CN115886204A - Preparation method of Pickering high internal phase emulsion for dumpling filling additive - Google Patents
Preparation method of Pickering high internal phase emulsion for dumpling filling additive Download PDFInfo
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- CN115886204A CN115886204A CN202211648899.9A CN202211648899A CN115886204A CN 115886204 A CN115886204 A CN 115886204A CN 202211648899 A CN202211648899 A CN 202211648899A CN 115886204 A CN115886204 A CN 115886204A
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Images
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A40/00—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
- Y02A40/90—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in food processing or handling, e.g. food conservation
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- Colloid Chemistry (AREA)
Abstract
The invention provides a preparation method of Pickering high internal phase emulsion for a dumpling filling additive, which comprises the following preparation steps of S1: obtaining a covalent compound of Bemisia tabaci protein (SBP) -epigallocatechin gallate (EGCG) by using a free radical induction method by taking the SBP and the EGCG as raw materials; and (3) mixing the SBP-EGCG covalent compound in the step (S1) with edible oil, and then shearing and emulsifying to obtain the stable Pickering high internal phase emulsion. The Pickering high internal phase emulsion obtained by the invention has stronger stability and can effectively improve the protection effect on bioactive substances; the emulsion has excellent viscoelasticity, self-supporting property and thixotropic recovery property, and can be used for 3D printing food; the emulsion can be used as additive of dumpling stuffing to impart dumpling functional food property. The preparation method is simple and easy to operate, and has a good prospect in the aspects of novel nutrient delivery systems, food-grade 3D printing materials, functional nutrient additive and the like.
Description
Technical Field
The invention relates to the field of food industry, in particular to a preparation method of Pickering high internal phase emulsion for a dumpling filling additive.
Background
Pickering high internal phase emulsions generally refer to emulsions stabilized with rigid particles having an internal phase volume fraction greater than 74%. Compared to traditional emulsions, pickering high internal phase emulsions have a high capacity to load hydrophobic biological compounds due to their higher internal phase. Therefore, the potential of Pickering high internal phase emulsions as encapsulation and delivery systems for nutrients is of great interest. The irreversible adsorption of solid particles at the oil-water interface imparts resistance to Ostwald ripening, resistance to coalescence, and excellent stability to Pickering high internal phase emulsions. In addition, pickering high internal phase emulsions have adjustable viscoelasticity, which also provides convenient conditions for the application of functional foods. However, food safety issues with solid particles have limited the use of Pickering high internal phase emulsions in the food industry. Therefore, the production of solid particle stabilizers with a "clean" label is a key factor in the widespread adoption of Pickering high internal phase emulsions. In recent years, food grade solid particle stable Pickering high internal phase emulsions, such as protein based, polysaccharide based and composite particles have been reported. It is noted that functional particles are also of great interest. Epigallocatechin gallate (EGCG) is a polyphenol compound with antioxidant, anti-inflammatory, antibacterial and other activities. Previously, several studies have shown that EGCG can be combined with proteins to prepare particulate stabilizers with antioxidant activity for the stabilization of emulsions. The interaction of EGCG with proteins changes the structure of the proteins, thereby improving the stability of the emulsion. Furthermore, the protein-based complex with EGCG stabilizes the emulsion, thereby improving the stability of the bioactive substance in the emulsion.
CN110498935A describes a high internal phase emulsion of soy protein isolate-pectin complex stabilized quercetin and its preparation method, dissolving soy protein isolate in distilled water to obtain soy protein isolate solution; dissolving pectin in distilled water, and adjusting pH to obtain pectin solution; mixing the soy protein isolate solution with the pectin solution; adjusting the pH value of the solution to 3.0-11.0; mixing the obtained solution with vegetable oil containing quercetin at a certain proportion, performing ultrasonic treatment, and centrifuging to obtain high internal phase emulsion containing stable quercetin of soybean protein isolate pectin compound. The inventive high internal phase emulsions require a two-step process for preparation and no direction of application in the food industry is mentioned in the invention.
Recently, as consumer demand for foods has been increasing, three-dimensional (3D) printed foods have received much attention. Compared with traditional food, the 3D printed food has a shape with exquisite design. In addition, the 3D printed food can also provide special nutritional requirements for special people. For example, 3D printed food may serve people with chewing disorders. Rheological properties are key factors in assessing whether a material is suitable for 3D printing. The 3D printed material needs to have high viscoelasticity, excellent thixotropic recovery properties, and self-supporting properties. However, the number of food-print materials having biocompatibility and biodegradability is extremely limited. Therefore, there is a great interest in developing a 3D printed food based on Pickering high internal phase emulsion with specific nutritional ingredients and natural materials.
CN113306271a describes a medium and high internal phase emulsion material for 3D printing and its application, the material is prepared by the following method: 1) Dispersing cellulose nanocrystals in an aqueous solution containing salt, and preparing a nano material suspension as a water phase; 2) Forming an emulsion by an oil-water two-phase emulsification method; 3) Excess water in the emulsion was removed by centrifugation to give a medium to high internal phase emulsion. The high internal phase emulsion in the invention needs to be prepared by a two-step method, and the 3D printing material in the invention is not loaded with any nutrient substances, and the encapsulation condition is unknown.
