Preparation method and application of moringa seed oil liposome composition

Abstract

The invention discloses a preparation method of a moringa seed oil liposome composition, which comprises the following steps: weighing cholesterol, lecithin, moringa seed oil and TW-80, adding absolute ethyl alcohol, carrying out ultrasonic dissolution, carrying out rotary evaporation to remove an organic solvent to form a lipid film, then adding water for activation, carrying out ultrasonic treatment until the formed solution is uniform in texture, and drying to obtain the moringa seed oil liposome composition. The liposome compound containing the moringa seed oil is obtained. The invention further discloses application of the moringa seed oil liposome composition in cosmetics. According to the invention, a lipidosome wrapping process is combined, the moringa seed oil raw material is optimized and innovated, the problems of insufficient deep processing technology and the like in extraction and application of active substances of the moringa seed oil raw material are solved, and the moringa seed oil lipidosome with tightening and anti-wrinkle effects is obtained. The application of vegetable oil components in the formulas of toning lotion, water essence and the like is improved, the sticky and greasy skin feeling of the vegetable oil is improved, the effects of the raw materials are reflected to the maximum extent, and the development of the moringa oleifera industry is driven while the market requirements are met.

Description

Technical Field

[0001] The invention relates to a composition, and in particular to a preparation method and application of a moringa seed oil liposome composition with firming and anti-wrinkle effects. Background Art

[0002] Moringa has many uses in production and life, and is widely planted around the world. my country has introduced it since the early 1960s and promoted its planting in South China and Southwest China. The diameter of Moringa seeds is about 8mm. They are white after shelling and can be eaten directly or after simple processing. Moringa seeds are rich in nutrients such as oil, protein, and vitamins. Modern pharmacology reports point out that Moringa seeds have good anti-inflammatory, anti-tumor, antibacterial and hypoglycemic effects. Domestic and foreign research on Moringa seeds mainly focuses on the extraction of oil from seed kernels and their related basic properties, and is mainly used in food, medicine, health care products and chemical industries. At present, the commercial deep processing research and related industries of Moringa seeds are immature and still in the primary stage, far from meeting the needs of the continuously expanding Moringa industry. It is urgent to support and promote the deep processing technology of Moringa-related raw materials to empower the Moringa raw material industry, improve its product added value, and increase industry competitiveness. Summary of the invention

[0003] The technical problem to be solved by the present invention is to provide a moringa seed oil liposome composition and a preparation method thereof.

[0004] A method for preparing a moringa seed oil liposome composition comprises the following steps: weighing cholesterol, lecithin, moringa seed oil and TW-80, adding anhydrous ethanol, ultrasonically dissolving, removing the organic solvent by rotary evaporation to form a lipid film, adding water for activation, and ultrasonicating until a solution with a uniform texture is formed to obtain a liposome complex containing moringa seed oil.

[0005] The preparation method of the present invention specifically comprises the following steps: weighing cholesterol, lecithin, moringa seed oil and TW-80 in a round-bottom flask in a mass ratio of 1:4:1:1, adding 30-40 mL of anhydrous ethanol, and dissolving by ultrasonication for 10-20 min; the temperature is 45-50° C., the vacuum degree is 0.6-0.8 Bar, and the organic solvent is removed by rotary evaporation to form a lipid film, and then 40-50 mL of water is added to maintain a constant temperature of 45-50° C. and a vacuum degree of 0.6-0.8 Bar for activation for 10-20 min; and ultrasonication is performed until a solution with a uniform texture is formed to obtain a liposome complex containing moringa seed oil.

[0006] The preparation method of the present invention, wherein the Moringa seed oil is prepared by a supercritical extraction method, comprises the following steps:

[0007] Crush the Moringa seeds and load them into the extraction kettle, turn on the carbon dioxide switch, adjust the pressure and temperature of the extraction kettle and the first separation kettle and the second separation kettle, adjust the valve to make it stable, the carbon dioxide fluid is fully in contact with the Moringa seed material in the extraction kettle, and the carbon dioxide fluid carrying Moringa seed oil enters the first separation kettle through a pipeline to perform the first separation of the Moringa seed oil, and then a small amount of unseparated Moringa seed oil is allowed to enter the second separation kettle with the carbon dioxide fluid for secondary separation. The separated carbon dioxide is circulated through a loop, and when the preset pressure and temperature of the extraction kettle, the first separation kettle and the second separation kettle are stabilized, the Moringa seed oil is collected from the first separation kettle and the second separation kettle in batches.

[0008] The preparation method of the present invention, wherein the pressure and temperature of the extraction kettle, the first separation kettle and the second separation kettle are adjusted, and when the extraction pressure reaches 35MPa and the extraction temperature reaches 40°C, the pressure of the first separation kettle reaches 12MPa and the separation temperature reaches 45°C, and the pressure of the second separation kettle reaches 5MPa and the separation temperature reaches 35°C, the valve is adjusted to stabilize;

[0009] After the preset pressure and temperature of the extraction kettle, the first separation kettle and the second separation kettle are stabilized for 10-20 minutes, Moringa seed oil is collected from the first separation kettle and the second separation kettle every 30 minutes, and the overall extraction time is 3 hours.

[0010] The moringa seed oil liposome composition is prepared by the method of the invention.

