular compound are 0.1%, 0.5%, 1%, 2% and 5%.
Preferably, the method for improving the emulsion stability of the polysaccharide/protein complex comprises the steps of (1) preparing a polysaccharide selected from the group consisting of gum arabic, beet pectin, and soybean polysaccharide, preferably gum arabic; the protein is any one of whey protein isolate, soy protein isolate and casein. .
Preferably, the method for improving the emulsion stability of the polysaccharide/protein complex is as described above, wherein the fatty acid in the step (2) is any one of oleic acid, linolenic acid and conjugated linoleic acid.
Compared with the prior art, the invention has the advantages that: the invention takes polysaccharide/protein compound as an emulsifier, adopts an emulsification-solvent volatilization method to prepare the compound particles with the shell-core structure of the polysaccharide/protein compound and the fatty acid, utilizes the volatilization of solvent ethanol to lead the polysaccharide/protein intramolecular compound on the interface of the fatty acid particle to generate interface aggregation, leads the interface of the fatty acid particle to generate collapse and shrinkage, leads the interface layer to be thickened, effectively improves the pH stability of the polysaccharide/protein intramolecular compound, leads the compound to have good gastrointestinal delivery characteristics of the fatty acid, and improves the application value of the polysaccharide/protein electrostatic compound.
Drawings
FIG. 1 is a graph of average particle size and particle size relationship of GA-WPI GLA particles at different concentrations at a GA/WPI stoichiometric ratio of 2 and pH = 4.4; as can be seen from the graph, the average particle size of the fresh CLA particles tended to decrease and then increase with the increase in the concentration of the GA/WPI intramolecular complex, the particle size of the 0.1% GA/WPI intramolecular complex was larger, the particle size distribution of the CLA particles prepared at the concentration of 0.5-2% was close, and the average particle size reached a constant value, which means that the adsorption of the GA/WPI intramolecular complex at the CLA particle interface had reached saturation. When the concentration was increased to 5%, the average particle diameter showed an increasing tendency, and the CLA particles were slightly flocculated. This is due to the fact that free excess emulsifier in the aqueous phase can lead to particle flocculation due to the emptying effect.
FIG. 2 shows the variation of particle size of GLA microparticles prepared at different concentrations of GA/WPI intramolecular complex when stored at 40 ℃. As can be seen from the figure, the particle size distribution of the CLA particles at each concentration has no obvious change in the storage period of 7d, and the CLA particles prepared from the 5% GA/WPI intramolecular compound have a small amount of particle flocculation along with the prolongation of the storage period, which indicates that the CLA particles have better physical stability.
FIG. 3 a micro-topography of CLA microparticles prepared in 2% GA/WPI intramolecular complex; as can be seen, the CLA particles prepared by the emulsion-solvent evaporation method are distributed uniformly, and the wrinkles on the surfaces of the particles collapse, so that the CLA particles have a thicker interface layer. This is due to the evaporation of the solvent which occurs after emulsification, which causes the escape of the ethanol which is encapsulated inside the CLA particles, causing the collapse and interfacial shrinkage of the circular particles formed by the emulsification.
FIG. 4 is a graph of the lyophilization profile and the reconstituted particle size distribution of CLA microparticles prepared from the GA-WPI intramolecular complex at various concentrations, at a GA/WPI stoichiometric ratio of 2 and a pH = 4.4; as can be seen from the figure, when the concentration of the GA/WPI intramolecular complex is 0.1%, the prepared CLA particles can not be lyophilized basically, the oil yield is serious, and the GA/WPI can not completely coat CLA liquid drops at the interface, so that a large amount of CLA overflows in the lyophilization process; when the concentration of the GA/WPI intramolecular compound is 0.5 percent, the CLA particles are obviously agglomerated after being freeze-dried to form blocks; when the concentration of the GA/WPI intramolecular compound is increased to more than 1 percent, the CLA particles are in a powder shape after being freeze-dried, and the CLA particles prepared from the 5 percent GA/WPI intramolecular compound are in the most fine powder shape and have the best storage dispersibility. The CLA particle powder prepared by freeze-drying is dissolved and reduced to the concentration of a freshly prepared dispersion liquid, and particle size analysis is carried out, so that partial particle aggregation and large particle size are found after the CLA particle powder prepared by 1% of GA/WPI intramolecular compound is redissolved, the particle size distribution of the CLA particle powder prepared by 2% and 5% of GA/WPI intramolecular compound is close to that of the freshly prepared CLA particle powder, and the redissolving effect of the CLA particle powder is good.
