Mirabilis jalapa endosperm powder Pickering emulsion as well as preparation method and application thereof

Abstract

The invention relates to the field of Pickering emulsion, and particularly discloses mirabilis jalapa endosperm powder Pickering emulsion as well as a preparation method and application thereof. The mirabilis jalapa endosperm powder Pickering emulsion is prepared from the following raw materials in percentage by weight: 1 to 10 percent of mirabilis jalapa endosperm powder particles, 10 to 70 percent of grease and the balance of water. The mirabilis jalapa endosperm powder Pickering emulsion can be used in the field of cosmetics, and has the advantages of good heat resistance and cold resistance, excellent long-term stability, capability of emulsifying polar oil and non-polar oil at the same time, and no conflict with a thickening agent.

Description

Technical Field

[0001] This application relates to the field of Pickering emulsion preparation technology, and more specifically, to a Pickering emulsion made from four o'clock flower endosperm powder, its preparation method, and its application. Background Technology

[0002] An emulsion is a homogeneous system in which the dispersed phase is dispersed as droplets within a continuous phase. From a thermodynamic perspective, emulsions are unstable systems and will demulsify over time under the influence of various factors. To ensure the long-term stability of emulsions, emulsifiers are typically added during their preparation to improve stability. Pickering emulsions are a novel type of emulsion prepared using ultrafine solid particles or solid colloidal particles instead of traditional surfactants as emulsifiers. They offer advantages such as good stability, ease of control, environmental friendliness, low cost, and relative safety and non-toxicity, and are widely used in various fields including pharmaceuticals, food, petroleum, water treatment, and cosmetics.

[0003] In the prior art, Chinese invention patent application CN201180060001X discloses a new particle-stabilized emulsion or foam comprising at least two phases and a plurality of solid particles, wherein the solid particles are starch granules and the starch granules or a portion thereof are located at the interface between the two phases, and the starch granules undergo physical modification and / or chemical modification to increase the hydrophobicity of these starch granules.

[0004] When starch granules are used in the above emulsions, the starch granules need to be physically or chemically modified to increase their hydrophobicity, which is a complicated process. Moreover, the gelatinization temperature of starch is generally below 70°C, which cannot withstand pasteurization, making the resulting emulsions unsuitable for applications requiring heating. In addition, starch granules themselves cannot simultaneously emulsify polar and non-polar oils, resulting in oil phase limitations.

[0005] In response to the aforementioned technologies, the inventors discovered an urgent need for a Pickering emulsion that can simultaneously emulsify polar and non-polar oils and has excellent heat resistance. Summary of the Invention

[0006] In order to make Pickering have excellent thermal stability and no oil phase limitation, this application provides a Pickering emulsion of four o'clock flower endosperm powder, its preparation method and application.

[0007] In a first aspect, this application provides a Pickering emulsion of four o'clock flower endosperm powder, which adopts the following technical solution: a four o'clock flower endosperm powder Pickering emulsion, comprising the following raw materials by weight percentage: 1-10% four o'clock flower endosperm powder particles, 10-70% oil, and water to make up to 100%.

[0008] By adopting the above technical solution, the main components of the four o'clock flower endosperm powder are starch, protein and a small amount of polysaccharide / lipid. It is amphiphilic and can be closely arranged at the oil-water interface to form a physical barrier, preventing droplet aggregation and thus improving the stability of the emulsion. The gelatinization temperature of the four o'clock flower endosperm powder is greater than 80℃, and it can still maintain the particle shape and interfacial adsorption capacity under high temperature environment, so that the emulsion exhibits good heat resistance.

[0009] Optionally, the four o'clock flower endosperm powder Pickering emulsion comprises the following ingredients by weight percentage: 8% four o'clock flower endosperm powder particles, 48% oil, and water to make up to 100%.

[0010] Optionally, the particle size D50 of the four o'clock flower endosperm powder Pickering emulsion is <20 μm.

[0011] By adopting the above technical solutions, the finished Pickering emulsion has a small particle size, which can slow down the tendency of droplets to settle or float under gravity and extend the storage stability period of the emulsion. Moreover, the smaller droplet size results in a larger specific surface area, allowing the Mirabilis endosperm powder particles to cover the droplet surface more evenly, forming a denser particle film. At the same time, the probability of collision between droplets is high, and the particle film is more resistant to deformation caused by collisions, reducing the risk of droplet coalescence. The larger specific surface area of ​​the droplets can accommodate more functional ingredients. Furthermore, the smaller particle size of the Pickering emulsion results in a purer color, appearing milky white, with no obvious particle texture, and superior visual and tactile qualities.

[0012] Optionally, the oil is selected from at least one of isododecane, isohexadecane, squalane, isopropyl myristate, phosphatidylcholine, phosphatidylethanolamine, caprylic / capric triglyceride, isononyl isononanoate, dioctyl carbonate, diethylhexyl carbonate, pentaerythritol tetraisostearate, propylene glycol caprylic / capric acid ester, neopentyl glycol diheptanoate, green tea seed oil, jojoba seed oil, macadamia nut oil, argan oil, shea butter, cyclomethyl silicone oil (D4, D5), dimethyl silicone oil (5cst polydimethylsiloxane), polyphenyl silicone oil (phenyl polytrimethylsiloxane), octyl methoxycinnamate, and alkyl-modified silicone oil (octyl polymethylsiloxane).

[0013] Optionally, the particle size of the four o'clock flower endosperm powder is 0.5-2.0 μm.

