High-stability resveratrol lipid pickering emulsion, and preparation method and application thereof

By preparing lipid nanoparticles loaded with resveratrol from high-melting-point lipids and forming an antioxidant film layer, the problem of poor oxidative stability of the emulsion was solved, and the preparation and application of highly stable resveratrol lipid Pickering emulsion was achieved.

CN117958425BActive Publication Date: 2025-10-14SOUTH CHINA UNIV OF TECH
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Patent Information

Application Number
CN202311835704.6
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-12-28
Publication Date
2025-10-14
Estimated Expiration
2043-12-28

AI Technical Summary

Technical Problem

Existing emulsions have poor oxidative stability, especially at the oil-water interface, and existing technologies have failed to effectively utilize lipid nanoparticles loaded with natural antioxidants to construct oil-in-water emulsions with antioxidant activity.

Method used

Lipid nanoparticles were prepared by loading resveratrol with high melting point lipids. An antioxidant film layer was formed at the oil-water interface, combined with high-speed shearing and ultrasonic treatment to prepare a highly stable resveratrol lipid Pickering emulsion.

Benefits of technology

The oxidative stability and antioxidant properties of the emulsion are improved, the dispersibility and interfacial antioxidant activity of resveratrol are enhanced, and the emulsion is suitable for the fields of food, medicine and cosmetics.

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Abstract

The application discloses a high-stability resveratrol lipid Pickering emulsion and a preparation method thereof. The preparation method is as follows: (1) resveratrol is dissolved in anhydrous ethanol, mixed with high-melting-point lipids, heated to obtain an oil phase, edible emulsifiers are dissolved in distilled water, heated to obtain an aqueous phase, the aqueous phase is slowly poured into the oil phase and stirred, and then the mixed solution is subjected to high-speed shearing, ultrasonic treatment and cooling to obtain a resveratrol-loaded lipid nanoparticle dispersion; (2) the above particle dispersion is mixed with edible vegetable oil, and subjected to ultrasonic emulsification treatment to obtain the high-stability resveratrol lipid Pickering emulsion. The application has the advantages of convenient operation and mild conditions, the dispersibility of resveratrol is improved by means of the lipid nanoparticles, the oxidation stability of the food-grade lipid Pickering emulsion is greatly improved, and the application can be widely applied to the food, medicine and cosmetic industries.
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Description

Technical Field

[0001] The invention belongs to the technical field of emulsion preparation, and particularly relates to a highly stable resveratrol lipid Pickering emulsion and a preparation method and application thereof. Background Art

[0002] Emulsions are common in complex food systems, and the presence of an oil-water interface accelerates the interaction between the oil phase and pro-oxidants in the aqueous phase, resulting in lower oxidative stability of oils in emulsions than in pure oil systems. Most efforts to address the oxidation problem of emulsions have focused on adding antioxidants to the oil phase. However, research has shown that antioxidants exert a greater antioxidant effect at the emulsion interface than in the oil phase. Pickering emulsions, stabilized by solid particles instead of surfactants, have attracted widespread attention for their excellent physical stability. Because the irreversible adsorption of solid particles at the oil-water interface prevents the aggregation and merging of oil droplets, using them to load antioxidants is a novel and effective means of improving the oxidative stability of emulsions.

[0003] Compared to inorganic particles, food-grade lipid nanoparticles serve as safe and reliable delivery vehicles for encapsulating natural antioxidants such as resveratrol, curcumin, and paclitaxel, increasing the availability of functional ingredients while achieving a sustained, slow release. Studies have shown that lipid nanoparticles with excellent wetting properties form a "rigid membrane" by adsorbing at the oil-water interface and a "three-dimensional network" distributed in the continuous phase, providing a physical barrier to droplet aggregation and maintaining system stability. However, the use of lipid nanoparticles loaded with natural antioxidants to construct oil-in-water emulsions with antioxidant activity has not yet been reported. Summary of the Invention

[0004] In order to overcome the deficiencies and shortcomings of the prior art, the primary purpose of the present invention is to provide a method for preparing a highly stable resveratrol lipid Pickering emulsion. This preparation method uses high-melting-point lipids to load resveratrol to form lipid nanoparticles, which are used to prepare edible Pickering emulsions with high biosafety, strong antioxidant efficacy and good storage stability. The emulsion has broad development prospects in the fields of food, medicine and cosmetics.