In summary, the following problems also exist for the preparation of Pickering high internal phase emulsions and their use in the food field: the existing Pickering high internal phase emulsion mostly lacks biocompatibility and biodegradability, so that the Pickering high internal phase emulsion has lower food safety; the existing Pickering high internal phase emulsion still lacks excellent rheological properties, so that the Pickering high internal phase emulsion cannot be used as a food-grade 3D printing material; the existing Pickering high internal phase emulsion can not load bioactive substances to meet the requirements of people on specific nutrients; at present, no Pickering high internal phase emulsion is used as an additive of dumpling fillings to improve the oil retention condition of the fillings and endow the dumpling fillings with special nutritional requirements.
Disclosure of Invention
The invention aims to provide a preparation method of Pickering high internal phase emulsion for a dumpling filling additive. According to the invention, the SBP-EGCG covalent compound is prepared by a free radical induction method, and the SBP-EGCG covalent compound is used as a stabilizer to prepare the Pickering high internal phase emulsion which has stronger stability, can effectively prevent oxidation of internal phase algal oil, and improves the stability and biological accessibility of astaxanthin; the emulsion also has excellent rheological property and can be used as a food-grade 3D printing material; in addition, the emulsion can be attached to the filling due to the excellent viscosity, and can be used as an additive of the filling of dumplings.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of Pickering high internal phase emulsion is characterized by comprising the following steps:
s1: preparing SBP solution from SBP, standing overnight, adding H into SBP solution 2 O 2 And vitamin C, incubating for 1-4 h, adding EGCG to obtain a mixed solution, adjusting the pH of the mixed solution, incubating for 24h, dialyzing the sample, and freeze-drying the content to obtain an SBP-EGCG covalent complex;
s2: and (3) preparing the SBP-EGCG covalent compound solution from the SBP-EGCG covalent compound in the step (S1), mixing the SBP-EGCG covalent compound solution with edible oil, and then shearing and emulsifying to obtain the Pickering high internal phase emulsion.
In one embodiment of the present invention, the mass ratio of EGCG to SBP in S1 is 0.03-0.2.
In one embodiment of the invention, the concentration of SBP in the SBP solution in S1 is 5-20 g/L.
In one embodiment of the invention, the pH of the mixture in S1 is in the range of 3 to 11.
In one embodiment of the invention, the concentration of SBP-EGCG covalent complex in the SBP-EGCG covalent complex solution in S2 is 0.5-2 wt%.
In one embodiment of the invention, the volume ratio of the SBP-EGCG covalent compound solution to the edible oil is 4:6-1:9.
In one embodiment of the invention, the rotation speed of the shearing is 6000-12000 rpm, and the shearing time is 1-5 min.
A preparation method of Pickering high internal phase emulsion comprises the following steps:
s1: dissolving 1g of SBP in 50-200 mL of deionized water, stirring for 2-8H, standing overnight at 2-8 ℃, and adding 0.5-2 mL of H into the obtained SBP solution 2 O 2 And 0.2-0.4 g of vitamin C, incubating for 1-4 h at 20-30 ℃, adding EGCG into the mixture, adjusting the pH of the mixture, incubating for 24h at 20-30 ℃, dialyzing the sample for 48h by a dialysis bag (MWCO: 6000-8000 Da), and freeze-drying the content to obtain the SBP-EGCG covalent complex.
S2: and (3) mixing the SBP-EGCG covalent compound in the step (S1) with edible oil, and then shearing and emulsifying to obtain the astaxanthin-loaded Pickering high internal phase emulsion which can be used as the dumpling filling additive.
In one embodiment of the invention, the amount of EGCG added to S1 is from 30 to 200mg.
In one embodiment of the invention, the SBP-EGCG covalent compound solution with the concentration of 0.5-2 wt% prepared in S2 is prepared by stirring and dissolving the SBP-EGCG covalent compound, and hydrating at 2-8 ℃ for 8-24 h to obtain the SBP-EGCG covalent compound solution.
In one embodiment of the invention, the edible oil selected in S2 is algal oil; the volume ratio of the SBP-EGCG covalent compound to the algae oil is 4:6-1:9; the high-speed shearing rotating speed is 6000-12000 rpm, and the shearing time is 1-5 min.
The Pickering high internal phase emulsion prepared by the method is provided by the invention.
A second object of the invention is to apply the Pickering high internal phase emulsion described above to entrap, load or deliver nutrients.
The third purpose of the invention is to apply the Pickering high internal phase emulsion to the field of 3D printing food.
A third object of the present invention is to apply the Pickering high internal phase emulsion described above to a filling for dumplings.
Advantageous effects
The Pickering high internal phase emulsion prepared by using the sea bass protein and the EGCG as raw materials without adding any inorganic material has high biological safety; the highest internal phase of the Pickering high-internal-phase emulsion prepared by the method can reach 85 percent, and the embedding of hydrophobic functional active substances can be effectively realized; the Pickering high internal phase emulsion can effectively prevent the oxidation of internal phase algae oil, and improve the stability and the biological accessibility of astaxanthin; the Pickering high internal phase emulsion has excellent self-supporting property and thixotropic recovery property, and can be used as a 3D printing material; the Pickering high internal phase emulsion has excellent viscosity, can be attached to stuffing and can be used as an additive of dumpling stuffing.
Drawings
FIG. 1 shows the results of measuring the total polyphenol content of the SBP-EGCG complex of example 1.