[0014] By adopting the above technical solution, the four o'clock endosperm powder particles with a particle size of 0.5-2.0μm can be effectively adsorbed onto the interface of tiny oil droplets or water droplets, while not detaching from the interface due to Brownian motion, thus forming an extremely stable interface film.

[0015] Optionally, the raw materials of the four o'clock flower endosperm powder Pickering emulsion may also include 1-3% thickener.

[0016] By adopting the above technical solution, the thickener can increase the viscosity of the aqueous phase, slow down the movement speed of oil droplets, effectively prevent stratification, maintain the uniform appearance of the emulsion, and improve long-term stability.

[0017] Optionally, the thickener is selected from at least one of hydroxycellulose, xanthan gum, gellan gum, hyaluronic acid, magnesium aluminum silicate, acrylate, carbomer, potassium chloride, succinyl polysaccharide, and polyacrylamide.

[0018] Optionally, the raw materials for the four o'clock flower endosperm powder Pickering emulsion also contain preservatives.

[0019] By adopting the above technical solutions, the preservatives can play an antibacterial role, enhance the antibacterial ability of the emulsion, and improve storage stability.

[0020] Optionally, the preservative is selected from at least one of phenoxyethanol, hexanediol, p-hydroxyacetophenone, ethylhexylglycerin, capryloyl hydroxamic acid, caprylic acid glyceride, and sodium benzoate.

[0021] Optionally, the four o'clock flower endosperm powder Pickering emulsion comprises the following ingredients by weight percentage: 6.25% four o'clock flower endosperm powder particles, 18.75% oil, 0.05% thickener, 0.8% preservative, and water to make up to 100%.

[0022] Secondly, this application provides a method for preparing Pickering emulsion from Mirabilis jalapa endosperm powder, using the following technical solution: A method for preparing Pickering emulsion from Mirabilis jalapa endosperm powder includes the following steps: The endosperm particles of Mirabilis jalapa were dispersed in water, ultrasonicated, and homogenized to form a suspension. An oil phase was added to the suspension and homogenized to obtain a Pickering emulsion.

[0023] By adopting the above technical solution, the endosperm powder particles of Mirabilis jalapa are ultrasonically and homogenized to form a suspension. Then, an oil phase is added, followed by homogenization and emulsification, or further high-pressure homogenization / ultrasonic emulsification, to further adjust the emulsion particle size and produce an emulsion with stable structure and small particle size.

[0024] Optionally, the method for preparing the Pickering emulsion containing thickeners and preservatives includes the following steps: The four o'clock flower endosperm particles and preservatives were dispersed in water, homogenized, and formed a suspension. Add xanthan gum to water and stir to dissolve it into a gel; The gel was added to the suspension, homogenized, and then the oil phase was added and homogenized again to obtain the Pickering emulsion.

[0025] By adopting the above technical solution, adding xanthan gum and preservatives to the emulsion does not affect the rheology and stability of the emulsion, has good compatibility with additives, and does not cause additive conflicts.

[0026] Thirdly, this application provides an application of a four o'clock flower endosperm powder Pickering emulsion for loading fat-soluble ingredients or sunscreens in cosmetics.

[0027] By adopting the above technical solutions, the cosmetics industry can be used to target children, sensitive skin, and high-end consumers who seek pure and natural beauty.

[0028] Optionally, the fat-soluble active ingredient is selected from at least one of vitamins, retinyl palmitate, tea polyphenols, and flavonoids; the sunscreen agent is selected from at least one of avobenzone, octocrylene, and ethyl methoxycinnamate.

[0029] Optionally, the fat-soluble component accounts for 1% of the total weight of the Pickering emulsion of Mirabilis jalapa endosperm powder loaded with the fat-soluble component, and the sunscreen agent accounts for 10-68.6% of the total weight of the Pickering emulsion of Mirabilis jalapa endosperm powder loaded with the sunscreen agent.

[0030] Optionally, in the Pickering emulsion of four o'clock flower endosperm powder loaded with fat-soluble components, the mass ratio of four o'clock flower endosperm powder to fat-soluble active ingredients is 7:1.

[0031] Optionally, in the Pickering emulsion loaded with sunscreen, the four o'clock flower endosperm powder accounts for 2% of the total weight of the emulsion, and the sunscreen accounts for 68.6%.

[0032] In summary, this application has the following beneficial effects: 1. Because this application uses four o'clock flower endosperm powder particles with high gelatinization temperature as a stabilizer, the Pickering emulsion maintains structural stability during high-temperature processing (such as pasteurization, hot melt formulation, etc.), avoiding emulsion demulsification caused by gelatinization. It is suitable for heat-processing formulations and heat treatment sterilization processes. Moreover, four o'clock flower endosperm powder particles have high emulsifying activity and can stably emulsify a variety of oils. It is suitable for different polar oil phases, which is in line with the "Clean Beauty" trend. It can be used in cosmetics and is suitable for high-end fields such as sensitive skin and infant formula.

[0033] 2. The Mirabilis jalapa endosperm powder particles in this application are compatible with thickeners (such as xanthan gum) and preservatives (such as hexanediol and p-hydroxyacetophenone), and do not affect the rheology and stability of the emulsion, thus broadening the application scenarios and facilitating formula optimization.