[0005] The second object of the present invention is to provide a highly stable resveratrol lipid Pickering emulsion prepared by the above preparation method.

[0006] The third object of the present invention is to provide the application of the highly stable resveratrol lipid Pickering emulsion.

[0007] The primary purpose of the present invention is achieved through the following technical solutions:

[0008] The present invention provides a highly stable resveratrol lipid Pickering emulsion and a preparation method thereof, thereby solving the problem that natural antioxidants can exert a strong antioxidant effect on oils and fats at the emulsion interface layer.

[0009] The primary purpose of the present invention is achieved through the following solutions:

[0010] A method for preparing a highly stable resveratrol lipid Pickering emulsion comprises the following steps:

[0011] (1) Dissolving resveratrol in anhydrous ethanol, mixing with a high melting point lipid, and heating to obtain an oil phase; then dissolving an edible emulsifier in distilled water and heating to obtain an aqueous phase; slowly pouring the aqueous phase into the oil phase and stirring; then subjecting the mixture to high-speed shearing, ultrasonic treatment, and cooling to obtain a stable resveratrol lipid nanoparticle dispersion;

[0012] (2) adding edible vegetable oil to the resveratrol lipid nanoparticle dispersion, and obtaining a highly stable resveratrol lipid Pickering emulsion through shear premixing and ultrasonic dispersion;

[0013] In step (1), the mass concentration of resveratrol in the high melting point lipid is 1-3 wt.%; the mass concentration of the high melting point lipid in the dispersion is 0.5-20 wt.%; the mass concentration of the edible emulsifier in the aqueous phase is 0.5-6 wt.%;

[0014] The high melting point lipid in step (1) is a lipid with a melting point ≥ 46.9°C;

[0015] In step (2), the mass ratio of the resveratrol lipid nanoparticle dispersion to the edible vegetable oil is 7:3 to 9:1;

[0016] Steps (1) and (2) require light shielding throughout the entire process.

[0017] Preferably, the high melting point lipid is at least one of palm stearin and fully hydrogenated vegetable oil; the edible emulsifier is at least one of sodium caseinate and Tween series; the edible vegetable oil is at least one of low melting point animal and vegetable oils such as fish oil, corn oil, rapeseed oil, soybean oil, peanut oil, camellia oil, safflower oil, olive oil, walnut oil, sunflower oil, and linseed oil.

[0018] Preferably, the high melting point lipid is palm stearin.

[0019] Preferably, the heating in step (1) means that the water phase and the oil phase can reach similar temperatures under the premise of ensuring that the high melting point lipid is completely melted; the heating conditions are: temperature of 70-85°C, time of 20-35 minutes; the stirring in step (1) is magnetic stirring; the stirring conditions are: rotation speed of 100-200 rpm, time of 3-8 minutes.

[0020] Preferably, the high-speed shearing conditions in step (1) are: a rotation speed of 10,000 to 20,000 rpm, and a time of 1 to 5 minutes.

[0021] Preferably, the ultrasonic treatment conditions in step (1) are: power of 100 to 500 W, and time of 5 to 10 min.

[0022] Preferably, the cooling conditions in step (1) are: temperature of 4 to 37° C., and time of ≥24 h.

[0023] Preferably, the shear premixing conditions in step (2) are: a rotation speed of 10,000 to 14,000 rpm, and a time of 1 to 5 minutes.

[0024] Preferably, the ultrasonic dispersion conditions in step (2) are: power of 300-500W, time of 3-5 minutes.