FIG. 2 shows the results of measuring the content of free amino groups in the SBP-EGCG complex of example 1.
FIG. 3 shows the results of measuring the thiol group content of the SBP-EGCG complex of example 1.
FIG. 4 shows the results of determining the tryptophan content of the SBP-EGCG complex of example 1.
FIG. 5 is an infrared spectrum of the SBP-EGCG complex of example 1.
FIG. 6 is a Cryo-SEM image of the SBP-EGCG complex of example 2.
FIG. 7 is a graph of the three-phase contact angle results for the SBP-EGCG complex of example 2.
FIG. 8 is a graph showing the result of DPPH radical scavenging activity of the SBP-EGCG complex of example 2.
FIG. 9 is a graph showing the results of dynamic interfacial tension of the SBP-EGCG complex of example 2.
Fig. 10 is an appearance plot of the example 3Pickering high internal phase emulsion freshly prepared and stored at room temperature for 50 days.
FIG. 11 is a Cryo-SEM image of a Pickering high internal phase emulsion of example 3.
FIG. 12 is a measurement of storage modulus and loss modulus as a function of frequency for the Pickering high internal phase emulsion of example 3.
Fig. 13 is a measurement of viscosity as a function of shear rate for the Pickering high internal phase emulsion of example 3.
Fig. 14 is a measurement of viscosity over time for the Pickering high internal phase emulsion of example 3.
FIG. 15 is a measurement of storage modulus and loss modulus as a function of temperature for the Pickering high internal phase emulsion of example 3.
Fig. 16 is the encapsulation efficiency of astaxanthin in the Pickering high internal phase emulsion loaded with astaxanthin of example 4.
Fig. 17 is the retention of astaxanthin after 15 days of storage at room temperature for the astaxanthin-loaded Pickering high internal phase emulsion of example 4.
Fig. 18 is bioavailable data from the in vitro simulated digestion experiments for the astaxanthin-loaded Pickering high internal phase emulsion of example 4.
FIG. 19 is the hydroperoxide content of the astaxanthin-loaded Pickering high internal phase emulsion of example 4 after 15 days of storage at 50 ℃.
FIG. 20 is the malondialdehyde content of the astaxanthin-loaded Pickering high internal phase emulsion of example 4 after storage at 50 ℃ for 15 days.
Fig. 21 is an appearance of the Pickering high internal phase emulsion loaded with astaxanthin of example 4 after 3D printing.
Fig. 22 is an appearance of the astaxanthin-loaded Pickering high internal phase emulsion of example 4 before and after mixing with dumpling filling and centrifugation.
Fig. 23 is a graph of the oil holdup of example 4 astaxanthin-loaded Pickering high internal phase emulsion mixed with dumpling filling after centrifugation.
Detailed Description
The present invention will be described in further detail with reference to examples and fig. 1 to 23, but the present invention is not limited thereto.
The following specific test protocol is as follows:
determination of total polyphenol content: 2.5mL of Folin phenol reagent was added to 0.5mL of SBP-EGCG complex (1 mg/mL) and reacted for 5min in the absence of light. Then, 2mL of Na2CO3 solution was added thereto, and the mixture was reacted for 2 hours under dark conditions. The absorbance values were measured at 760 nm.
Determination of the content of free amino groups: 0.2mL of SBP-EGCG complex (1 mg/mL) was mixed with 4mL of phthalaldehyde solution, and the mixture was incubated at 35 ℃ for 2min. O-phthalaldehyde solution: 80mg of phthalaldehyde was dissolved in 2mL of methanol, 5mL of SDS, 50mL of borax solution and 0.2mL of beta-mercaptoethanol were added, and the mixture was made to a volume of 100mL in a volumetric flask. The absorbance was measured at 340 nm.
Determination of the free thiol content: 1mL Tris-glycine buffer was added to 3mg SBP-EGCG complex and 10. Mu.L 5,5-dithio-bis- (2-nitrobenzoic acid) solution was added. The mixture was reacted at 25 ℃ for 30min. Absorbance was measured at 412 nm.
Determination of the free tryptophan content: 0.9mL of SBP-EGCG complex (1 mg/mL) was added to 1mL of nitric acid (16 mol/L) and mixed at 50 ℃ for 15min. The mixture was cooled to room temperature and 4mL NaOH and 4mL ethanol were added. The absorbance was measured at 360nm and 430nm, respectively.
Fourier transform infrared spectroscopy (FTIR): after 2mg of the SBP-EGCG complex was mixed uniformly with 200mg of potassium bromide, the mixture was compressed into transparent tablets. FTIR spectra were collected from 4000 to 500-1cm using a FTIR spectrometer.
Microstructure: the microstructure of the SBP-EGCG complex was obtained by low temperature scanning electron microscope (cryo-SEM), the concentration of SBP-EGCG complex was 0.5wt%;
the microstructure of the Pickering high internal phase emulsion is captured by a low-temperature scanning electron microscope, the Pickering high internal phase emulsion is frozen in liquid nitrogen slurry, sublimed and plated with gold in a low-temperature transport system, and a sample is observed in a test room at-145 ℃.
Three-phase contact angle (θ): the theta of the SBP-EGCG complex was measured by a droplet shape analyzer. The freeze-dried SBP-EGCG complexes were compressed into 2mm tablets, which were soaked in algal oil. The tablets were placed on a glass slide and 5. Mu.L of deionized water was added using a syringe. The topography of the droplets was obtained by a high-speed camera.