[0034] 3. The Mirabilis endosperm powder particles prepared in this application can form a dense interfacial film at the oil-water interface, which can efficiently encapsulate heat-sensitive or photosensitive active ingredients, form a physical barrier, reduce oxidation and photodegradation, improve bioavailability, and stably encapsulate organic sunscreens, reduce stickiness, slow down photodegradation and skin penetration, and improve SPF durability. Compared with synthetic polymers (such as PLGA and polyvinyl alcohol), it has the advantages of being non-toxic, biodegradable, and suitable for children and sensitive skin. Attached Figure Description

[0035] Figure 1 Particle size distribution diagram of the four o'clock endosperm powder particles prepared for Example I.

[0036] Figure 2 This is a particle size distribution diagram of the corn starch used in Comparative Example 1.

[0037] Figure 3 Morphological diagram of the four o'clock endosperm powder particles prepared for Example I dispersed in the water and oil phases.

[0038] Figure 4 A comparison chart of the gelatinization temperatures of the four o'clock flower endosperm powder granules and corn starch prepared in Example I.

[0039] Figure 5 The images show the appearance of the Pickering emulsions prepared in Example 1 and Comparative Example 1.

[0040] Figure 6 Microscopic images of the Pickering emulsions prepared in Example 1 and Comparative Example 1.

[0041] Figure 7 This is a comparison chart showing the high and low temperature resistance of the Pickering emulsion prepared in Example 1.

[0042] Figure 8 The particle size distribution diagram is shown for the Pickering emulsion prepared in Example 3.

[0043] Figure 9 This is a comparison chart showing the effect of different homogenization methods on the particle size of Pickering emulsions.

[0044] Figure 10 Appearance of Pickering emulsions prepared in Examples 3 and 4 (Left: Example 4, Right: Example 3).

[0045] Figure 11 This is an image of the appearance of the vitamin E-loaded Pickering emulsion prepared using Example I-1.

[0046] Figure 12 Microscopic image of the vitamin E-loaded Pickering emulsion prepared using Example I-1.

[0047] Figure 13 The images show the appearance and microscopic view of sunscreen products A and G (a is sunscreen product G, b is sunscreen product A). Detailed Implementation

[0048] The following embodiments provide a further detailed description of this application.

[0049] Example I: Preparation of Mirabilis jalapa endosperm powder granules Preparation Example I: Four o'clock seeds were shelled to obtain a first mixture of outer shell, seed coat, embryo coat, and endosperm blocks. The roller spacing of the shelling equipment was 6.5 mm. The first mixture was received and separated using a rice bran separator with a vibration frequency of 249 times / second and a horizontal inclination angle of 16°, resulting in a second mixture of seed coat, embryo coat, and endosperm blocks. The seed coat and embryo coat of the second mixture were separated at an air velocity of 2.5 m / s to obtain endosperm blocks with a particle size of 3 mm. The blocks were then pulverized at a speed of 15000 r / min for 20 s to obtain coarse endosperm powder. This powder was then subjected to air jet milling with a feed pressure of 0.3 MPa. By adjusting the air pressure, four o'clock endosperm powder particles with a particle size of 0.5-2 μm were obtained. The particle size distribution is shown in the figure below. Figure 1 As shown.

[0050] Take an appropriate amount of corn starch and test its particle size. The particle size distribution is as follows: Figure 2 As shown, comparison Figure 1 and Figure 2 It is evident that the particle size of the four o'clock flower endosperm powder is smaller.

[0051] Take 1g of 1.2μm four o'clock endosperm powder particles, add them to 10mL of water, then sonicate for 2min, and homogenize at 3000r / min for 2min. Figure 3 As shown in the left figure; take 1g of four o'clock flower endosperm powder particles with a particle size of 2μm, add them to 10mL of jojoba seed oil, sonicate for 2min using the same method, and homogenize at 3000r / min for 2min. Figure 3 As shown in the figure on the right.

[0052] Depend on Figure 2 It is evident that the four o'clock flower endosperm powder particles can be evenly dispersed in the water and oil phases, being both hydrophilic and lipophilic, and can be used in O / W formulations, W / O formulations, and wax formulations.

[0053] Take four o'clock flower endosperm powder and corn starch, and use differential scanning calorimetry (DSC) to determine the gelatinization temperature of the four o'clock flower endosperm powder particles and corn starch particles, such as... Figure 4 As shown, Figure 4The data shows that the initial gelatinization temperature of the four o'clock flower endosperm powder is 80.39℃, the peak gelatinization temperature is 96.76℃, and the termination gelatinization temperature is 113.4℃. The initial gelatinization temperature of corn starch is 52.09℃, the peak gelatinization temperature is 65.06℃, and the termination gelatinization temperature is 70.81℃. It can be seen that the four o'clock flower endosperm powder in this application has a higher gelatinization temperature and better heat resistance, thereby improving the heat resistance stability of Pickering emulsion.

[0054] The components of the four o'clock flower endosperm powder were tested, and the results are as follows: protein 1.41g / 100g, fat 0.4g / 100g, moisture 7.78g / 100g, ash 0.2g / 100g, dietary fiber 1.2g / 100g, and carbohydrates 89g / 100g. Protein content was determined using the Kjeldahl method, fat using the Soxhlet extraction method, moisture using the direct drying method, dietary fiber using a colorimetric method, and carbohydrates using the Pasteur reaction method. The flavonoid content was also determined to be 849mg / kg using high-performance liquid chromatography. Example

[0055] Example 1: A method for preparing a Pickering emulsion from Mirabilis jalapa endosperm powder, comprising the following steps: 8g of four o'clock endosperm powder particles were added to 44g of water, ultrasonically dispersed at 250W for 2min, and then homogenized at 3000r / min for 2min to obtain a suspension. The four o'clock endosperm powder particles were prepared by Preparation Example I and had a particle size of 1.2μm. Add 48g of oil phase to the suspension and homogenize at 6000r / min for 3min to form a Pickering emulsion. The oil phase is jojoba seed oil.