[0011] Application of the Moringa seed oil liposome composition of the present invention in cosmetics.

[0012] In the application of the present invention, the cosmetic is moisturizing lotion, essence liquid or essence water.

[0013] A Moringa moisturizing water, composed of the following raw materials in percentage by mass:

[0014] Moringa seed oil liposome: 1-3%, 1,3-butylene glycol: 2-5%, glycerol: 5-6%, carbomer: 0.1-0.15%, D-panthenol: 0.5-1%, triethanolamine: 0.1-0.3%, PE9010: 0.8%, the balance is water;

[0015] The preparation method of the Moringa moisturizing water comprises the following steps: pre-dispersing the carbomer in phase A into water for swelling; after complete swelling, adding the remaining raw materials of phase A, heating to 60-70° C., and cooling at room temperature; adding phase B at below 40° C., adjusting the pH to 5.0-6.5, and stirring and mixing evenly; and sequentially adding phase C, stirring and mixing at a low speed evenly.

[0016] A Moringa essence, consisting of the following raw materials in percentage by mass:

[0017] Moringa seed oil liposome: 1-3%, xanthan gum: 0.2-0.3%, glycerol: 2-5%, sodium hyaluronate: 0.1-0.2%, dipropylene glycol: 2-5%, p-hydroxyacetophenone: 0.3-0.5%, 1,2-hexanediol: 0.3-0.5%, tetrahydromethylpyrimidine carboxylic acid: 0.1-0.2%, the balance is water;

[0018] The preparation method of the moringa essence comprises the following steps: pre-dispersing the xanthan gum in phase A into water for swelling; after complete swelling, adding the remaining raw materials of phase A, heating to 60-70° C. for dissolution, and cooling at room temperature; pre-heating phase B to 60-75° C. for dissolution for standby use, adding phase B at below 40° C., and stirring at low speed for uniform mixing; adding raw materials of phase C in sequence, and stirring at low speed for uniform mixing.

[0019] A Moringa essence water, composed of the following raw materials in percentage by mass:

[0020] Moringa seed oil liposome: 1-3%, dipropylene glycol: 2-5%, EDTA-2Na: 0.01%, betaine: 0.5-1%, ammonium acryloyldimethyltaurate / VP copolymer: 0.15-0.2%, xanthan gum: 0.1-0.2%, p-hydroxyacetophenone: 0.3-0.5%, 1,2-hexanediol: 0.3-0.5%, the balance is water;

[0021] The preparation method of the Moringa essence water comprises the following steps: pre-dispersing xanthan gum and ammonium acryloyldimethyltaurate / VP copolymer in phase A into water for swelling; after complete swelling, adding the remaining raw materials of phase A, heating to 60-70° C. for complete dissolution, and cooling at room temperature; adding phase B at below 40° C., and stirring at a low speed for uniform mixing.

[0022] Beneficial effects of the Moringa seed oil liposome composition and preparation method thereof:

[0023] 1. The traditional extraction of vegetable oil is processed by physical pressing, but the oil yield is low. The solvent extraction method has a relatively high yield of oil, but it still faces the risk of organic solvent residues, which is not conducive to its application in cosmetics. The Moringa seed oil used in Moringa seed liposomes is obtained by supercritical CO2 extraction. This technology has the characteristics of low extraction temperature, non-toxicity, no solvent residue, environmental protection, short extraction time, etc., and has the advantages of high activity and high quality.

[0024] Second, although Moringa seed oil is mentioned in the prior art, Moringa seed oil liposomes and the application in the field of cosmetics are not related to, vegetable oil is applied in cosmetics, although the compatibility with skin is better, it is difficult to dissolve, easily oxidized and rancid, produces unpleasant odor, increases the problems of skin irritation, and reduces the biological activity of its skin external use. And the vegetable oil component skin feel is also heavier, mainly concentrated in cream, essence oil, makeup remover, lacks the refreshing feeling of water product, and the incompatible characteristic of water and oil makes the vegetable oil component difficult to add toner, water essence. The present invention adopts liposome encapsulation technology, Moringa seed oil is encapsulated in liposome, improves its solubility, and alleviates greasy feeling.

[0025] 3. On this basis, the present invention has developed three mature formulas of dosage forms. In the formula development, the application of high-quality plant oil ingredients in aqueous formulas is improved, the stability of plant oils is increased, and the sticky skin feel of plant oils is improved, which improves its precision and sense of technology in skin care and solves the production and application problems of Moringa seed oil.

[0026] Fourth, the present invention extracts moringa seed oil through supercritical CO2 to obtain high-quality moringa seed oil without solvent residue, and uses liposome encapsulation technology to load the obtained moringa seed oil with a ratio of cholesterol: lecithin: moringa seed oil: TW-80 of 1:4:1:1, and verifies the firming and anti-wrinkle effect of moringa seed oil liposomes. Moringa seed oil liposomes are applied to cosmetic formulas in a certain proportion, and their efficacy and skin feel evaluation are verified to obtain a product that has firming, anti-wrinkle, soothing and repairing while having a refreshing and non-greasy skin feel. Improve the heavy skin feel of the plant oil moringa seed oil, increase its solubility, and expand its application in cosmetic formulas such as lotions and water essences, practice high-quality development of the cosmetics industry, combine market demand, deeply integrate production, education, research and use, empower moringa products, and help the high-quality development of the moringa industry. Combine scientific and technological technologies and market advantages with the agricultural industry to achieve sustainable agricultural development and promote farmers' income growth.