DPPH radical scavenging activity: 2mL of SBP-EGCG complex (0.5 mg/mL) was mixed with 2mL of DPPH solution. The mixture was reacted in the dark for 15min and the absorbance was measured at 517 nm.
Dynamic interfacial tension measurement: 34 μ L of SBP-EGCG complex was dripped into algal oil for 180min. The adsorption behavior of the SBP-EGCG complex at the oil-water interface was measured by a droplet shape analyzer. The dynamic interfacial tension was determined according to the equation of the young-laplace formula (the protein to EGCG ratio of the complex used in this measurement was 10, ph 9.
Rheological testing: the rheological behavior of the Pickering high internal phase emulsion is characterized by a rheometer. The frequency sweep test was performed at a frequency range of 0.1 to 10Hz with a fixed strain of 0.5% at 25 ℃. The viscosity curve is obtained by a shear rate of 0.1 to 100s-1 at 25 ℃. Structure recovery characteristics: the viscosity was measured at a shear rate of 0.1s-1 for 60s, 100s-1 for 20s and 0.1s-1 for 100 s. The temperature sweep test was determined at a fixed strain of 0.5% and an angular frequency of 10 rad/s. The heating rate is 5 ℃/min, and the temperature range is 20-80 ℃.
Stability of astaxanthin in Pickering high internal phase emulsions: after 15 days of storage of the astaxanthin-loaded Pickering high internal phase emulsion at room temperature/visible light, the retention of astaxanthin was determined.
Determination of the bioassaability of astaxanthin: an in vitro simulated digestion model was designed, and the entire simulation was performed at 37 ℃. Oral phase: 7.5mL of the sample was mixed with 7.5mL of simulated saliva containing mucin (30 mg/mL). The pH of the mixture was adjusted to 6.8 and incubated at 100rpm for 10 minutes. Stomach phase: to the oral digestive juice was added 15mL simulated gastric juice containing pepsin (3.2 mg/mL). The pH of the mixture was adjusted to 2 and incubated at 100rpm for 2 hours. Small intestinal phase: 7.5mL of simulated intestinal fluid was added to the gastric digestive juice. Simulated intestinal fluid comprised 60 mg of pancreatin, 60 mg of lipase and 187.5 mg of bile salts. The pH of the mixture was adjusted to 7 and incubated at 100rpm for 2 hours. The crude chyme was centrifuged at 10,000rpm for 60min to obtain a middle micellar phase. The concentrations of astaxanthin in the initial sample, chyme and micelles were measured separately. And calculating the conversion, bioacessability index and bioacessability of the astaxanthin.
Algal oil stability determination in Pickering high internal phase emulsions: the samples were incubated at 50 ℃ for 15 days to accelerate the oxidation of algal oil. Lipid hydrogen peroxide (LH): 1.5mL of 2-propanol/isooctane (1, 3,v/v) was added to the 0.2mL of sample, and the mixture was centrifuged at 8000rpm for 3min to obtain a supernatant. To 0.2mL of the supernatant were added 2.8mL of methanol/1-butanol (2, 1,v/v), 15. Mu.L of ammonium thiocyanate and Fe2+ solution, and the mixture was reacted for 20min with exclusion of light. Absorbance was measured at 510 nm. Malondialdehyde (MDA): 1.8mL of deionized water and 4mL of thiobarbituric acid (TBA) solution were added to 0.2mL of the sample. The TBA solution contained 0.375g TBA, 15g trichloroacetic acid, 100mL HCl (0.25 mol/L). The sample mixture was incubated at 100 ℃ for 10 minutes, cooled to room temperature, and then the mixture was centrifuged at 8000rpm for 3 minutes to obtain a supernatant. The absorbance was measured at 532 nm.
3D printing test: the Pickering high internal phase emulsion loaded with astaxanthin was 3D printed by 3D printing with a 1mm nozzle. The sample after 3h of preparation was placed in a feeder before printing, the extrusion rate at printing was 1mm3s-1. The "symbol" model, which is 49.58 mm long, 51.01 mm wide and 5.78 mm high, is fed into the printer. The printing process was carried out at 25 ℃ and pictures were taken after printing.
Oil retention of Pickering high internal phase emulsion in dumpling filling: according to the ratio of the pork stuffing to the algae oil of 10:1 and 5:1, respectively mixing the Pickering high internal phase emulsion loaded with astaxanthin or unencapsulated dissolved astaxanthin algal oil with stuffing, centrifuging at 3000 rpm for 10 minutes, and measuring the oil holding level of the stuffing.
Example 1
The preparation method of the sea bass protein-EGCG compound (under different pH conditions) comprises the following specific steps:
1g of SBP was dissolved in 100mL of deionized water and stirred for 4H, hydrated at 4 ℃ overnight, and 1mL of H was added to the resulting SBP solution 2 O 2 And 0.25g of vitamin C and given at 25 ℃ for 2.5h, 100mg of EGCG was added to the mixture, the pH of the mixture was adjusted to 9, and after 24h of incubation at 25 ℃, the samples were passed through dialysis bags (MWCO:6000-8000 Da) for 48h, and freeze-drying the content to obtain an SBP-EGCG covalent compound; SBP of the study, which passed through the entire preparation of all SBP-EGCG complexes, was used as a control, and SBP + EGCG indicated that no H was added during the preparation of the SBP-EGCG complexes 2 O 2 A mixture of (a).