[0056] Figure 5 Appearance of the emulsion prepared in Example 1.

[0057] The emulsions prepared in Example 1 were placed in screw-top bottles, sealed, and placed at 50°C and -18°C respectively. The changes in the emulsions after 5 weeks of storage were observed. Figure 7 As can be seen, the Pickering emulsion prepared using natural four o'clock endosperm powder particles in Example 1 was relatively stable after being placed at 50°C and -18°C for 5 weeks, and no oil-water separation occurred.

[0058] Example 2: A method for preparing a Pickering emulsion of four o'clock flower endosperm powder, comprising the following steps: adding 8g of four o'clock flower endosperm powder particles to 44g of water, ultrasonically dispersing at 250W for 2min, and then homogenizing at 3000r / min for 2min to obtain a suspension. The four o'clock flower endosperm powder particles are prepared from Preparation Example I and have a particle size of 1.2μm. Add 48g of oil phase to the suspension and mix. Homogenize at 6000r / min for 5min to form a Pickering emulsion. The oil phase contains jojoba seed oil and caprylic / capric triglycerides in a mass ratio of 1:1.

[0059] Example 3: A method for preparing a Pickering emulsion from Mirabilis jalapa endosperm powder, comprising the following steps: 73.2g of water and 0.8g of phenoxyethanol were stirred evenly, and 6.25g of four o'clock endosperm powder particles were added. The mixture was homogenized at 3000r / min for 10min to obtain a suspension. The four o'clock endosperm powder particles were prepared from Preparation Example I and had a particle size of 1.2μm. Add 5g xanthan gum to 95g water, stir to dissolve, and form a gel; Add 1g of gel to the suspension and homogenize at 5000r / min for 3min. Add 18.75g of oil phase and homogenize at 6000r / min for 3min. The oil phase is jojoba seed oil.

[0060] The particle size distribution of the Pickering emulsion prepared in Example 3 is shown in Figure 8. It can be seen that the D50 of the prepared Mirabilis endosperm powder Pickering emulsion is 10.63 μm, and the microscopic image is shown below. Figure 9 As shown in (a), the Pickering emulsion of Mirabilis jalapa endosperm powder prepared in Example 3 was ultrasonically emulsified at 80% power for 2 minutes, and the resulting microscopic image of the emulsion is shown below. Figure 9 (b) shows the result of homogenizing the Pickering emulsion of Mirabilis jalapa endosperm powder prepared in Example 3 under high pressure at 500 Pa for 3 min. The resulting emulsion is shown in the microscope image. Figure 9 As shown in (c), it can be seen that ordinary homogenization can achieve the level of microemulsion, and further high-pressure homogenization or ultrasonic emulsification can be used to produce emulsions with finer particle sizes.

[0061] Example 4: A method for preparing a Pickering emulsion from Mirabilis jalapa endosperm powder, comprising the following steps: 73.2g of water and 0.8g of phenoxyethanol were stirred evenly, and 6.25g of four o'clock endosperm powder particles were added. The mixture was homogenized at 3000r / min for 10min to obtain a suspension. The four o'clock endosperm powder particles were prepared from Preparation Example I and had a particle size of 1.2μm. Add 18.75g of oil phase to the suspension and homogenize at 6000r / min for 3min. The oil phase is jojoba seed oil.

[0062] The Pickering emulsions prepared in Examples 3 and 4 have the following appearance: Figure 10 As shown, the absence of xanthan gum makes it easy for water and emulsion to separate into layers.

[0063] Example 5: A method for preparing a Pickering emulsion of four o'clock flower endosperm powder, comprising the following steps: 73.2g of water and 0.8g of phenoxyethanol were stirred evenly, and 6.25g of four o'clock endosperm powder particles were added. The mixture was homogenized at 3000r / min for 10min to obtain a suspension. The four o'clock endosperm powder particles were prepared from Preparation Example 1. Add 5g xanthan gum to 95g water, stir to dissolve, and form a gel; Add 1g of gel to the suspension and homogenize at 5000r / min for 3min. Add 18.75g of oil phase and homogenize at 6000r / min for 3min. The oil phase is caprylic / capric triglyceride.

[0064] Example 6: A method for preparing a Pickering emulsion of four o'clock flower endosperm powder, comprising the following steps: 73.2g of water and 0.8g of phenoxyethanol were stirred evenly, and 6.25g of four o'clock endosperm powder particles were added. The mixture was homogenized at 3000r / min for 10min to obtain a suspension. The four o'clock endosperm powder particles were prepared from Preparation Example 3. Add 5g xanthan gum to 95g water, stir to dissolve, and form a gel; Add 1g of gel to the suspension and homogenize at 5000r / min for 3min. Add 18.75g of oil phase and homogenize at 6000r / min for 3min. The oil phase is caprylic / capric triglyceride and isopropyl myristate in a mass ratio of 1:1.