[0025] The second object of the present invention is achieved through the following solutions:

[0026] A highly stable resveratrol lipid Pickering emulsion is prepared by the above preparation method.

[0027] The third object of the present invention is achieved through the following solutions:

[0028] A highly stable resveratrol lipid Pickering emulsion is used in the fields of food, medicine and cosmetics.

[0029] Compared with the prior art, the present invention has the following advantages and beneficial effects:

[0030] The highly stable resveratrol lipid Pickering emulsion of the present invention uses food-grade lipid as the particle base material, has convenient and mild preparation conditions, and is easy to achieve large-scale production; compared with synthetic antioxidants currently on the market, the natural active substance resveratrol greatly improves its nutritional value and safety.

[0031] The highly stable resveratrol lipid Pickering emulsion of the present invention has long been considered to have an emulsion interface that is a key location for oil oxidation. The resveratrol lipid nanoparticles have a distinct adsorption assembly structure of Pickering particles at the oil-water interface, which improves the poor dispersibility of resveratrol. The antioxidant activity at the interface has a certain degree of persistence and is less affected by fluctuations in external environmental factors.

[0032] The highly stable resveratrol lipid Pickering emulsion of the present invention has improved overall hydrophilicity and antioxidant properties of oils and fats, and lipid nanoparticles can self-assemble at the oil-water interface to form a monolayer or multilayer crystalline film to stably disperse oil droplets, which is also more conducive to addition and utilization in food, medicine and cosmetics. BRIEF DESCRIPTION OF THE DRAWINGS

[0033] Figure 1 (a) is a graph showing the POV values ​​of the highly stable resveratrol lipid Pickering emulsions (untreated) in Examples 1 and 2; (b) is a graph showing the TBARS values ​​of the highly stable resveratrol lipid Pickering emulsions (untreated) in Examples 1 and 2;

[0034] Figure 2 (a) is a graph showing the POV values ​​of the highly stable resveratrol lipid Pickering emulsions (with adjusted salt ion concentration) in Examples 1 and 2; (b) is a graph showing the TBARS values ​​of the highly stable resveratrol lipid Pickering emulsions (with adjusted salt ion concentration) in Examples 1 and 2;

[0035] Figure 3 (a) is a graph showing the POV values ​​of the highly stable resveratrol lipid Pickering emulsions (pH adjusted) in Examples 1 and 2; (b) is a graph showing the TBARS values ​​of the highly stable resveratrol lipid Pickering emulsions (pH adjusted) in Examples 1 and 2;

[0036] Figure 4 (a) is a graph showing the POV values ​​of the highly stable resveratrol lipid Pickering emulsions (untreated) in Examples 3 to 5 and Comparative Examples 1 and 2; (b) is a graph showing the TBARS values ​​of the highly stable resveratrol lipid Pickering emulsions (untreated) in Examples 3 to 5 and Comparative Examples 1 and 2. DETAILED DESCRIPTION

[0037] The present invention will be further described in detail below with reference to specific examples, but the embodiments of the present invention are not limited thereto. The materials used in the examples of the present invention can all be purchased commercially.

[0038] Example 1

[0039] Preparation of stable reed lipid nanoparticles: 0.15 parts by mass of resveratrol was dissolved in 10 ml of anhydrous ethanol, 4.85 parts by mass of palm stearin (PS) was added, and the temperature was raised to 80°C and kept at this temperature for 20-35 minutes to completely melt it. Then, it was slowly mixed with 95 parts by mass of a 2.0 wt.% sodium caseinate solution at a similar temperature, stirred at 150 rpm for 5 minutes, sheared at a speed of 13400 rpm for 2 minutes using a high-speed shearing machine, and then ultrasonically treated at a power of 400 W for 6 minutes. The mixture was placed in a 25°C water bath, stirred, cooled for 1 hour, removed, and stored at the same temperature for 24 hours for use, thereby preparing stable reed lipid nanoparticles.