Example 2
The preparation method of the sea bass protein-EGCG compound (under different pH conditions) comprises the following specific steps:
1g of SBP was dissolved in 100mL of deionized water and stirred for 4H, hydrated at 4 ℃ overnight, and 1mL of H was added to the resulting SBP solution 2 O 2 And 0.25g of vitamin C, endowing the mixture at 25 ℃ for 2.5h, adding 100mg of EGCG into the mixture, adjusting the pH of the mixture to be 3,5,7,9 and 11 respectively, incubating the mixture at 25 ℃ for 24h, dialyzing the sample through a dialysis bag (MWCO: 6000-8000 Da) for 48h, and freeze-drying the content to obtain an SBP-EGCG covalent complex; SBP of the study, which passed through the entire preparation of all SBP-EGCG complexes, was used as a control, and SBP + EGCG indicated that no H was added during the preparation of the SBP-EGCG complexes 2 O 2 A mixture of (a).
The results of the measurement of the total polyphenol content in the SBP-EGCG complex obtained in example 2 are shown in FIG. 1.
As shown in FIG. 1, the content of polyphenol in SBP-EGCG complex was 69.76, 73.58, 91.80, 100.18, 72.35. Mu.g/mL at pH 3,5,7,9 and 11, respectively. The results show that the amount of grafting of EGCG is higher at pH9 than at other pH's, with higher amounts of grafting of EGCG.
The results of the measurement of the free amino group content in the SBP-EGCG complex obtained in example 2 are shown in FIG. 2.
As shown in FIG. 2, the binding capacity of SBP to EGCG increased with increasing pH, with the binding strength being highest at pH 9. At pH 3 and 5, the solubility of SBP is low due to the proximity of the isoelectric point of SBP; at pH11, the structure of SBP is excessively denatured, which limits the exposure of reactive groups.
The results of the measurement of the free thiol content in the SBP-EGCG complex obtained in example 2 are shown in FIG. 3.
As shown in FIG. 3, the free thiol content was lowest at pH9, and the binding ability of SBP to EGCG was strongest.
The results of the measurement of the content of free tryptophan in the SBP-EGCG complex obtained in example 2 are shown in FIG. 4.
As shown in FIG. 4, the content of free tryptophan was the lowest at pH9, and the binding ability of SBP to EGCG was the strongest.
The IR spectrum of the SBP-EGCG complex obtained in example 2 is shown in FIG. 5.
As shown in FIG. 5, the spectrum of SBP has characteristic peaks in the amide I band, the amide II band and the amide A band. Compared with SBP, the absorption peak of SBP-EGCG complex in the amide II band is shifted to low wavenumber, and the absorption peak of SBP-EGCG complex in the amide I and amide A bands is shifted to high wavenumber. Interestingly, all characteristic peak shifts of the SBP-EGCG complex shifted at pH9, indicating that the complex had a higher amount of EGCG grafting at pH 9.
Example 3:
the preparation method of the sea bass protein-EGCG compound (under the conditions of different proportions of protein and EGCG) comprises the following specific steps:
1g of SBP was dissolved in 100mL of deionized water and stirred for 4H, hydrated at 4 ℃ overnight, and 1mL of H was added to the resulting SBP solution 2 O 2 And 0.25g of vitamin C and given for 2.5h at 25 ℃, 33, 50, 100, 200mg of EGCG were added to the mixture separately, the pH of the mixture was adjusted to 9 (resulting in a mixture of protein to EGCG ratio of 30; SBP of the study, which passed through the entire preparation of all SBP-EGCG complexes, was used as a control, and SBP + EGCG indicated that no H was added during the preparation of the SBP-EGCG complexes 2 O 2 A mixture of (a).
The microstructure of the SBP-EGCG complex obtained in example 3 is shown in FIG. 6.
As shown in FIG. 6, the spherical particles of SBP formed large aggregates in aqueous solution, and the particle size of the SBP + EGCG mixture was also slightly reduced compared to SBP due to the presence of EGCG. The complexes formed by SBP and EGCG in different proportions (30. However, at higher EGCG content, the particles of SBP-EGCG-5:1 complex dispersed into larger spherical particles.
The three-phase contact angle results of the SBP-EGCG complex obtained in example 3 are shown in FIG. 7.
As shown in fig. 7, the formation of SBP-EGCG complex by radical induced reaction enhanced surface hydrophobicity and interfacial wettability compared to SBP and SBP + EGCG. In addition, in the complexes formed by SBP and EGCG with different proportions, the theta angle of the SBP-EGCG-10.
The results of the DPPH radical scavenging activity of the SBP-EGCG complex obtained in example 3 are shown in FIG. 8.
As shown in FIG. 8, the mixture of SBP + EGCG and all SBP-EGCG complexes enhanced DPPH radical scavenging activity compared to SBP, especially the DPPH radical scavenging activity of SBP-EGCG-10.
The results of the dynamic interfacial tension of the SBP-EGCG complex obtained in example 3 are shown in FIG. 9.