[0065] Example 7: A method for preparing a Pickering emulsion of four o'clock flower endosperm powder, comprising the following steps: 8g of four o'clock endosperm powder particles were added to 44g of water, ultrasonically dispersed at 250W for 2min, and then homogenized at 3000r / min for 2min to obtain a suspension. The four o'clock endosperm powder particles were prepared by Preparation Example I and had a particle size of 1.2μm. Add 48g of oil phase to the suspension and homogenize at 6000r / min for 3min to form a Pickering emulsion. The oil phase is isododecane.

[0066] Comparative Example Comparative Example 1: A method for preparing a Pickering emulsion, comprising the following steps: Add 8g of corn starch to 44g of water, ultrasonically disperse for 2 minutes at 250W, then homogenize for 2 minutes at 3000r / min to form a suspension. The particle size distribution of the corn starch is as follows: Figure 3 As shown; Add 48g of oil phase to the suspension and homogenize at 6000r / min for 3min. The oil phase is jojoba seed oil.

[0067] See Figure 5 Compared with the control group, the emulsion prepared in Comparative Example 1 is prone to oil-water separation and cannot form a uniform emulsion.

[0068] Performance testing of Pickering emulsion The Pickering emulsions prepared in Examples 1-6 and Comparative Example 1 were subjected to emulsification index testing. The emulsification index was recorded after storage at 40°C for 30, 45, and 60 days. The emulsification index testing method is as follows: the emulsion was centrifuged in a centrifuge tube at 5000 rpm for 5 min, and the emulsification index was calculated according to the following formula: E = Hs / Ht, where Hs is the height of the emulsion phase (mm) and Ht is the total height of the emulsion (mm). The test results are shown in Table 1.

[0069] Table 1. Stability testing of Pickering emulsions As can be seen from the data comparison in Table 1, the Pickering emulsion prepared using Mirabilis endosperm powder particles in Example 1 still has a high emulsification index after being stored at 40°C for 60 days, indicating that the emulsion has high stability and little oil-water separation.

[0070] Example 2 uses four o'clock endosperm powder particles, while Examples 7 and 8 use hydrophobically modified four o'clock endosperm powder particles. At the same time, polar oil and non-polar oil are emulsified. It can be seen that the emulsification effect is good, the emulsification index is high, and the emulsion is stable.

[0071] The Pickering emulsion prepared in Example 3 contained xanthan gum and preservatives, and it is evident that the prepared Pickering emulsion still exhibits good stability. The Pickering emulsion prepared in Example 4 did not contain xanthan gum. Figure 9 It is evident that not only is the emulsion yellowish in color, but its stability is also inferior to that of Example 3.

[0072] In Example 5, caprylic / capric triglyceride was used as an oil, and in Example 6, caprylic / capric triglyceride and isopropyl myristate were used as oils. It can be seen that Mirabilis endosperm powder particles can emulsify polar and non-polar oils, are applicable to different polar oils, and are compatible with thickeners, preservatives, etc., without affecting the rheology and stability of the emulsion.

[0073] In Example 7, isododecane was used as an oil, and it can be seen that the prepared Pickering emulsion has good heat resistance stability.

[0074] Comparative Example 1 uses corn starch to prepare Pickering emulsion. Compared with Example 1, it has a lower emulsification index and is more prone to oil-water separation.

[0075] Application examples Application Example I-1: A Pickering emulsion of four o'clock flower endosperm powder loaded with the fat-soluble component vitamin E, prepared by the following method: 7g of four o'clock endosperm powder particles were added to 43g of water and ultrasonically dispersed at 250W for 2min, and then homogenized at 3000r / min for 2min to obtain a suspension. The four o'clock endosperm powder particles were prepared by Preparation Example I and had a particle size of 1.2μm. Disperse 1g of vitamin E into 49g of oil-phase isododecane, stir well, and then add it to the suspension. Homogenize at 6000r / min for 3min.

[0076] The product appearance of Pickering emulsion, loaded with vitamin E from four o'clock flower endosperm powder, is as follows: Figure 11 As shown, the microscope image is as follows. Figure 12 As shown.

[0077] Application Example I-2: A Pickering emulsion of four o'clock flower endosperm powder loaded with the fat-soluble component vitamin E, prepared by the following method: 7g of four o'clock endosperm powder particles were added to 43g of water and ultrasonically dispersed at 250W for 2min, and then homogenized at 3000r / min for 2min to obtain a suspension. The four o'clock endosperm powder particles were prepared by Preparation Example I and had a particle size of 1.2μm. Disperse 1g of vitamin E into 49g of oil phase jojoba seed oil, stir well, and then add it to the suspension. Homogenize at 6000r / min for 3min.

[0078] Application Example I-3: A Pickering emulsion of four o'clock flower endosperm powder loaded with the fat-soluble component vitamin E, prepared by the following method: 7g of four o'clock endosperm powder particles were added to 43g of water and ultrasonically dispersed at 250W for 2min, and then homogenized at 3000r / min for 2min to obtain a suspension. The four o'clock endosperm powder particles were prepared by Preparation Example I and had a particle size of 1.2μm. 1g of vitamin E was dispersed into 49g of oil phase, stirred evenly, and then added to the suspension. The mixture was homogenized at 6000r / min for 3min. The oil phase consisted of jojoba seed oil and caprylic / capric triglycerides in a mass ratio of 1:1.