[0040] Highly stable resveratrol lipid Pickering emulsion: the above lipid nanoparticle dispersion was diluted 5 times, mixed with flaxseed oil (FLO) at a mass ratio of 9:1, first treated with a high-speed shearing machine at 13400 rpm for 2 min, then treated with an ultrasonic dispersion device at 350 W for 4 min, and finally stored at 25 °C for 24 h for standby, to prepare a highly stable resveratrol lipid Pickering emulsion.

[0041] Accelerated oxidation experiment of Pickering emulsion under different external environmental factors.

[0042] Freshly prepared Pickering emulsion was added to an oxidation accelerator (1 mmol of ferric chloride, 1 mmol of vitamin C and 50 mmol of hydrogen peroxide) in a 1:1 (v / v) manner and oxidized for 3 days, and treated according to the following conditions: (1) adding 50 and 400 mM of sodium chloride; (2) adjusting the pH to 3, 7 and 11. The untreated lipid Pickering emulsion was the control group. The primary oxidation product (POV value) and the secondary oxidation product (TBARS value) were detected.

[0043] Determination of primary oxidation product (POV value): 0.2 mL of the lipid Pickering emulsion sample after accelerated oxidation was mixed with 1.5 mL of a mixture of isooctane / isopropyl alcohol (3:1, v / v), vortexed 3 times, each for 10 s, and then centrifuged at 10000 rpm for 10 min; 40 μL of the upper organic phase solution was mixed with 4.96 mL of a mixture of methanol / n-butanol (2:1, v / v), and then 100 μL of 3.94 mol / L ammonium thiocyanate solution and 100 μL of 0.144 mol / L ferrous chloride solution were added. The ferrous chloride solution was prepared by mixing equal amounts of 0.132 mol / L barium dichloride (dissolved in 0.4 mol / L hydrochloric acid solution) and 0.144 mol / L ferrous sulfate solution, and was used immediately after preparation. After shaking and mixing, the mixture was reacted in the dark for 20 min, and the absorbance was measured at 510 nm. A standard curve was prepared using benzene hydroperoxide as the standard.

[0044] Determination of secondary oxidation product (TBARS value): 1 mL of thiobarbituric acid reagent (15% (w / v) trichloroacetic acid and 0.375% (w / v) thiobarbituric acid reagent, and 0.25 M hydrochloric acid solution) was mixed with 0.5 mL of the lipid Pickering emulsion sample after accelerated oxidation, and then vortexed for 20 s. The resulting mixture was heated in a boiling water bath for 20 min, and the water bath was cooled to room temperature. The mixture was centrifuged at 10000 rpm for 10 min, and then stored in the dark for 10 min. The absorbance was read at 532 nm. The concentration of thiobarbituric acid was calculated using a 1,1,3,3-tetraethoxypropane standard curve.

[0045] The POV value of the food-grade lipid Pickering emulsion stabilized by resveratrol lipid nanoparticles (RSP) in this example is about 60 mmol / kg ( Figure 1 a), TBARS value is around 1mmol / kg ( Figure 1 b), which is significantly lower than that of the emulsion stabilized by empty lipid nanoparticles (SP). When salt ions are added to 50mM, the POV value is around 95mmol / kg ( Figure 2 a), TBARS value is around 26mmol / kg ( Figure 2 b), when the salt ion concentration was further increased to 400 mM, the POV value dropped to about 60 mmol / kg, indicating that the Pickering emulsion had a good inhibitory effect on the oxidation products of oils and fats at high salt ion concentrations. The change in pH did not affect the oxidative stability of the Pickering emulsion ( Figure 3 a&b).

[0046] Example 2

[0047] Preparation of stable resveratrol lipid nanoparticles: 0.15 parts by mass of resveratrol was dissolved in 10 ml of anhydrous ethanol, 4.85 parts by mass of palm stearin (PS) was added, and the temperature was raised to 80°C. The temperature was kept constant for 20-35 minutes to completely melt it. Then, it was slowly mixed with 95 parts by mass of a 2.0 wt.% sodium caseinate solution at a similar temperature, stirred at 150 rpm for 5 minutes, sheared at a speed of 13400 rpm for 2 minutes using a high-speed shearing machine, and then ultrasonically treated at a power of 400 W for 6 minutes. The mixture was placed in a 25°C water bath, stirred, cooled for 1 hour, taken out, and stored at the same temperature for 24 hours for use, thereby preparing stable resveratrol lipid nanoparticles.