As shown in FIG. 9, the interfacial tension of the SBP-EGCG complex is lower than that of SBP and SBP + EGCG, which indicates that the covalent bonding of SBP and EGCG can effectively reduce the interfacial tension and is beneficial to stabilize the emulsion. In addition, as the content of the SBP-EGCG complex increases, the interfacial tension gradually decreases, indicating that the concentration of the complex affects the rearrangement of the oil-water interfacial particles and the thickness of the particle layer. The SBP-EGCG complex has the potential to stabilize Pickering emulsions.
Example 4:
the preparation method of the Pickering high internal phase emulsion with stable sea bass protein-EGCG compound comprises the following specific steps:
the concentrations of the obtained jewfish protein-EGCG (ratio of jewfish protein to EGCG of 10:1, ph of 9) complexes in example 3 were 0.5wt%,1wt%,1.5wt% and 2wt%, with jewfish protein alone, jewfish protein and EGCG mixture as experimental controls; selecting algae oil as an oil phase; the volume ratio of the sea bass protein-EGCG compound to the algae oil is 2:8; the high-speed shearing rotation speed is 10000rpm, the shearing time is 2min, and the stable Pickering high internal phase emulsion of the sea bass protein-EGCG compound is obtained.
The appearance of fresh emulsions and after 50 days of storage of Pickering high internal phase emulsions stabilized by the sea bass protein-EGCG complex are shown in fig. 10.
As shown in fig. 10, fresh Pickering high internal phase emulsion stabilized by sea bass protein-EGCG complex has a homogeneous gel state, all samples still have self-supporting ability after inversion, which suggests that Pickering high internal phase emulsion is in 3D printed product. After 50 days of storage at room temperature/visible light, the Pickering high internal phase emulsion stabilized by 0.5wt% of sea bass protein showed phase separation. However, other Pickering high internal phase emulsions exhibit gel-like behavior and can remain self-supporting at the bottom of the vial even when the sample vial is inverted.
Cryo-SEM results of Pickering high internal phase emulsions stabilized by sea bass protein-EGCG complex are shown in figure 11.
Cryo-SEM was used to directly visualize the droplet status of Pickering high internal phase emulsions as shown in figure 11. Compared to SBP and SBP + EGCG, pickering high internal phase emulsions prepared at sea bass protein-EGCG complexes exhibit smaller droplet size, smaller droplet spacing and tighter structure, which contributes to the improved viscosity and stability of Pickering high internal phase emulsions. And further increasing the concentration of the compound can improve the particle coverage rate on the surface of the liquid drop and the filling rate of the gap of the liquid drop, so that the liquid drop is fixed in the 3D network structure of the Pickering high internal phase emulsion.
The results of the measurements of storage modulus and loss modulus as a function of frequency for Pickering high internal phase emulsions are shown in figure 12.
As shown in fig. 12, the storage modulus was higher than the loss modulus for all samples over the entire frequency range, indicating the solid viscoelastic behavior of the Pickering high internal phase emulsion. The Pickering high internal phase emulsion prepared from the sea bass protein-EGCG complex has higher viscoelasticity than SBP and SBP + EGCG. As the concentration of the complex increases, the storage modulus of the Pickering high internal phase emulsion also increases. Furthermore, the storage modulus of all samples was almost an order of magnitude higher than the loss modulus, indicating a strong network structure. Also, at constant strain, the storage modulus is almost independent of frequency, showing the typical characteristics of a gel-like emulsion.
The viscosity of Pickering high internal phase emulsions is measured as a function of shear rate as shown in figure 13.
As shown in fig. 13, all Pickering high internal phase emulsions exhibited typical shear thinning behavior. This shear thinning behavior of Pickering high internal phase emulsions may support its application in 3D printing. The viscosity of Pickering high internal phase emulsions prepared from the sea bass protein-EGCG complex was higher compared to SBP and SBP + EGCG. In addition, the viscosity of the Pickering high internal phase emulsion is positively correlated with the concentration of the weever protein-EGCG complex.
The results of measuring the viscosity of Pickering high internal phase emulsions at different shear rates over time are shown in figure 14.
As shown in fig. 14, therefore, the recovery characteristics of Pickering high internal phase emulsions at shear rate were investigated by three-zone thixotropy experiments. The change in viscosity of the Pickering high internal phase emulsion was observed at shear frequencies of 0.1s-1, 100s-1 and 0.1s-1 alternating. The storage modulus of the Pickering high internal phase emulsion did not change much when the shear frequency was 0.1 s-1. The storage modulus of all samples dropped significantly as the strain increased from 0.1s-1 to 100 s-1. When the strain was reduced to 0.1s-1, the storage modulus of the Pickering high internal phase emulsion returned to the initial state. Compared with SBP and SBP + EGCG, the Pickering high internal phase emulsion prepared from the sea bass protein-EGCG compound has better recovery property. In addition, the higher the concentration of the perch protein-EGCG complex, the stronger the recovery properties of the Pickering high internal phase emulsion.
The results of the storage/loss modulus measurements of Pickering high internal phase emulsions as a function of temperature are shown in figure 15.
As shown in fig. 15, therefore, the storage modulus of all samples remained at the original level throughout the temperature rise, demonstrating excellent thermal stability, which lays the foundation for the Pickering high internal phase emulsion as an additive for dumpling fillings.