[0027] Five, the present invention uses supercritical CO2 fluid extraction technology to extract high-quality moringa seed oil, and uses biochemistry, cell level, human efficacy test and other multi-dimensional evaluations to successfully transform food-grade moringa seed raw materials into cosmetic-grade raw materials, providing a valuable reference method in process optimization. The current plant oil components are mainly directly used in cosmetic formulas, but it is inevitable that there will be common problems such as oxidation and taste change in the use of plant oils. The present invention combines liposome encapsulation technology to optimize and innovate the moringa seed oil raw materials, improve the extraction and application of active substances in moringa raw materials, and there are problems such as insufficient deep processing technology. The obtained moringa seed oil liposome with firming and anti-wrinkle effect improves the application of plant oil components in formulas such as lotions and water essences, improves the sticky skin feel of plant oils, and reflects the efficacy of raw materials to the greatest extent. While meeting market demand, it also drives the development of the moringa industry.

[0028] The Moringa seed oil liposome composition and the preparation method thereof of the present invention will be further described below in conjunction with the accompanying drawings. BRIEF DESCRIPTION OF THE DRAWINGS

[0029] Figure 1 The present invention is a flow chart of the method for preparing the Moringa seed oil liposome composition;

[0030] Figure 2 This is a graph showing the DPPH clearance rate of Moringa seed liposomes in the method of the present invention. DETAILED DESCRIPTION

[0031] 1. Supercritical extraction of Moringa seed oil

[0032] The Moringa seeds are crushed and loaded into the extraction kettle of HA221-50-10-C supercritical carbon dioxide extraction device (Nantong Hua'an Supercritical Extraction Co., Ltd.), the carbon dioxide switch is turned on, the pressure and temperature of the extraction kettle, the first separation kettle and the second separation kettle are adjusted, when the extraction pressure is 35MPa and the extraction temperature is 40°C, the separation pressure of the separation kettle can be 12MPa and the separation temperature is 45°C, and the pressure of the second separation kettle is 5MPa and the separation temperature is 35°C, and the valve is adjusted to stabilize it. The carbon dioxide fluid is fully contacted with the Moringa seeds material in the extraction kettle, and the carbon dioxide fluid carrying Moringa seed oil is entered into the first separation kettle through a pipeline to separate Moringa seed oil for the first time, and then a small amount of unseparated Moringa seed oil is entered into the secondary separation with the carbon dioxide fluid, and the separated carbon dioxide is circulated by a loop. After the preset pressure and temperature of the extraction kettle, the first separation kettle and the second separation kettle are stabilized for 10-20min, Moringa seed oil is collected from the first separation kettle and the second separation kettle every 30min. The overall extraction time is 3 hours. After the extraction is completed, the moringa seed oil is combined and the supercritical carbon dioxide moringa seed oil extraction rate is calculated to be 30%-31.07%. The obtained moringa seed oil has high purity and no risk of solvent residue.

[0033] 2. Moringa Seed Oil Liposomes

[0034] (1) Preparation of Moringa seed oil liposomes

[0035] Weigh 2.5 mg cholesterol, 10 mg lecithin, 2.5 mg moringa seed oil and 2.5 mg TW-80 into a round-bottom flask, add 30-40 mL anhydrous ethanol, and sonicate for 10-20 min to dissolve; the temperature is 45-50 ° C, the vacuum degree is 0.6-0.8 Bar, and the organic solvent is removed by rotary evaporation to form a lipid film, and then 40-50 mL of water is added to maintain a constant temperature of 45-50 ° C and a vacuum degree of 0.6-0.8 Bar to activate for 10-20 min; sonicate until a solution with a uniform texture is formed to obtain a liposome complex containing moringa seed oil.

[0036] (2) Packet rate

[0037] Take 1mL of Moringa seed oil liposomes in a 10mL centrifuge tube, add 4mL of petroleum ether, vortex mix and centrifuge (6000r / min, 10min), collect the supernatant, repeat the operation twice and combine the organic phases, dilute to 25mL with anhydrous ethanol, measure the absorbance at 290nm, and calculate the free essential oil content A1 according to the above standard curve. Take another 1mL of liposomes, dilute to 25mL with anhydrous ethanol, sonicate in a water bath for 1h, measure the absorbance value and calculate the total cinnamon essential oil content A2 according to the formula The encapsulation efficiency was found to be 56.99%.

[0038] (3) DPPH clearance test

[0039] DPPH is a stable free radical, and its alcohol solution is dark purple. When a free radical scavenger is present, the light absorption of the DPPH ethanol solution weakens. The degree of fading can be used to evaluate the free radical scavenging ability of the sample and the effect of the sample on promoting skin firming and anti-wrinkle.