[0048] Preparation of a highly stable resveratrol lipid Pickering emulsion: The above lipid nanoparticle dispersion was diluted 5 times, mixed with fish oil (FO) at a mass ratio of 9:1, first treated with a high-speed shearing machine at 13400 rpm for 2 minutes, then treated with an ultrasonic dispersion device at 350W for 4 minutes, and finally stored at 25°C for 24 hours to obtain a highly stable resveratrol lipid Pickering emulsion.

[0049] In this embodiment, the POV value and TBARS value of the food-grade lipid Pickering emulsion stabilized by resveratrol lipid nanoparticles (RSP) are about 60 mmol / kg ( Figure 1 a) and about 1mmol / kg ( Figure 1 b), similar to Example 1, and significantly lower than the emulsion stabilized by empty lipid nanoparticles (SP). Compared with the low salt ion concentration (50mM), the Pickering emulsion at a high salt ion concentration (400mM) reduced the POV value of oil to about 23mmol / kg ( Figure 2a). When the pH changes, the antioxidant activity of the Pickering emulsion in alkaline environment (pH=11) is stronger than that in acidic (pH=3) and neutral (pH=7) environments ( Figure 3 a&b).

[0050] Example 3

[0051] Preparation of stable resveratrol lipid nanoparticles: 0.15 parts by mass of resveratrol was dissolved in 10 ml of anhydrous ethanol, 4.85 parts by mass of palm stearin (PS) was added, and the temperature was raised to 80°C. The temperature was kept constant for 20-35 minutes to completely melt it. Then, it was slowly mixed with 95 parts by mass of a 2.0 wt.% sodium caseinate solution at a similar temperature, stirred at 150 rpm for 5 minutes, sheared at a speed of 13400 rpm for 2 minutes using a high-speed shearing machine, and then ultrasonically treated at a power of 400 W for 6 minutes. The mixture was placed in a 25°C water bath, stirred, cooled for 1 hour, taken out, and stored at the same temperature for 24 hours for use, thereby preparing stable resveratrol lipid nanoparticles.

[0052] Preparation of a highly stable resveratrol lipid Pickering emulsion: The above lipid nanoparticle dispersion was diluted 5 times and mixed with corn oil (CO) at a mass ratio of 9:1. The mixture was first treated with a high-speed shearing machine at 13400 rpm for 2 minutes, then treated with an ultrasonic dispersion device at 350W for 4 minutes, and finally stored at 25°C for 24 hours to obtain a highly stable resveratrol lipid Pickering emulsion.

[0053] The POV value of the Pickering emulsion stabilized by resveratrol lipid nanoparticles (RSP) in this example is about 65.5 mmol / kg ( Figure 4 a), TBARS value is around 0.2mmol / kg ( Figure 4 b), the POV value (60 mmol / kg) and TBARS value (1 mmol / kg) of the food-grade lipid Pickering emulsion stabilized by resveratrol lipid nanoparticles (RSP) in Example 1 and Example 2 are slightly different ( Figure 1 a&b), which may be because the difference in the internal phase oil composition will have a certain impact on the antioxidant effect provided by the palm stearin-based particles. Overall, the Pickering emulsions in Examples 1 to 3 all have good oxidative stability.