Figure 5 graph of particle size variation and CLA release rate in simulated gastrointestinal tract for CLA microparticles prepared in 2% GA/WPI intramolecular complex. As can be seen from the figure, the CLA particles prepared by the emulsion-solvent evaporation method have improved pH stability due to the aggregation of the GA/WPI intramolecular complex at the interface. CLA particles are stable in simulated gastric fluid and basically keep unimodal distribution, and large particle aggregation peaks appear along with the time extension in the simulated gastric fluid, so that the release rate of CLA is slowly increased. Presumably, because the GA/WPI intramolecular complex at the interface of CLA microparticles starts to be gradually enzymolyzed under the action of pepsin, the interface protection barrier of the CLA microparticles is reduced, so that the diffusion rate of CLA to the system is gradually increased, and the release rate reaches 36.0% at 180min of gastric juice. In the simulated intestinal fluid, the large particle aggregation peak of the CLA particles is obviously increased along with the time, the CLA release rate also shows a rapid increasing trend, and the CLA release rate reaches about 62.2 percent at 180 min. The release rate of CLA in simulated intestinal fluid is faster compared to simulated gastric fluid. This is because the CLA microparticles are obviously aggregated in large particles in simulated intestinal fluid, and it is presumed that the bile salt in the small intestine replaces CLA at the microparticle interface, which accelerates the adsorption of trypsin at the interface and the destruction of the protective barrier at the microparticle interface, and the aggregation among the microparticles is relatively more easily occurred, resulting in a significant increase in the CLA release rate.
Detailed Description
In order to clearly illustrate the technical features of the scheme of the invention, the invention is explained below with reference to specific embodiments. The scope of protection of the invention is not limited to these examples. All changes, modifications and equivalents that do not depart from the spirit of the invention are intended to be included within the scope thereof.
Example 1
The polysaccharide is Arabic gum, the protein is whey protein isolate, the fatty acid is conjugated linoleic acid, and the preparation method comprises the following steps:
(1) weighing Arabic gum and whey protein isolate in a mass ratio of 2:1, mixing in a roller mixer at room temperature for 12 hr to dissolve completely, adjusting pH to 4.4, and stirring for 1 hr to obtain polysaccharide/protein complex.
(2) Taking a proper amount of CLA in absolute ethyl alcohol, preparing 100mg/mL CLA ethanol solution, and stirring for 1 h.
(3) Slowly dropwise adding CLA ethanol solution into GA/WPI water solution which is sheared and stirred at a high speed (20000 rpm/min), carrying out rotary evaporation at 45 ℃ and 0.1Mpa, quickly removing ethanol to obtain dispersion of WPI/GA compound and shell-core structure compound particles of conjugated linoleic acid, and freeze-drying a freshly prepared sample to obtain powder WPI/GA compound and shell-core structure compound particles of conjugated linoleic acid. Wherein, based on 100 percent of the total mass of the Conjugated Linoleic Acid (CLA) emulsion, the final concentration of the conjugated linoleic acid is 2 percent, the final concentration of the WPI/GA intramolecular compound is 1 percent, and the balance is water.
Example 2
The polysaccharide is Arabic gum, the protein is whey protein isolate, the fatty acid is conjugated linoleic acid, and the preparation method comprises the following steps:
(1) weighing Arabic gum and whey protein isolate in a mass ratio of 2:1, mixing in a roller mixer at room temperature for 12 hr to dissolve completely, adjusting pH to 4.4, and stirring for 1 hr to obtain polysaccharide/protein complex.
(2) Taking a proper amount of CLA in absolute ethyl alcohol, preparing 100mg/mL CLA ethanol solution, and stirring for 1 h.
(3) Slowly dropwise adding CLA ethanol solution into GA/WPI water solution which is sheared and stirred at a high speed (20000 rpm/min), carrying out rotary evaporation at 45 ℃ and 0.1Mpa, quickly removing ethanol to obtain dispersion of WPI/GA compound and shell-core structure compound particles of conjugated linoleic acid, and freeze-drying a freshly prepared sample to obtain powder WPI/GA compound and shell-core structure compound particles of conjugated linoleic acid. Wherein, based on 100 percent of the total mass of the Conjugated Linoleic Acid (CLA) emulsion, the final concentration of the conjugated linoleic acid is 2 percent, the final concentration of the WPI/GA intramolecular compound is 5 percent, and the balance is water.