[0040] Prepare 80μg / mL DPPH-anhydrous ethanol solution, prepare 4 groups of test tubes numbered A, B, C, and D, mix 0.5mL of the test solution with 0.5mL of DPPH ethanol solution (tube A), mix 0.5mL of the solvent with 0.5mL of DPPH ethanol solution (tube B), mix 0.5mL of the test solution with 0.5mL of anhydrous ethanol (tube C), and mix 0.5mL of the solvent with 0.5mL of anhydrous ethanol as a blank control (tube D). After reacting at room temperature in the dark for 20 minutes, measure the absorbance of A, B, C, and D at 517nm. According to the formula The scavenging effect of Moringa seed oil liposomes on DPPH free radicals was calculated. Moringa seed liposomes at a concentration of 50% had a scavenging effect on DPPH free radicals. According to the correlation between DPPH free radicals and skin firming and anti-wrinkle, Moringa seed oil liposomes have a certain firming and anti-wrinkle effect. Figure 2 shown.

[0041] Table 1 DPPH free radical scavenging rate of Moringa liposomes

[0042] Moringa seed oil liposome concentration 50.00％ 25.00％ 12.50％ 6.25％ DPPH clearance 48.22％ 9.54％ 7.17％ 4.66％

[0043] 3. Formula Preparation

[0044] 1. Moringa moisturizing water

[0045] The raw materials are calculated based on 100% total mass, including moringa seed oil liposome: 1-3%, 1,3-butylene glycol: 2-5%, glycerol: 5-6%, carbomer: 0.1-0.15%, D-panthenol: 0.5-1%, triethanolamine: 0.1-0.3%, PE9010: 0.8%, and the balance is water.

[0046] The preparation method of the soft essence water comprises the following steps: pre-dispersing the carbomer in phase A into water to swell; after the swelling is complete, adding the remaining raw materials of phase A, heating to 60-70 degrees Celsius, and cooling at room temperature; adding phase B below 40 degrees Celsius, adjusting the pH to 5.0-6.5, and stirring and mixing at a low speed to be uniform; adding phase C in sequence, and stirring and mixing at a low speed to be uniform.

[0047] Table 2 Moringa moisturizing water formula

[0048]

[0049] (1) In vitro evaluation of firming and anti-wrinkle efficacy:

[0050] Evaluation method: DPPH clearance rate is used as an indicator to evaluate the firming and anti-wrinkle effect. If the clearance rate of the sample is higher than that of the negative control and there is a significant difference, it can be considered that the sample has a certain anti-wrinkle effect.

[0051] Table 3 DPPH free radical scavenging rate

[0052]

[0053] Under laboratory conditions, the average DPPH free radical scavenging rate of Moringa moisturizing water was 24.56%±1.08%, which was significantly different from that of the negative control (p<0.05). The DPPH free radical scavenging rate of the positive control was >25%, and the reaction system was effective, verifying that Moringa moisturizing water has firming and anti-wrinkle effects.

[0054] Evaluation method: The collagenase inhibition rate is used as an indicator to evaluate the anti-wrinkle effect. The higher the collagenase inhibition rate, the stronger the anti-wrinkle and firming effect on the skin. By comparing with the negative control, it is determined whether it has the effect of inhibiting the production of collagenase.

[0055] Table 4 Collagenase inhibition rate

[0056]

[0057] Under the conditions of this experiment, the inhibition rate of Moringa moisturizing water on collagenase was 10.08%. By comparing with the blank control, it was shown that Moringa moisturizing water has the effect of inhibiting the production of collagenase.

[0058] (2) Human skin patch test

[0059] Patch test method: Select qualified patch test equipment and use the closed patch test method. Place approximately 0.020g~0.025g (solid) or 0.020mL~0.025mL (liquid) of the test substance in the patch test device and apply it to the subject's forearm with low-allergenic tape. Remove the test substance after 24 hours and observe the skin reaction at 0.5, 24, and 48 hours after removal. Record the results according to the skin reaction grading standards in the current valid technical specifications.

[0060] Table 5 Human skin patch test results

[0061]

[0062] Test results: The results of the human skin patch test showed that 29 subjects had no adverse skin reactions in the test area 0.5h, 24h, and 48h after removing the test patch tester, indicating that Moringa moisturizing water is non-irritating to the human body surface.

[0063] (3) Use sensory evaluation

[0064] Evaluation method and indicators: 10 testers who have certain skin care habits, often use moisturizing products, have no physical discomfort that affects sensory evaluation when participating in the test, have a certain level of education, and can clearly understand the description of the questionnaire were selected. Select a 4cm2 area on the volunteer's arm, apply 2g of sample evenly on the arm, and the volunteer uses the other hand to make circles until the sample is completely absorbed. The sensory score is scored during the application process. The scoring standards are excellent (90 points), good (80 points), and qualified (60 points), and the volunteer scores are statistically analyzed using the questionnaire survey method.

[0065] Table 6 Sensory evaluation standards

[0066]

[0067] Table 7 Sensory evaluation results

[0068]

[0069] Sensory evaluation results: The spreadability, moisturizing, permeability, uniformity, fineness and direct usability of Moringa Moisturizing Water are all excellent, and the skin feels refreshing and easy to absorb.

[0070] (4) Human efficacy evaluation test

[0071] Test method: By comparing the changes in transepidermal water loss (TEWL) values, skin elasticity and other skin test indicators of 30 subjects before use, 14 days after use and 28 days after use, this paper verifies whether Moringa Moisturizing Water can help replenish or enhance the content of moisture, oil and other components in the application area, or maintain the moisture content in the application area or reduce water loss, whether it can help maintain the application area in a normal state, and whether it can help improve skin irritation, etc., in order to evaluate the moisturizing and repairing effects of Moringa Moisturizing Water.