Example 5:
a preparation method of Pickering high internal phase emulsion for a dumpling filling additive comprises the following specific steps:
the concentrations of the obtained jewfish protein-EGCG (ratio of jewfish protein to EGCG of 10:1, ph of 9) complexes in example 3 were 0.5wt%,1wt%,1.5wt% and 2wt%, with jewfish protein alone, jewfish protein and EGCG mixture as experimental controls; selecting algae oil as an oil phase; dissolving 0.1wt% astaxanthin in algal oil; the volume ratio of the sea bass protein-EGCG compound to the algae oil is 2:8; the high-speed shearing rotation speed is 10000rpm, the shearing time is 2min, and the stable Pickering high internal phase emulsion of the astaxanthin-loaded sea bass protein-EGCG compound is obtained.
And (3) performance testing:
the encapsulation efficiency of astaxanthin in Pickering high internal phase emulsions is shown in figure 16.
As shown in fig. 16, the effect of the jewfish protein microgel particles on the ability of the Pickering high internal phase emulsion to encapsulate astaxanthin was investigated. As a result, the encapsulation efficiencies of astaxanthin in the Pickering high internal phase emulsion were found to be 87.19% (SBP), 88.70% (SBP + EGCG), 90.72% (SBP-EGCG-0.5%), 91.98% (SBP-EGCG-1%), 95.26% (SBP-EGCG-1.5%) and 96.01% (SBP-EGCG-2%), respectively. All Pickering high internal phase emulsions have a relatively high encapsulation efficiency. Compared with SBP and SBP + EGCG, the Pickering high internal phase emulsion prepared from the sea bass protein-EGCG compound has better encapsulation efficiency. In addition, higher concentrations of the perch protein-EGCG complex may increase the encapsulation efficiency of astaxanthin in Pickering high internal phase emulsions.
The retention of astaxanthin in the Pickering high internal phase emulsion after 15 days of storage at room temperature/visible light loaded Pickering high internal phase emulsion was measured as shown in fig. 17.
As shown in fig. 17, the retention rates of astaxanthin after 15 days of storage are listed in the following order: 80.64% (SBP-EGCG-2%) >78.85% (SBP-EGCG-1.5%) >67.33% (SBP-EGCG-1%) >57.09% (SBP-EGCG-0.5%) >41.98% (SBP + EGCG) >38.65% (SBP) >25.85% (algal oil). Compared with SBP and SBP + EGCG, the Pickering high internal phase emulsion prepared from the sea bass protein-EGCG compound has better protection effect. This result indicates that a Pickering high internal phase emulsion delivery system stabilized by a sea bass protein-EGCG complex can increase the retention level of astaxanthin. In addition, increasing the concentration of the sea bass protein-EGCG complex can increase the protective effect of Pickering high internal phase emulsion on astaxanthin.
The conversion rate, bioassability index and bioassability of astaxanthin obtained from in vitro simulated digestion of the astaxanthin-loaded Pickering high internal phase emulsion are shown in FIG. 18.
As shown in fig. 18, the conversion rate, bioacessability index and bioacessability of astaxanthin were decreased as follows: SBP-EGCG-2% (conversion =67.80%, bioacessability index =70.81%, bioacessability = 48.01%) > SBP-EGCG-1.5% (conversion =66.66%, bioacessability index =69.98%, bioacessability = 46.65%), SBP-EGCG-1% (conversion =62.47%, bioacessability index =69.05%, bioacessability = 3579%) > SBP-EGCG-0.5% (conversion =61.11 ft%, bioacessability index = 3525%, bioacessability = 41.89%), SBP + EGCG (conversion = 3735 zxft 35%, bioacessability index =68.18%, bioacessability =38.15% > (conversion = 5253%, bioacessability index = 3856% 5253%), bioacessability index 5256.83%, bioacessability index = 3755%). Importantly, the bioassability of astaxanthin in Pickering high internal phase emulsions stabilized by SBP-EGCG complex was greatly improved and was positively correlated with the concentration of the complex.
Thus, the SBP-EGCG complex stabilized Pickering high internal phase emulsion can be used as an effective delivery system to improve the bioassability of astaxanthin.
The hydroperoxide content of the astaxanthin-loaded Pickering high internal phase emulsion after 15 days of storage at 50 ℃ is shown in figure 19.
As shown in FIG. 19, after 15 days of storage, the LH content of all samples was 93.39mmol/kg oil (algae oil) >85.42mmol/kg oil (SBP) >79.03mmol/kg oil (SBP + EGCG) >71.16mmol/kg oil (SBP) -EGCG-0.5%) >63.09mmol/kg oil (SBP-EGCG-1%) >38.64mmol/kg oil (SBP-EGCG-1.5%) >26.37mmol/kg oil (SBP-EGCG-2%). Compared with SBP and SBP + EGCG, the Pickering high internal phase emulsion prepared from the sea bass protein-EGCG compound has better protection effect. The results show that the Pickering high internal phase emulsion stabilized by the sea bass protein-EGCG compound can effectively prevent the oxidation of internal phase oil. In addition, increasing the concentration of the sea bass protein-EGCG complex can increase the protective effect of Pickering high internal phase emulsions on algal oil.
The malondialdehyde content of the astaxanthin-loaded Pickering high internal phase emulsion after 15 days storage at 50 ℃ is shown in figure 20.