Example 3
The polysaccharide is Arabic gum, the protein is whey protein isolate, the fatty acid is conjugated linoleic acid, and the preparation method comprises the following steps:
(1) weighing Arabic gum and whey protein isolate in a mass ratio of 2:1, mixing in a roller mixer at room temperature for 12 hr to dissolve completely, adjusting pH to 4.4, and stirring for 1 hr to obtain polysaccharide/protein complex.
(2) Taking a proper amount of CLA in absolute ethyl alcohol, preparing 100mg/mL CLA ethanol solution, and stirring for 1 h.
(3) Slowly dropwise adding CLA ethanol solution into GA/WPI water solution which is sheared and stirred at a high speed (20000 rpm/min), carrying out rotary evaporation at 45 ℃ and 0.1Mpa, quickly removing ethanol to obtain dispersion of WPI/GA compound and shell-core structure compound particles of conjugated linoleic acid, and freeze-drying a freshly prepared sample to obtain powder WPI/GA compound and shell-core structure compound particles of conjugated linoleic acid. Wherein, based on 100 percent of the total mass of the Conjugated Linoleic Acid (CLA) emulsion, the final concentration of the conjugated linoleic acid is 2 percent, the final concentration of the WPI/GA intramolecular compound is 3 percent, and the balance is water.
Example 4
The polysaccharide is Arabic gum, the protein is whey protein isolate, the fatty acid is conjugated linoleic acid, and the preparation method comprises the following steps:
(1) weighing Arabic gum and whey protein isolate in a mass ratio of 2:1, mixing in a roller mixer at room temperature for 12 hr to dissolve completely, adjusting pH to 4.4, and stirring for 1 hr to obtain polysaccharide/protein complex.
(2) Taking a proper amount of CLA in absolute ethyl alcohol, preparing 100mg/mL CLA ethanol solution, and stirring for 1 h.
(3) Slowly dropwise adding CLA ethanol solution into GA/WPI water solution which is sheared and stirred at a high speed (20000 rpm/min), carrying out rotary evaporation at 45 ℃ and 0.1Mpa, quickly removing ethanol to obtain dispersion of WPI/GA compound and shell-core structure compound particles of conjugated linoleic acid, and freeze-drying a freshly prepared sample to obtain powder WPI/GA compound and shell-core structure compound particles of conjugated linoleic acid. Wherein, based on 100 percent of the total mass of the Conjugated Linoleic Acid (CLA) emulsion, the final concentration of the conjugated linoleic acid is 2 percent, the final concentration of the WPI/GA intramolecular compound is 1 percent, and the balance is water.
Example 5
The polysaccharide is Arabic gum, the protein is whey protein isolate, the fatty acid is conjugated linoleic acid, and the preparation method comprises the following steps:
(1) weighing Arabic gum and whey protein isolate in a mass ratio of 2:1, mixing in a roller mixer at room temperature for 12 hr to dissolve completely, adjusting pH to 4.4, and stirring for 1 hr to obtain polysaccharide/protein complex.
(2) Taking a proper amount of CLA in absolute ethyl alcohol, preparing 100mg/mL CLA ethanol solution, and stirring for 1 h.
(3) Slowly dropwise adding CLA ethanol solution into GA/WPI water solution which is sheared and stirred at a high speed (20000 rpm/min), carrying out rotary evaporation at 45 ℃ and 0.1Mpa, quickly removing ethanol to obtain dispersion of the polysaccharide/protein compound and conjugated linoleic acid shell-core structure compound particles, and freeze-drying a freshly prepared sample to obtain powdery polysaccharide/protein compound and conjugated linoleic acid shell-core structure compound particles. Wherein, based on 100 percent of the total mass of the Conjugated Linoleic Acid (CLA) emulsion, the final concentration of the conjugated linoleic acid is 2 percent, the final concentration of the WPI/GA intramolecular compound is 0.5 percent, and the balance is water.