[0072] Table 8 Statistical table of test results of moisture content of stratum corneum (n=30)

[0073]

[0074] *p<0.05 / **p<0.01 indicates that the index value is improved after using the sample, and the difference is statistically significant.

[0075] Test results of stratum corneum moisture content: Compared with before using Moringa moisturizing water (D0), the stratum corneum moisture content increased after using Moringa moisturizing water for 14 days (D14) and after using the sample for 28 days (D28), and the difference in stratum corneum moisture content compared with D0 was statistically significant (p < 0.05), with the increase rates being 6.74% and 11.83%, respectively.

[0076] Table 9 TEWL value test results statistics (n = 30)

[0077]

[0078] *p<0.05 / **p<0.01 indicates that the index value is improved after using the sample, and the difference is statistically significant.

[0079] Transepidermal water loss TEWL value test results: Compared with before using Moringa moisturizing water (D0), the TEWL values ​​of transepidermal water loss decreased after using Moringa moisturizing water for 14 days (D14) and after using the sample for 28 days (D28), and the difference with the TEWL values ​​of D0 was statistically significant (p < 0.05), and the decrease rates were 13.73% and 27.40%, respectively.

[0080] (5) Consumer use test

[0081] Test method: The subjects should visit the laboratory 14 days (D14) and 28 days (D28) after using Moringa Moisturizing Water, clean the test area with cleaning products, dry it and sit quietly in a constant temperature and humidity room. During the meditation period, fill in the questionnaire based on the subjective feelings after using the sample.

[0082] Table 10 Statistical table of sensory evaluation results of the questionnaire survey of subjects (n=30)

[0083]

[0084] Scoring criteria: 5-strongly agree; 4-agree; 3-neutral; 2-disagree; 1-strongly disagree. Scores > 3 are considered positive options.

[0085] Results of sensory evaluation tests by consumers: After using Moringa Moisturizing Water, 93.33% of the subjects believed that [the product has a pleasant smell]; 96.67% of the subjects believed that [the product is absorbed quickly when used]; 96.67% of the subjects believed that [the product feels good on the skin]; 93.33% of the subjects believed that [the product is gentle and non-irritating when used]; 96.67% of the subjects believed that [the skin is not sticky after using the product].

[0086] Table 11 Statistics of the results of the efficacy evaluation part of the questionnaire survey of subjects (n=30)

[0087]

[0088] Rating criteria: 5-strongly agree / satisfied; 4-agree / satisfied; 3-average; 2-disagree / dissatisfied; 1-strongly disagree / strongly dissatisfied. Ratings > 3 are considered positive options.

[0089] Results of the efficacy evaluation test by consumers: After using Moringa Moisturizing Water for 14 days (D14) and 28 days (D28), the results of the efficacy evaluation part of the questionnaire survey showed that 63.33% and 80.00% of the subjects believed that [skin sensitivity and redness were improved]; 70.00% and 86.67% of the subjects believed that [skin barrier ability was improved]; 76.67% and 86.67% of the subjects believed that [skin elasticity was improved]; 73.3 3% and 86.67% of the subjects believed that [skin fine lines and dry lines were improved]; 73.33% and 86.67% of the subjects believed that [dull skin tone was improved]; 80.00% and 86.67% of the subjects believed that [skin hydration was improved]; 83.33% and 93.33% of the subjects believed that [skin felt lastingly moisturized]; 100.00% and 100.00% of the subjects believed that [overall, they were satisfied with the product].

[0090] 2. Moringa Essence

[0091] The raw materials are calculated based on 100% total mass, including moringa seed oil liposome: 1-3%, xanthan gum: 0.2-0.3%, glycerol: 2-5%, sodium hyaluronate: 0.1-0.2%, dipropylene glycol: 2-5%, p-hydroxyacetophenone: 0.3-0.5%, 1,2-hexanediol: 0.3-0.5%, tetrahydromethylpyrimidine carboxylic acid: 0.1-0.2%, and the balance is water.

[0092] The preparation method of the moringa essence comprises the following steps: pre-dispersing the xanthan gum in phase A into water for swelling; after complete swelling, adding the remaining raw materials of phase A, heating to 60-70° C. for dissolution, and cooling at room temperature; pre-heating phase B to 60-75° C. for dissolution for standby use, adding phase B at below 40° C., and stirring at low speed for uniform mixing; adding raw materials of phase C in sequence, and stirring at low speed for uniform mixing.

[0093] Table 12 Moringa essence formula

[0094]

[0095] (1) In vitro evaluation of firming and anti-wrinkle efficacy

[0096] Table 13 DPPH free radical scavenging rate

[0097]

[0098] Under laboratory conditions, the average DPPH free radical scavenging rate of Moringa essence was 28.75%±1.23%, which was significantly different from that of the negative control (p<0.05). The DPPH free radical scavenging rate of the positive control was >25%, indicating that the reaction system was effective, verifying that Moringa essence has firming and anti-wrinkle effects.