[0054] Example 4

[0055] Preparation of stable resveratrol lipid nanoparticles: 0.15 parts by mass of resveratrol was dissolved in 10 ml of anhydrous ethanol, 4.85 parts by mass of palm stearin (PS) was added and warmed to 80°C, and then kept at a constant temperature for 20-35 min to completely melt it. Then, it was slowly mixed with 95 parts by mass of a 4.0 wt.% sodium caseinate solution at a similar temperature, stirred at 150 rpm for 5 min, sheared at a speed of 13400 rpm for 2 min using a high-speed shearing machine, and then treated with ultrasonic waves at a power of 400 W for 6 min. It was then placed in a 25°C water bath, stirred and cooled for 1 h, taken out, and stored at the same temperature for 24 h to prepare stable resveratrol lipid nanoparticles.

[0056] Preparation of resveratrol lipid Pickering emulsion with high stability: the above-mentioned lipid nanoparticle dispersion was diluted 5 times, mixed with corn oil (CO) at a mass ratio of 9:1, first treated with a high-speed shearing machine at 13400 rpm for 2 min, then treated with an ultrasonic dispersion device at 350 W for 4 min, and finally stored at 25°C for 24 h to prepare a resveratrol lipid Pickering emulsion with high stability.

[0057] The Pickering emulsion in Example 3 used a 2.0 wt.% sodium caseinate solution, and the POV value was about 65.5 mmol / kg ( Figure 4 a), and the TBARS value was about 0.2 mmol / kg ( Figure 4 b). As the concentration of the sodium caseinate emulsifier increased to 4.0 wt.%, the POV value of the food-grade lipid Pickering emulsion stabilized by the resveratrol lipid nanoparticles (R-S-P) in this example increased slightly, and the TBARS value decreased slightly ( Figure 4 a&b), but the oxidative stability was still within an acceptable range, indicating that the antioxidant effect provided by the palm stearin particles was not greatly affected by changes in the concentration of the sodium caseinate emulsifier.

[0058] Example 5

[0059] Preparation of stable resveratrol lipid nanoparticles: 0.15 parts by mass of resveratrol was dissolved in 10 ml of anhydrous ethanol, 4.85 parts by mass of palm stearin (PS) was added and warmed to 80°C, and then kept at a constant temperature for 20-35 min to completely melt it. Then, it was slowly mixed with 95 parts by mass of a 4.0 wt.% sodium caseinate solution at a similar temperature, stirred at 150 rpm for 5 min, sheared at a speed of 13400 rpm for 2 min using a high-speed shearing machine, and then treated with ultrasonic waves at a power of 400 W for 6 min. It was then placed in a 25°C water bath, stirred and cooled for 1 h, taken out, and stored at the same temperature for 24 h to prepare stable resveratrol lipid nanoparticles.

[0060] Preparation of the stable resveratrol lipid nanoparticles: 0.15 parts by mass of resveratrol was dissolved in 10 ml of anhydrous ethanol, and 4.85 parts by mass of fully hydrogenated soybean oil (HSO) was added and warmed to 80°C. The mixture was completely melted at a constant temperature of 20-35 min, and then slowly mixed with 95 parts by mass of a 2.0 wt.% sodium caseinate solution at a similar temperature. The mixture was stirred at 150 rpm for 5 min, sheared at a speed of 13400 rpm using a high-speed shearing machine for 2 min, and then treated with ultrasound at a power of 400 W for 6 min. The mixture was placed in a 25°C water bath and stirred to cool for 1 h, and then stored at the same temperature for 24 h to prepare the stable resveratrol lipid nanoparticles.

[0061] There was no significant difference in the POV value and TBARS value of the food-grade lipid Pickering emulsion stabilized by the resveratrol lipid nanoparticles (R-S-P) in this example when a 2.0 wt.% or 4.0 wt.% Tween 40 solution was used Figure 4 a&b), which was similar to the regularity shown by the antioxidant results of the Pickering emulsions with different concentrations of sodium caseinate in Example 3 and Example 4. According to Example 3 to Example 5, it can be seen that the different types of emulsifiers have little effect on the antioxidant effect provided by the palm stearin type particles.