[0079] Application Example I-4: A Pickering emulsion of four o'clock flower endosperm powder loaded with the fat-soluble component vitamin E, prepared by the following method: 7g of four o'clock endosperm powder particles were added to 43g of water and ultrasonically dispersed at 250W for 2min, and then homogenized at 3000r / min for 2min to obtain a suspension. The four o'clock endosperm powder particles were prepared by Preparation Example I and had a particle size of 1.2μm. 1g of vitamin E was dispersed into 49g of oil phase, stirred evenly, and then added to the suspension. The mixture was homogenized at 6000r / min for 3min. The oil phase included caprylic / capric triglycerides in a mass ratio of 1:1.

[0080] Application Example I-5: A Pickering emulsion of four o'clock flower endosperm powder loaded with the fat-soluble component vitamin E, prepared by the following method: 7g of four o'clock endosperm powder particles were added to 43g of water and ultrasonically dispersed at 250W for 2min, and then homogenized at 3000r / min for 2min to obtain a suspension. The four o'clock endosperm powder particles were prepared by Preparation Example I and had a particle size of 1.2μm. 1g of vitamin E was dispersed into 49g of oil phase, stirred evenly, and then added to the suspension. The mixture was homogenized at 6000r / min for 3min. The oil phase consisted of caprylic / capric triglyceride and isopropyl myristate in a mass ratio of 1:1.

[0081] Application Example I-6: A Pickering emulsion loaded with the fat-soluble component vitamin E was prepared by the following method: 7g of corn starch was added to 43g of water, ultrasonically dispersed at 250W for 2min, and then homogenized at 3000r / min for 2min to obtain a suspension. The particle size distribution of the corn starch was as follows: Figure 3 As shown; Disperse 1g of vitamin E into 49g of oil-phase isododecane, stir well, and then add it to the suspension. Homogenize at 6000r / min for 3min.

[0082] After storing the vitamin E-loaded four o'clock flower endosperm powder Pickering emulsion at 25°C for 30 days, the vitamin E content was measured, and the vitamin E retention rate was calculated as (vitamin E content before storage test / vitamin E content after storage test) × 100. Ten groups were tested for each application example, and the average results were recorded in Table 2. The vitamin E content in the four o'clock flower endosperm powder Pickering emulsion was determined using high performance liquid chromatography (HPLC).

[0083] The method for detecting vitamin E was modified based on the method of Wang Ruiying et al. (Wang Ruiying, Tang Jing, Zhang Lijing, Wang Qiang. Determination of vitamin E content in various vegetable oils by high performance liquid chromatography [J]. Journal of Xinjiang University (Natural Science Edition), 2003). The chromatographic conditions were as follows: (1) Column: Nova-Park C18 column, inner diameter 4.6 mm, length 150 mm, particle size 4 μm; (2) Mobile phase: methanol: water = 98:2; (3) Flow rate: 0.8 mL / min; (4) Column temperature: room temperature; (5) Detection wavelength: 295 nm; (6) Injection volume: 3 μL.

[0084] Table 2. Pickering emulsion stability test of vitamin E-loaded Mirabilis endosperm powder. As can be seen from the data in Table 2, compared with using corn starch, encapsulating vitamin E with four o'clock flower endosperm powder granules can effectively improve the storage stability of vitamin E.

[0085] Application Example II-1: A Pickering emulsion of Mirabilis jalapa endosperm powder loaded with sunscreen was prepared by the following method: 2g of Mirabilis jalapa endosperm powder particles were added to 29.4g of water, ultrasonically dispersed at 250W for 2min, and then homogenized at 3000r / min for 2min to obtain a suspension. The Mirabilis jalapa endosperm powder particles were prepared in Preparation Example I and had a particle size of 1.2μm. 68.6g of organic sunscreen ( MC80) was added to the suspension and homogenized at 6000 r / min for 3 min to obtain a Pickering emulsion of Mirabilis jalapa endosperm powder loaded with sunscreen.

[0086] Application Example II-2: A Pickering emulsion of Mirabilis jalapa endosperm powder loaded with sunscreen was prepared by the following method: 2g of Mirabilis jalapa extract was added to 29.4g of water, ultrasonically dispersed at 250W for 2min, and then homogenized at 3000r / min for 2min to obtain a suspension. The Mirabilis jalapa endosperm powder particles were prepared by Preparation Example I and had a particle size of 1.2μm. 10g of octocrylene was added to 58.6g of oil-phase isododecane, stirred evenly, and then added to the suspension. The mixture was homogenized at 6000r / min for 3min to obtain a Pickering emulsion of Mirabilis endosperm powder loaded with sunscreen.

[0087] Application Example II-3: A Pickering emulsion of Mirabilis jalapa endosperm powder loaded with sunscreen was prepared by the following method: 2g of Mirabilis jalapa extract was added to 29.4g of water, ultrasonically dispersed at 250W for 2min, and then homogenized at 3000r / min for 2min to obtain a suspension. The Mirabilis jalapa endosperm powder particles were prepared by Preparation Example I and had a particle size of 1.2μm. 10g of octocrylene was added to 58.6g of oil phase, stirred evenly, and added to the suspension. The mixture was homogenized at 6000r / min for 3min to obtain a Pickering emulsion of Mirabilis jalapa endosperm powder loaded with sunscreen. The oil phase consisted of jojoba seed oil and caprylic / capric triglycerides in a mass ratio of 1:1.