[0099] Table 14 Collagenase inhibition rate

[0100]

[0101] Results of the in vitro firming and anti-wrinkle efficacy evaluation test: Under the conditions of this test, the inhibition rate of Moringa essence on collagenase was 11.20%. By comparing with the blank control, it was shown that Moringa essence has the effect of inhibiting the production of collagenase.

[0102] (2) Human skin patch test

[0103] Table 15 Human skin patch test results

[0104]

[0105] Test results: The results of the human skin patch test showed that 30 subjects had no adverse skin reactions in the test area 0.5h, 24h, and 48h after removing the test patch tester, indicating that Moringa essence is non-irritating to the human body surface.

[0106] (3) Use sensory evaluation

[0107] Table 16 Sensory evaluation results

[0108]

[0109] Sensory evaluation results: The spreadability, moisturizing, permeability, uniformity, fineness and direct usability of the Moringa essence were all excellent, and the skin feels refreshing and non-sticky.

[0110] (4) Human efficacy evaluation test (5)

[0112] Table 17 Statistical table of test results of moisture content of stratum corneum (n=30)

[0113]

[0114] *p<0.05 / **p<0.01 indicates that the index value is improved after using the sample, and the difference is statistically significant.

[0115] Test results of stratum corneum moisture content: Compared with before using Moringa essence (D0), the stratum corneum moisture content increased after using Moringa essence for 14 days (D14) and 28 days (D28), and the difference in stratum corneum moisture content compared with D0 was statistically significant (p < 0.05), with the increase rates being 17.08% and 30.20%, respectively.

[0116] Table 18 TEWL value test results statistics (n = 30)

[0117]

[0118] *p<0.05 / **p<0.01 indicates that the index value is improved after using the sample, and the difference is statistically significant.

[0119] Transepidermal water loss TEWL value test results: Compared with before using Moringa essence (D0), the TEWL values ​​of transepidermal water loss decreased after using Moringa essence for 14 days (D14) and 28 days (D28) of using the sample, and the difference with the TEWL values ​​of D0 was statistically significant (p < 0.05), and the decrease rates were 5.88% and 15.73%, respectively.

[0120] (5) Consumer use test

[0121] The subjects should visit the laboratory 14 days (D14) and 28 days (D28) after using the Moringa essence, clean the test area with cleaning products, dry it and sit quietly in a constant temperature and humidity room. During the meditation period, fill in the questionnaire based on the subjective feelings after using the sample.

[0122] Table 19 Statistical table of sensory evaluation results of the questionnaire survey of subjects (n=30)

[0123]

[0124] Scoring criteria: 5-strongly agree; 4-agree; 3-neutral; 2-disagree; 1-strongly disagree. Scores > 3 are considered positive options.

[0125] Results of sensory evaluation tests by consumers: After using Moringa essence, 90.00% of the subjects believed that [the product has a pleasant smell]; 96.67% of the subjects believed that [the product is absorbed quickly when used]; 93.33% of the subjects believed that [the product feels good on the skin]; 93.33% of the subjects believed that [the product is gentle and non-irritating when used]; 96.67% of the subjects believed that [the skin is not sticky after using the product].

[0126] Table 20 Statistics of the results of the efficacy evaluation part of the questionnaire survey of subjects (n=30)

[0127]

[0128] Rating criteria: 5-strongly agree / satisfied; 4-agree / satisfied; 3-average; 2-disagree / dissatisfied; 1-strongly disagree / strongly dissatisfied. Ratings > 3 are considered positive options.

[0129] Results of the efficacy evaluation test by consumers: After using Moringa essence for 14 days (D14) and 28 days (D28), 60.00% and 76.67% of the subjects respectively believed that [skin sensitivity and redness were improved]; 66.67% and 86.67% of the subjects respectively believed that [skin barrier ability was improved]; 70.11% and 86.67% of the subjects respectively believed that [skin elasticity was improved]; 70. 00% and 86.67% of the subjects respectively believed that [skin dry lines and fine lines were improved]; 66.67% and 86.67% of the subjects respectively believed that [dull skin tone was improved]; 76.67% and 86.67% of the subjects respectively believed that [skin hydration was improved]; 83.33% and 93.33% of the subjects respectively believed that [skin felt lastingly moisturized]; 96.67% and 100.00% of the subjects respectively believed that [overall, they were satisfied with the use of the product].

[0130] 3. Moringa Essence Water

[0131] The raw materials are calculated based on 100% total mass, including moringa seed oil liposome: 1-3%, dipropylene glycol: 2-5%, EDTA-2Na: 0.01%, betaine: 0.5-1%, ammonium acryloyldimethyltaurate / VP copolymer: 0.15-0.2%, xanthan gum: 0.1-0.2%, p-hydroxyacetophenone: 0.3-0.5%, 1,2-hexanediol: 0.3-0.5%, and the balance is water.

[0132] The preparation method of the Moringa essence water comprises the following steps: pre-dispersing xanthan gum and ammonium acryloyldimethyltaurate / VP copolymer in phase A into water for swelling; after complete swelling, adding the remaining raw materials of phase A, heating to 60-70° C. for complete dissolution, and cooling at room temperature; adding phase B at below 40° C., and stirring at a low speed for uniform mixing.