[0062] Comparative Example 1

[0063] Preparation of the stable resveratrol lipid nanoparticles: 0.15 parts by mass of resveratrol was dissolved in 10 ml of anhydrous ethanol, and 4.85 parts by mass of fully hydrogenated soybean oil (HSO) was added and warmed to 80°C. The mixture was completely melted at a constant temperature of 20-35 min, and then slowly mixed with 95 parts by mass of a 2.0 wt.% sodium caseinate solution at a similar temperature. The mixture was stirred at 150 rpm for 5 min, sheared at a speed of 13400 rpm using a high-speed shearing machine for 2 min, and then treated with ultrasound at a power of 400 W for 6 min. The mixture was placed in a 25°C water bath and stirred to cool for 1 h, and then stored at the same temperature for 24 h to prepare the stable resveratrol lipid nanoparticles.

[0064] Preparation of the stable resveratrol lipid nanoparticles: 0.15 parts by mass of resveratrol was dissolved in 10 ml of anhydrous ethanol, and 4.85 parts by mass of fully hydrogenated soybean oil (HSO) was added and warmed to 80°C. The mixture was completely melted at a constant temperature of 20-35 min, and then slowly mixed with 95 parts by mass of a 2.0 wt.% sodium caseinate solution at a similar temperature. The mixture was stirred at 150 rpm for 5 min, sheared at a speed of 13400 rpm using a high-speed shearing machine for 2 min, and then treated with ultrasound at a power of 400 W for 6 min. The mixture was placed in a 25°C water bath and stirred to cool for 1 h, and then stored at the same temperature for 24 h to prepare the stable resveratrol lipid nanoparticles.

[0065] The POV value of the food-grade lipid Pickering emulsion stabilized by the resveratrol lipid nanoparticles (R-S-P) in this comparative example was about 184.3 mmol / kg Figure 4 a), and the TBARS value was about 1.6 mmol / kg Figure 4 b), which was much higher than that in Example 3 and Example 4, and the emulsion had the worst oxidative stability. Under the same conditions (including the oil in the inner phase, the emulsifier, etc.), the fully hydrogenated soybean oil type particles provided a stronger antioxidant effect than the palm stearin type particles.

[0066] Comparative Example 2

[0067] Preparation of stable resveratrol lipid nanoparticles: 0.15 parts by mass of resveratrol was dissolved in 10 ml of anhydrous ethanol, 4.85 parts by mass of hydrogenated soybean oil (HSO) was added and warmed to 80°C, and then allowed to completely melt for 20-35 min, and then slowly mixed with 95 parts by mass of a 4.0 wt.% sodium caseinate solution at a similar temperature, stirred at 150 rpm for 5 min, sheared at 13400 rpm using a high-speed shearing machine for 2 min, and then subjected to ultrasonic treatment at 400 W for 6 min, and then placed in a 25°C water bath and stirred to cool for 1 h, and then stored at the same temperature for 24 h to prepare stable resveratrol lipid nanoparticles.

[0068] Preparation of resveratrol lipid Pickering emulsion with high stability: the above-mentioned resveratrol lipid nanoparticle dispersion was diluted 5-fold, mixed with corn oil (CO) at a mass ratio of 9:1, first treated using a high-speed shearing machine at 13400 rpm for 2 min, then treated using an ultrasonic dispersion device at 350 W for 4 min, and finally stored at 25°C for 24 h to prepare a resveratrol lipid nanoparticle (R-S-P) stabilized food-grade lipid Pickering emulsion.

[0069] Analysis of the results of Comparative Example 1 Figure 4 a&b), the POV value and the TBARS value of the resveratrol lipid nanoparticle (R-S-P) stabilized food-grade lipid Pickering emulsion of this comparative example decreased significantly Figure 4 a&b), but the overall antioxidant properties of the emulsion still could not reach the same level of stability as in Example 3 and Example 4. At the same time, compared with the palm stearin type particles, the antioxidant effect provided by the hydrogenated soybean oil type particles was also easily disturbed by changes in the concentration of the emulsifier.