Example 6
The polysaccharide is beet pectin, the protein is soybean protein isolate, and the fatty acid is linolenic acid, and the preparation method comprises the following steps:
(1) weighing beet pectin and protein which are soybean protein isolate and dissolved in pure water with the mass ratio of 1:2, placing in a roller mixer, mixing at room temperature for 12h to fully dissolve and mix, adjusting pH to 4.2, and continuously stirring for 1h to obtain polysaccharide/protein complex.
(2) Taking a proper amount of linolenic acid in absolute ethyl alcohol to prepare 100mg/mL CLA ethanol solution, and stirring for 1 h.
(3) Slowly dropwise adding linolenic acid ethanol solution into beet pectin/soybean protein isolate water solution which is sheared and stirred at a high speed (20000 rpm/min), carrying out rotary evaporation at 45 ℃ and 0.1Mpa, quickly removing ethanol to obtain a dispersion of beet pectin/soybean protein isolate compound and linolenic acid shell-core structure compound particles, and freeze-drying a freshly prepared sample to obtain powdery beet pectin/soybean protein isolate compound and linolenic acid shell-core structure compound particles. Wherein, based on 100 percent of the total mass of the linolenic acid emulsion, the final concentration of the linolenic acid is 2 percent, the final concentration of the beet pectin/soybean protein isolate intramolecular compound is 1.0 percent, and the rest is water.
Example 7
The polysaccharide is soybean polysaccharide, the protein is casein, and the fatty acid is oleic acid, and the preparation method comprises the following steps:
(1) weighing soybean polysaccharide and casein as casein, dissolving in pure water at a mass ratio of 1:1, placing in a roller mixer, mixing at room temperature for 12 hr to dissolve completely, adjusting pH to 4.2, and stirring for 1 hr to obtain polysaccharide/protein complex.
(2) Taking a proper amount of oleic acid in absolute ethyl alcohol, preparing 100mg/mL CLA ethanol solution, and stirring for 1 h.
(3) Slowly dropwise adding the oleic acid ethanol solution into the soybean polysaccharide/casein aqueous solution which is subjected to high-speed shearing stirring (20000 rpm/min), carrying out rotary evaporation at 45 ℃ and 0.1Mpa, quickly removing ethanol to obtain a dispersion of the soybean polysaccharide/casein compound and oleic acid shell-core structure compound particles, and freeze-drying a freshly prepared sample to obtain powdery soybean polysaccharide/casein compound and oleic acid shell-core structure compound particles. Wherein, based on 100 percent of the total mass of the oleic acid emulsion, the final concentration of the oleic acid is 2 percent, the final concentration of the soybean polysaccharide/casein intramolecular compound is 2.0 percent, and the balance is water.
Example 8
The polysaccharide is soybean polysaccharide, the protein is soybean protein isolate, and the fatty acid is conjugated linoleic acid, and the preparation method comprises the following steps:
(1) weighing soybean polysaccharide and soybean protein which are soybean protein isolate and dissolving in pure water, wherein the mass ratio of the soybean polysaccharide to the soybean protein isolate is 2:1, placing the soybean polysaccharide to the soybean protein isolate in a roller mixer, mixing for 12 hours at room temperature to fully dissolve and uniformly mix, adjusting the pH value to 4.0, and continuously stirring for 1 hour to obtain a polysaccharide/protein complex.
(2) Taking a proper amount of conjugated linoleic acid in absolute ethyl alcohol to prepare 100mg/mL CLA ethanol solution, and stirring for 1 h.
(3) Slowly dropwise adding the ethanol solution of the conjugated linoleic acid into the soybean polysaccharide/soybean protein isolate water solution which is sheared and stirred at a high speed (20000 rpm/min), carrying out rotary evaporation at 45 ℃ and 0.1Mpa, quickly removing ethanol to obtain a dispersion of the soybean polysaccharide/soybean protein isolate compound and the shell-core structure compound particles of the conjugated linoleic acid, and freeze-drying a freshly prepared sample to obtain the powdered shell-core structure compound particles of the soybean polysaccharide/soybean protein isolate and the conjugated linoleic acid. Wherein, based on 100 percent of the total mass of the conjugated linoleic acid emulsion, the final concentration of the conjugated linoleic acid is 2 percent, the final concentration of the soybean polysaccharide/soybean protein isolate intramolecular compound is 5.0 percent, and the rest is water.