[0133] Table 21 Moringa Essence Water Formula

[0134]

[0135] (1) In vitro evaluation of firming and anti-wrinkle efficacy:

[0136] Table 22DPPH free radical scavenging rate

[0137]

[0138] Under laboratory conditions, the average DPPH free radical scavenging rate of Moringa essence water was 23.75%±1.25%, which was significantly different from that of the negative control (p<0.05). The DPPH free radical scavenging rate of the positive control was >25%, and the reaction system was effective, verifying that Moringa essence water has firming and anti-wrinkle effects.

[0139] Table 23 Collagenase inhibition rate

[0140]

[0141] Under the conditions of this experiment, the inhibition rate of Moringa essence water on collagenase was 10.23%. By comparing with the blank control, it was shown that Moringa essence water has the effect of inhibiting the production of collagenase.

[0142] (2) Human skin patch test

[0143] Table 24 Human skin patch test results

[0144]

[0145] Test results: The results of the human skin patch test showed that 30 subjects had no adverse skin reactions in the test area 0.5h, 24h, and 48h after removing the test patch tester, indicating that Moringa essence water is non-irritating to the human body surface.

[0146] (3) Use sensory evaluation:

[0147] Table 25 Sensory evaluation results

[0148]

[0149] Sensory evaluation results: The spreadability, moisturizing, permeability, uniformity, fineness and direct usability of Moringa essence water are all excellent, and the skin feels refreshing and is easy to absorb.

[0150] (4) Human efficacy evaluation test

[0151] Table 26 Statistical table of test results of moisture content of stratum corneum (n=30)

[0152]

[0153] *p<0.05 / **p<0.01 indicates that the index value is improved after using the sample, and the difference is statistically significant.

[0154] Test results of stratum corneum moisture content: Compared with before using Moringa essence water (D0), the stratum corneum moisture content increased after using the sample for 14 days (D14) and 28 days (D28), and the difference in stratum corneum moisture content compared with D0 was statistically significant (p < 0.05), and the increase rates were 11.21% and 23.57%, respectively.

[0155] Table 27 TEWL value test results statistics (n = 30)

[0156]

[0157] *p<0.05 / **p<0.01 indicates that the index value is improved after using the sample, and the difference is statistically significant.

[0158] Transepidermal water loss TEWL value test results: Compared with before using Moringa essence water (D0), the TEWL values ​​of transepidermal water loss decreased after using the sample for 14 days (D14) and 28 days (D28), and the difference with the TEWL values ​​of D0 was statistically significant (p < 0.05), and the decrease rates were 15.46% and 18.12%, respectively.

[0159] (5) Consumer use test

[0160] The subjects should visit the laboratory 14 days (D14) and 28 days (D28) after using the samples, clean the test areas with cleaning products, dry them and sit quietly in a constant temperature and humidity room. During the sitting period, they should fill in the questionnaire based on their subjective feelings after using the samples.

[0161] Table 28 Statistical table of sensory evaluation results of the questionnaire survey of subjects (n=30)

[0162]

[0163] Scoring criteria: 5-strongly agree; 4-agree; 3-neutral; 2-disagree; 1-strongly disagree. Scores > 3 are considered positive options.

[0164] Results of sensory evaluation tests by consumers: After using Moringa Essence Water, 93.33% of the subjects believed that [the product has a pleasant smell]; 96.67% of the subjects believed that [the product is absorbed quickly when used]; 96.67% of the subjects believed that [the product feels good on the skin]; 96.67% of the subjects believed that [the product is gentle and non-irritating when used]; 96.67% of the subjects believed that [the skin is not sticky after using the product].

[0165] Table 29 Results of the efficacy evaluation part of the questionnaire survey of subjects (n=30)

[0166]

[0167] Rating criteria: 5-strongly agree / satisfied; 4-agree / satisfied; 3-average; 2-disagree / dissatisfied; 1-strongly disagree / strongly dissatisfied. Ratings > 3 are considered positive options.

[0168] Results of the efficacy evaluation test by consumers: After using Moringa Essence Water for 14 days (D14) and 28 days (D28), 66.67% and 83.33% of the subjects respectively believed that [skin sensitivity and redness were improved]; 76.67% and 86.67% respectively believed that [skin barrier ability was improved]; 76.67% and 86.67% respectively believed that [skin elasticity was improved]; 70.0 0% and 86.67% of the subjects thought that [skin fine lines and dry lines were improved]; 76.67% and 86.67% of the subjects thought that [dull skin tone was improved]; 80.00% and 86.67% of the subjects thought that [skin hydration was improved]; 86.67% and 93.33% of the subjects thought that [skin felt lastingly moisturized]; 100.00% and 100.00% of the subjects thought that [overall, they were satisfied with the product].

[0169] The embodiments described above are merely descriptions of preferred implementation modes of the present invention and are not intended to limit the scope of the present invention. Without departing from the design spirit of the present invention, various modifications and improvements made to the technical solutions of the present invention by ordinary technicians in this field should all fall within the protection scope determined by the claims of the present invention.

Claims

1. A method for preparing a Moringa seed oil liposome composition, characterized in that: The method comprises the following steps: weighing cholesterol, lecithin, moringa seed oil and TW-80, adding anhydrous ethanol, ultrasonically dissolving, removing the organic solvent by rotary evaporation to form a lipid film, adding water for activation, and ultrasonically dissolving until a solution with a uniform texture is formed to obtain a liposome complex containing moringa seed oil.