[0088] Application Example II-4: A Pickering emulsion of Mirabilis jalapa endosperm powder loaded with sunscreen was prepared by the following method: 2g of Mirabilis jalapa extract was added to 29.4g of water, ultrasonically dispersed at 250W for 2min, and then homogenized at 3000r / min for 2min to obtain a suspension. The Mirabilis jalapa endosperm powder particles were prepared by Preparation Example I and had a particle size of 1.2μm. Add 10g of octocrylene to 58.6g of oil phase caprylic / capric triglyceride, stir well and add to the suspension. Homogenize at 6000r / min for 3min to obtain a Pickering emulsion of Mirabilis jalapa endosperm powder loaded with sunscreen.

[0089] Application Example II-5: A Pickering emulsion of Mirabilis jalapa endosperm powder loaded with sunscreen was prepared by the following method: 2g of Mirabilis jalapa extract was added to 29.4g of water, ultrasonically dispersed at 250W for 2min, and then homogenized at 3000r / min for 2min to obtain a suspension. The Mirabilis jalapa endosperm powder particles were prepared by Preparation Example I and had a particle size of 1.2μm. 10g of octocrylene was added to 58.6g of oil phase, stirred evenly, and added to the suspension. The mixture was homogenized at 6000r / min for 3min to obtain a Pickering emulsion of Mirabilis jalapa endosperm powder loaded with sunscreen. The oil phase included isopropyl myristate and caprylic / capric triglycerides in a mass ratio of 1:1.

[0090] Application Example II-6: A Pickering emulsion of Mirabilis jalapa endosperm powder loaded with sunscreen was prepared by the following method: 2g of corn starch was added to 29.4g of water, ultrasonically dispersed at 250W for 2min, and then homogenized at 3000r / min for 2min to obtain a suspension. The particle size distribution of the corn starch is as follows: Figure 3 As shown; 68.6g of organic sunscreen ( MC80) was added to the suspension and homogenized at 6000 r / min for 3 min to obtain a Pickering emulsion of Mirabilis jalapa endosperm powder loaded with sunscreen.

[0091] The Pickering emulsion containing sunscreen agents from Mirabilis jalapa endosperm powder prepared in Application Example II-1 was used to prepare a sunscreen product A, which is a Pickering emulsion type containing sunscreen agents, according to the dosage in Table 3 and the following method: Heat phase A to 80°C, homogenize for 3 minutes, and keep warm until ready for use; Heat phase B to 80°C and homogenize for 3 minutes; Phase C was added to Phase B, and the mixture was kept at 80°C and stirred until homogeneous to obtain mixture A. After stirring phase D evenly, add it to the mixture and homogenize at 80°C for 3 minutes to obtain mixture B; Phase A was added to mixture B, homogenized at high speed for 3 minutes, cooled to 45°C, and then phase E was added. The mixture was homogenized for 2 minutes, defoamed, and discharged to obtain sunscreen product A.

[0092] The Pickering emulsions containing sunscreen agents from Mirabilis jalapa endosperm powder prepared in Application Examples II2 to II-6 were used to prepare sunscreen products B, C, D, E, and F according to the dosages in Table 3 and the methods described above. The product made from the Pickering emulsion of Mirabilis jalapa endosperm powder without added sunscreen agents was designated as sunscreen product G. The appearance and microscopic images of sunscreen products A and G are shown below. Figure 13 As shown, the performance of sunscreen products was tested according to the following method. Five samples were tested for each sunscreen product, and the average value of the test results was taken. The test results are recorded in Table 4.

[0093] (1) Stability: The prepared sunscreen product AG was placed at room temperature for 1 hour and no separation was observed. It was then placed at 40°C for 30 days and observed. The stability of the sunscreen product was evaluated according to the following evaluation criteria: A is no separation confirmed; B is very slight separation; C is significant separation; D is separation occurring 1 hour after preparation. In this application, B grade and above are judged to be of excellent stability, that is, they meet the requirements.

[0094] (2) SPF value: After storing the sunscreen product at 40℃ for 30 days, it was tested according to ISO24443-2021. First, the blank film of the carrier was measured as the local curve. Then, a 1mL syringe was used to draw the sample and evenly applied it to Transpore MTE transparent tape. The sample was then quickly and evenly spread on the film with a finger wearing a latex finger cot, so that the sample on the film surface was at a concentration of 2mg / cm³. 2The sample was then distributed and placed in an environment of 25℃ and 60% humidity to air dry for 15 minutes. Nine points on the sample on the transparent tape were selected for testing using an SPF-290AS sun protection factor analyzer, and the average SPF value was calculated.

[0095] Table 3. Formulas of Pickering emulsion-type sunscreen products containing Mirabilis endosperm powder loaded with sunscreen agents. Table 4 Performance test results of sunscreen products (AE) As can be seen from the data in Table 4, the Pickering emulsion made from four o'clock flower endosperm powder can load sunscreen agents and, when combined with ingredients such as polydimethylsiloxane, produces sunscreen products with good stability and sun protection effect. However, the Pickering emulsion made from corn starch, when added to sunscreen products, does not improve the stability of sunscreen products as much as the Pickering emulsion made from four o'clock flower endosperm powder.

[0096] Application Example III-1: A lip gloss containing a four o'clock flower endosperm powder Pickering emulsion, wherein the four o'clock flower endosperm powder Pickering emulsion was prepared according to Example 1, the raw material amounts of the lip gloss are shown in Table 5, and the lip gloss is prepared by the following method: Stir phase A thoroughly; Phase B was heated to 105°C and stirred until homogeneous. Then it was cooled to 45°C and phase C was added. The mixture was homogenized at high speed for 5 minutes to obtain mixture A. Phase A is added to mixture A, homogenized at high speed for 5 minutes, then phase D is added, and the mixture is ground twice. The product is then discharged to obtain lip gloss A.