Example 9
The polysaccharide is beet pectin, the protein is whey protein isolate, the fatty acid is oleic acid, and the preparation method comprises the following steps:
(1) weighing beet pectin and protein which are whey protein isolate and dissolved in pure water at a mass ratio of 2:1, placing in a roller mixer, mixing at room temperature for 12h to fully dissolve and mix, adjusting pH to 4.4, and continuously stirring for 1h to obtain polysaccharide/protein complex.
(2) Taking a proper amount of oleic acid in absolute ethyl alcohol, preparing 100mg/mL CLA ethanol solution, and stirring for 1 h.
(3) Slowly dropwise adding the oleic acid ethanol solution into the beet pectin/whey protein isolate aqueous solution which is sheared and stirred at a high speed (20000 rpm/min), rotationally evaporating at 45 ℃ and 0.1Mpa, quickly removing ethanol to obtain a dispersion of the beet pectin/whey protein isolate compound and the shell-core structure compound particles of oleic acid, and freeze-drying a freshly prepared sample to obtain the powdered beet pectin/whey protein isolate and shell-core structure compound particles of oleic acid. Wherein, based on 100 percent of the total mass of the oleic acid emulsion, the final concentration of the oleic acid is 2 percent, the final concentration of the beet pectin/whey protein isolate intramolecular compound is 0.5 percent, and the rest is water.
Comparative example 1
The polysaccharide is Arabic gum, the protein is whey protein isolate, the fatty acid is conjugated linoleic acid, and the preparation method comprises the following steps:
(1) the weight ratio of GA to WPI is 2:1, the pH value is 4.4, and the mixture is stirred for 1 hour to form a stable WPI/GA soluble intramolecular compound.
(2) Taking a proper amount of CLA in absolute ethyl alcohol, preparing 100mg/mL CLA ethanol solution, and stirring for 1 h.
(3) The CLA ethanol solution was slowly added dropwise to the GA/WPI aqueous solution stirred at high shear (20000 rpm/min). Rotary evaporating at 45 deg.C and 0.1Mpa, rapidly removing ethanol to obtain CLA particle dispersion, and freeze drying freshly prepared sample. Wherein, based on 100 percent of the total mass of the Conjugated Linoleic Acid (CLA) emulsion, the final concentration of the conjugated linoleic acid is 2 percent, the final concentration of the WPI/GA intramolecular compound is 0.1 percent, and the balance is water.
Comparative example 2
The polysaccharide is Arabic gum, the protein is whey protein isolate, the fatty acid is conjugated linoleic acid, and the preparation method comprises the following steps:
(1) the weight ratio of GA to WPI is 2:1, the pH value is 4.4, and the mixture is stirred for 1 hour to form a stable WPI/GA soluble intramolecular compound.
(2) Slowly dropwise adding CLA into GA/WPI aqueous solution with high-speed shearing stirring (20000 rpm/min) to obtain CLA microparticle dispersion, and freeze drying freshly prepared sample. Wherein, based on 100 percent of the total mass of the CLA emulsion, the final concentration of the conjugated linoleic acid is 2 percent, the final concentration of the WPI/GA intramolecular compound is 5 percent, and the balance is water.
Comparative example 3
(1) The weight ratio of GA to WPI is 2:1, the pH value is 4.4, and the mixture is stirred for 1 hour to form a stable WPI/GA soluble intramolecular compound.
(2) Taking a proper amount of CLA in absolute ethyl alcohol, preparing 100mg/mL CLA ethanol solution, and stirring for 1 h.
(3) Slowly dropwise adding CLA ethanol solution into GA/WPI water solution with high shear stirring (20000 rpm/min) to obtain CLA microparticle dispersion, and freeze drying freshly prepared sample. Wherein, based on 100 percent of the total mass of the Conjugated Linoleic Acid (CLA) emulsion, the final concentration of the conjugated linoleic acid is 2 percent, the final concentration of the WPI/GA intramolecular compound is 2 percent, the ethanol content is 18 percent, and the balance is water.
The data of the properties of emulsions 1 to 9 and comparative emulsions 1 to 3 are shown in Table 1, the detection method used in the invention:
(1) measurement of particle size of CLA microparticles:
the size distribution of the GA microparticles at different concentrations was determined using a Mastersizer 2000 laser particle sizer. The emulsion was shaken up with gentle shaking, added dropwise to the dispersant and injected by a Hydro 2000MU wet sampler. Using ultrapure water as a dispersant, the refractive indices of the dispersed phase and the continuous phase were 1.52 and 1.33, respectively, the absorption of the sample was 0.01, and the pump speed was 2000 rpm. The measurement can be started by adding the sample until the laser index is slightly greater than 10%. The average particle size of the emulsion is represented by the surface weighted average D [3,2] and is calculated as follows:
D[3,2]=（Σnidi3/Σnidi2），
where ni represents the number of particles having a particle size di.