[0070] In summary, from Example 1 to Example 5 and Comparative Example 1 to Comparative Example 2, it can be seen that the antioxidant effect of the resveratrol lipid Pickering emulsion Pickering emulsion directly depends on the base type of the resveratrol lipid nanoparticles, and the influence of the internal phase oil and the emulsifier also depends on the base type; under changes in external environmental factors, the antioxidant effect provided by the palm stearin type particles is of high quality and stable.

[0071] The above examples are preferred embodiments of the present application, but the embodiments of the present application are not limited by the above examples, and any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present application should be equivalent replacement methods, and are all included in the protection scope of the present application.

Claims

1. A method for preparing a highly stable resveratrol lipid Pickering emulsion, characterized in that: The following steps are involved: (1) Resveratrol is first dissolved in anhydrous ethanol, mixed with a high melting point lipid, and then heated to obtain an oil phase. An edible emulsifier is then dissolved in distilled water and heated to obtain an aqueous phase. The aqueous phase is slowly poured into the oil phase and stirred. The mixture is then subjected to high-speed shearing, ultrasonic treatment, and cooling to obtain a stable resveratrol lipid nanoparticle dispersion. (2) Adding edible oil to the resveratrol lipid nanoparticle dispersion, followed by shear premixing and ultrasonic dispersion, to obtain a highly stable resveratrol lipid Pickering emulsion; In step (1), the mass concentration of resveratrol in the high melting point lipid is 1-3 wt %; the mass concentration of the high melting point lipid in the dispersion is 0.5-20 wt %; the mass concentration of the edible emulsifier in the aqueous phase is 0.5-6 wt %; The high melting point lipid in step (1) is a lipid with a melting point ≥ 46.9°C; In step (2), the mass ratio of the resveratrol lipid nanoparticle dispersion to the edible oil is 7:3 to 9:1; Steps (1) and (2) require shading throughout the process; The high melting point lipid is at least one of palm stearin and fully hydrogenated vegetable oil; the edible emulsifier is at least one of sodium caseinate and Tween series; the edible oil is at least one of fish oil, corn oil, rapeseed oil, soybean oil, peanut oil, camellia oil, safflower oil, olive oil, walnut oil, sunflower oil, and linseed oil.

2. The method for preparing the highly stable resveratrol lipid Pickering emulsion according to claim 1, wherein: The heating in step (1) refers to ensuring that the high-melting-point lipid is completely melted, so that the water phase and the oil phase reach similar temperatures; the heating conditions are: temperature of 70~85°C, time of 20~35 min; the stirring in step (1) is magnetic stirring; the stirring conditions are: rotation speed of 100~200 rpm, time of 3~8 min.

3. The method for preparing the highly stable resveratrol lipid Pickering emulsion according to claim 1, wherein: The high-speed shearing conditions in step (1) are: a rotation speed of 10,000 to 20,000 rpm, and a time of 1 to 5 minutes.

4. The method for preparing the highly stable resveratrol lipid Pickering emulsion according to claim 1, wherein: The ultrasonic treatment conditions in step (1) are as follows: power of 100-500 W and time of 5-10 min.

5. The method for preparing the highly stable resveratrol lipid Pickering emulsion according to claim 1, wherein: The cooling conditions in step (1) are: temperature of 4-37°C and time of ≥24 h.

6. The method for preparing the highly stable resveratrol lipid Pickering emulsion according to claim 1, wherein: The shear premixing conditions in step (2) are: a rotation speed of 10,000 to 14,000 rpm and a time of 1 to 5 minutes.

7. The method for preparing the highly stable resveratrol lipid Pickering emulsion according to claim 1, characterized in that: The conditions for ultrasonic dispersion in step (2) are: power of 300-500 W, time of 3-5 min.

8. A highly stable resveratrol lipid Pickering emulsion, characterized in that: Prepared according to the preparation method according to any one of claims 1 to 7.

9. Use of the highly stable resveratrol lipid Pickering emulsion according to claim 8 in the preparation of food, medicine and cosmetics.

Citation Information

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