[0097] Table 5. Lip gloss formulations containing Pickering emulsion with four o'clock flower endosperm powder. The four o'clock flower endosperm powder Pickering emulsion prepared in Examples 2-7 was used to prepare lip glosses B to G according to the dosage and method of Application Example III-1. The Pickering emulsion prepared in Comparative Example 1 was used to prepare lip gloss H according to the dosage and method of Application Example III-1.

[0098] The performance of the lip gloss AH was tested using the following method, and the test results are recorded in Table 6.

[0099] 1. Stability: The lip gloss samples were placed at 55℃ and -4℃ for one month under heat and cold resistance conditions, and the stability of the sunscreen product was evaluated according to the following evaluation criteria: A is no separation confirmed; B is very slight separation; C is significant separation; D is separation occurring 1 hour after preparation. In this application, grade B and above are considered to have excellent stability, that is, to meet the requirements.

[0100] 2. Lip Moisture Content: Fifty volunteers with dry, flaky, and fine-lined lips were selected and divided into 5 groups of 10 each. A skin moisture meter was used before the test. 825) The moisture content of volunteers' lips was measured. One hour after applying lip gloss to the lips, the moisture content of volunteers' lips was measured again, and the average value of each group's test results was taken.

[0101] Table 6. Performance test results of Pickering emulsion containing four o'clock flower endosperm powder for lip glosses. The data in Table 6 show that the lip gloss made from the Pickering emulsion of four o'clock flower endosperm powder in Example 1 has good storage stability and can effectively improve the moisture content of the lips, resulting in a better performance. However, the lip gloss made from the Pickering emulsion prepared with corn starch has reduced stability and its performance is not as good as that of this application.

[0102] This specific embodiment is merely an explanation of this application and is not intended to limit it. After reading this specification, those skilled in the art can make modifications to this embodiment without contributing any inventive step, but such modifications are protected by patent law as long as they fall within the scope of the claims of this application.

Claims

1. A Violette endosperm flour Pickering emulsion characterized in that, The raw materials include 1-10% of Plukenetia volubilis endosperm powder particles, 10-70% of oil, and water to make up 100%.

2. The V. majestica endosperm flour Pickering emulsion according to claim 1, characterized in that: The particle size D50 of the Plukenetia volubilis endosperm powder Pickering emulsion is less than 20 microns.

3. The V. majestica endosperm flour Pickering emulsion of claim 1, wherein: The oil is selected from at least one of isododecane, isohexadecane, squalane, isopropyl myristate, phosphatidylcholine, phosphatidylethanolamine, caprylic / capric triglyceride, isononyl isononanoate, dicaprylyl carbonate, diethylhexyl carbonate, pentaerythrityl tetraisostearate, propylene glycol dicaprylate / dicaprate, green tea seed oil, jojoba seed oil, macadamia integrifolia seed oil, argan oil, shea butter, cyclomethicone, dimethicone, polyphenylsiloxane, octyl methoxycinnamate, and alkyl-modified silicone oil.

4. The V. majestica endosperm flour Pickering emulsion according to claim 1, characterized in that: The raw materials of the Plukenetia volubilis endosperm powder Pickering emulsion further include 1-3% of a thickening agent.

5. The V. majestica endosperm flour Pickering emulsion according to claim 4, characterized in that: The thickening agent is selected from at least one of hydroxycellulose, xanthan gum, gellan gum, hyaluronic acid, magnesium aluminum silicate, acrylate, carbomer, potassium chloride, succinoglycan, and polyacrylamide.

6. The V. majestica endosperm flour Pickering emulsion according to claim 1, characterized in that: The raw materials of the Plukenetia volubilis endosperm powder Pickering emulsion further include a preservative.

7. The V. majestica endosperm flour Pickering emulsion according to claim 6, characterized in that: The preservative is selected from at least one of phenoxyethanol, hexylene glycol, p-hydroxyacetophenone, ethylhexylglycerin, caprylyl oxyhydroxamic acid, caprylyl glycol, and sodium benzoate.

8. A process for the preparation of a Pichia pastoris endosperm powder Pickering emulsion according to any one of claims 1 to 7, characterized in that: The method includes the following steps: Dispersing Plukenetia volubilis endosperm particles into water, ultrasonic treatment, and homogenization to form a suspension; Adding an oil phase to the suspension and homogenizing to obtain a Pickering emulsion.

9. Use of a P. grandiflora endosperm flour Pickering emulsion according to any one of claims 1 to 7 or a P. grandiflora endosperm flour Pickering emulsion prepared according to the method of claim 8, characterized in that, The Plukenetia volubilis endosperm powder Pickering emulsion is used to load liposoluble ingredients or sunscreen agents.

10. Use of a V. magus endosperm flour Pickering emulsion according to claim 9 in a cosmetic product, characterized in that, The proportion of the liposoluble ingredients in the Plukenetia volubilis endosperm powder Pickering emulsion loaded with the liposoluble ingredients is 1% of the total weight of the emulsion, and the proportion of the sunscreen agent in the Plukenetia volubilis endosperm powder Pickering emulsion loaded with the sunscreen agent is 10-68.6% of the total weight of the emulsion.

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