(2) Evaluation of physical stability of CLA microparticles:
and (3) placing the prepared fresh CLA particle dispersion liquid in a 40-DEG C constant-temperature incubator, and carrying out emulsion particle size measurement after placing the fresh CLA particle dispersion liquid for 0d, 3d, 5d and 7 d.
(3) And (3) observing the microstructure of the CLA particles:
and (3) placing a very small amount of CLA particle powder on a sample table of a scanning electron microscope, spraying gold, observing under a JSM-6390LV scanning electron microscope, and taking a picture for recording.
(4) The release rate of CLA particles in simulated gastrointestinal environment was determined:
placing 1.0 mL CLA microparticle suspension in 29.0mL simulated gastric juice (pH adjusted to 2.0 by 2mg/mL NaCl, 3.2mg/mL pepsin and HCl) pre-warmed at 37 deg.C, stirring at 100 rpm, digesting for 3 hr in constant temperature water bath at 37 deg.C, adjusting pH every 30min to stabilize at 2.0, and sampling samples at 30, 60, 90, 120, 150 and 180min respectivelyThe release rate of CLA was determined. Taking 1.0 mL for determining the particle size, adding an equal amount of n-hexane into 1.0 mL for extraction, fixing the volume to 10.0 mL, determining the light absorption value at 234 nm, and calculating the content. After the gastric digestion phase, the pH was adjusted to 7.0 with 1mol/L NaOH, transferred to 30mL simulated intestinal fluid (8 mg/mL NaCl, 40mg/mL CaCl2, 5 mg/mL bile salts, 10 mg/mL trypsin) and continued at 37oC, carrying out constant-temperature water bath, stirring at 100 rpm, digesting for 3h, adjusting the pH value every 30min to be stable at 7.0, and sampling at 30min, 60 min, 90 min, 120 min, 150 min and 180min respectively to determine the release rate of the CLA. Taking 1.0 mL for determining the particle size, adding an equal amount of n-hexane into 1.0 mL for extraction, fixing the volume to 10.0 mL, determining the light absorption value at 234 nm, and calculating the content.
TABLE 1 particle size and Freeze drying Performance of emulsions 1-9 and comparative emulsions 1-3
Claims (3)
1. A method for improving the emulsification stability of a polysaccharide/protein complex, which is characterized in that the pH stability of the polysaccharide/protein complex is improved by preparing a polysaccharide/protein complex and fatty acid shell-core structure complex particle through an emulsification-solvent volatilization method, wherein the emulsification-solvent volatilization method comprises the following steps:
(1) weighing polysaccharide and protein, dissolving in pure water, placing in a roller mixer, mixing at room temperature for 12 hr to dissolve completely, adjusting pH to 4.0-4.4, and stirring for 1 hr to obtain polysaccharide/protein complex;
(2) preparing 100mg/mL fatty acid ethanol solution, and stirring for 1 h;
(3) slowly dropwise adding the fatty acid ethanol solution obtained in the step (2) into the polysaccharide/protein compound aqueous solution obtained in the step (1) subjected to high-speed shearing and stirring, performing rotary evaporation at 45 ℃ and under 0.1Mpa, and quickly removing ethanol to obtain a fatty acid particle dispersion liquid;
the rotating speed of the high-speed shearing is 20000 rpm/min;
(4) and (4) freeze-drying the fatty acid particle dispersion liquid prepared in the step (3) to obtain the polysaccharide/protein compound and fatty acid shell-core structure compound particles.
2. The method of claim 1, wherein the polysaccharide/protein complex emulsion stability is increased by: the polysaccharide in the step (1) is any one of Arabic gum, beet pectin and soybean polysaccharide;
the protein is any one of whey protein isolate, soy protein isolate and casein.
3. The method of claim 1, wherein the polysaccharide/protein complex emulsion stability is increased by: the fatty acid in the step (2) is any one of oleic acid, linolenic acid and conjugated linoleic acid.
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