As shown in FIG. 20, MDA content measurement results were similar to LH after all samples were stored at 50 ℃ for 15 days. The results show that Pickering high internal phase emulsions are effective in inhibiting the oxidation of algal oil compared to unencapsulated algal oil. Furthermore, the oxidation rate of Pickering high internal phase emulsions stabilized by SBP + EGCG blends was relatively slow compared to SBP, indicating that the presence of EGCG inhibited oxide production. As expected, the SBP-EGCG covalent complex effectively inhibited lipid oxidation of algal oil in Pickering high internal phase emulsions, and the higher the complex concentration, the better the protective effect on algal oil.
The astaxanthin-loaded Pickering high internal phase emulsion is subjected to 3D printing, the emulsion is loaded into a material barrel of a 3D printer, a computer program controls a machine, and the shape of 3D printed food is a symbol, and the result is shown in figure 21.
As shown in fig. 21, based on the above analysis of the rheological properties of the Pickering high internal phase emulsion, the potential of the astaxanthin-loaded Pickering high internal phase emulsion in 3D printed food was investigated. The results show that the printed pattern self-supporting ability of Pickering high internal phase emulsions stabilized by SBP + EGCG blends is relatively better than SBP. Although the pattern printed by the stable Pickering high internal phase emulsion with the SBP-EGCG content of 0.5 percent has better self-supporting property, the pattern outline definition is poorer. The "symbol" printed by Pickering high internal phase emulsion stabilized by higher concentrations of SBP-EGCG covalent complex has an intact shape, clear outline and high definition, and is able to retain the printed structure. Therefore, the stable astaxanthin-loaded Pickering high internal phase emulsion of the SBP-EGCG covalent compound has wide application value and prospect in 3D printing.
The appearance before and after centrifugation of the astaxanthin-loaded Pickering high internal phase emulsion and pork filling, which were uniformly stirred, is shown in FIG. 22.
As shown in fig. 22, the dumpling filling and Pickering high internal phase emulsion/algae oil were mixed in a filling to oil mass ratio of 10:1 and 5:1 evenly stir the back, the adhesion that the emulsion can be fine is fragrant on the meat, but the algae oil of not encapsulation can not adsorb in the meat filling completely to discover after the centrifugation, filling and oil are at 10:1, the stuffing added with the emulsion is basically not separated from oil, but partial oil is separated after the stuffing added with the unencapsulated oil is centrifuged; filling and oil in the ratio of 5:1, the filling with the emulsion had substantially a small amount of oil separated, but after centrifugation the filling with unencapsulated oil had mostly separated.
The astaxanthin-loaded Pickering high internal phase emulsion and the pork filling were uniformly stirred, and the oil retention level of the centrifuged filling is shown in FIG. 23.
As shown in fig. 23, the filling and oil are in the ratio of 10:1, the oil retention rate of the stuffing added with the emulsion is 81 percent, but the oil retention rate of the stuffing added with the unencapsulated oil is 33 percent after centrifugation; the mass ratio of the stuffing to the oil is 5: at 1, the filling oil percentage of the emulsion added was 67%, but the oil retention of the filling with unencapsulated oil after centrifugation was 21%. The result shows that the oil holding rate is reduced along with the increase of the oil proportion, but the emulsion can be well adhered to the stuffing after the oil is packaged by the emulsion, so that the defect of separation of the stuffing and the oil is reduced, and the stuffing can achieve better mouthfeel. Importantly, the Pickering high internal phase emulsion serving as an additive of the filling can endow special nutritional value to the dumplings, and further provides a favorable basis for the development of functional foods.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. A preparation method of Pickering high internal phase emulsion is characterized by comprising the following steps:
s1: preparing SBP solution from SBP, standing overnight, adding H into SBP solution 2 O 2 And vitamin C, incubating for 1-4 h, adding EGCG to obtain a mixed solution, adjusting the pH of the mixed solution, incubating for 24h, dialyzing the sample, and freeze-drying the content to obtain an SBP-EGCG covalent complex;
s2: and (3) preparing the SBP-EGCG covalent compound solution from the SBP-EGCG covalent compound in the step (S1), mixing the SBP-EGCG covalent compound solution with edible oil, and then shearing and emulsifying to obtain the Pickering high internal phase emulsion.
2. The method of claim 1, wherein the concentration of SBP in the SBP solution in S1 is 5-20 g/L, and the mass ratio of EGCG to SBP in S1 is 0.03-0.2.
3. The method of claim 1, wherein the pH of the mixture in S1 is in the range of 3 to 11.
4. The method of claim 1, wherein the concentration of SBP-EGCG covalent complex in the solution of SBP-EGCG covalent complex in S2 is between 0.5 and 2wt%.
5. The method of claim 1, wherein the volume ratio of the SBP-EGCG covalent complex solution to the edible oil is 4:6-1:9.
6. The method according to claim 1, wherein the shearing speed is 6000-12000 rpm, and the shearing time is 1-5 min.
7. A Pickering high internal phase emulsion made by the process of any one of claims 1-6.
8. Use of the Pickering high internal phase emulsion of claim 7 for embedding, loading or delivering a nutritional substance.
9. Use of the Pickering high internal phase emulsion of claim 7 in the field of 3D printed food.
10. Use of the Pickering high internal phase emulsion of claim 7 in a dumpling filling.
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