2. The preparation method according to claim 1, characterized in that: The method specifically comprises the following steps: weighing cholesterol, lecithin, moringa seed oil and TW-80 in a round-bottom flask in a mass ratio of 1:4:1:1, adding 30-40 mL of anhydrous ethanol, and dissolving by ultrasound for 10-20 min; removing the organic solvent by rotary evaporation at a temperature of 45-50° C. and a vacuum degree of 0.6-0.8 Bar to form a lipid film, and then adding 40-50 mL of water at a constant temperature of 45-50° C. and a vacuum degree of 0.6-0.8 Bar to activate for 10-20 min; and ultrasound is performed until a solution with a uniform texture is formed to obtain a liposome complex containing moringa seed oil.

3. The preparation method according to claim 1, characterized in that: The moringa seed oil is prepared by a supercritical extraction method, comprising the following steps: Crush the Moringa seeds and load them into the extraction kettle, turn on the carbon dioxide switch, adjust the pressure and temperature of the extraction kettle and the first separation kettle and the second separation kettle, adjust the valve to make it stable, the carbon dioxide fluid is fully in contact with the Moringa seed material in the extraction kettle, and the carbon dioxide fluid carrying Moringa seed oil enters the first separation kettle through a pipeline to perform the first separation of the Moringa seed oil, and then a small amount of unseparated Moringa seed oil is allowed to enter the second separation kettle with the carbon dioxide fluid for secondary separation. The separated carbon dioxide is circulated through a loop, and when the preset pressure and temperature of the extraction kettle, the first separation kettle and the second separation kettle are stabilized, the Moringa seed oil is collected from the first separation kettle and the second separation kettle in batches.

4. The preparation method according to claim 3, characterized in that: Adjust the pressure and temperature of the extraction kettle, the first separation kettle and the second separation kettle. When the extraction pressure reaches 35 MPa and the extraction temperature reaches 40°C, the pressure of the first separation kettle reaches 12 MPa and the separation temperature reaches 45°C, and the pressure of the second separation kettle reaches 5 MPa and the separation temperature reaches 35°C, adjust the valve to stabilize; After the preset pressure and temperature of the extraction kettle, the first separation kettle and the second separation kettle are stabilized for 10-20 minutes, Moringa seed oil is collected from the first separation kettle and the second separation kettle every 30 minutes, and the overall extraction time is 3 hours.

5. The Moringa seed oil liposome composition prepared by the method according to any one of claims 1 to 4.

6. Application of the Moringa seed oil liposome composition according to claim 5 in cosmetics.

7. The use according to claim 6, characterized in that: The cosmetics are moisturizing lotion, essence or essence water.

8. A Moringa moisturizing water, characterized in that: It is composed of the following raw materials in percentage by weight: Moringa seed oil liposome: 1-3%, 1,3-butylene glycol: 2-5%, glycerol: 5-6%, carbomer: 0.1-0.15%, D-panthenol: 0.5-1%, triethanolamine: 0.1-0.3%, PE9010: 0.8%, the balance is water; The preparation method of the Moringa moisturizing water comprises the following steps: pre-dispersing the carbomer in phase A into water for swelling; after complete swelling, adding the remaining raw materials of phase A, heating to 60-70° C., and cooling at room temperature; adding phase B at below 40° C., adjusting the pH to 5.0-6.5, and stirring and mixing evenly; and sequentially adding phase C, stirring and mixing at a low speed evenly.

9. A Moringa essence, characterized in that: It is composed of the following raw materials in percentage by weight: Moringa seed oil liposome: 1-3%, xanthan gum: 0.2-0.3%, glycerol: 2-5%, sodium hyaluronate: 0.1-0.2%, dipropylene glycol: 2-5%, p-hydroxyacetophenone: 0.3-0.5%, 1,2-hexanediol: 0.3-0.5%, tetrahydromethylpyrimidine carboxylic acid: 0.1-0.2%, the balance is water; The preparation method of the moringa essence comprises the following steps: pre-dispersing the xanthan gum in phase A into water for swelling; after complete swelling, adding the remaining raw materials of phase A, heating to 60-70° C. for dissolution, and cooling at room temperature; pre-heating phase B to 60-75° C. for dissolution for standby use, adding phase B at below 40° C., and stirring at low speed for uniform mixing; adding raw materials of phase C in sequence, and stirring at low speed for uniform mixing.

10. A Moringa essence water, characterized in that: It is composed of the following raw materials in percentage by weight: Moringa seed oil liposome: 1-3%, dipropylene glycol: 2-5%, EDTA-2Na: 0.01%, betaine: 0.5-1%, ammonium acryloyldimethyltaurate / VP copolymer: 0.15-0.2%, xanthan gum: 0.1-0.2%, p-hydroxyacetophenone: 0.3-0.5%, 1,2-hexanediol: 0.3-0.5%, the balance is water; The preparation method of the Moringa essence water comprises the following steps: pre-dispersing xanthan gum and ammonium acryloyldimethyltaurate / VP copolymer in phase A into water for swelling; after complete swelling, adding the remaining raw materials of phase A, heating to 60-70° C. for complete dissolution, and cooling at room temperature; adding phase B at below 40° C., and stirring at a low speed for uniform mixing.

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