Ectoine supramolecular emulsifier as well as preparation method and application thereof
By preparing ectoine supramolecular emulsifier powder, the problems of high addition amount, skin irritation and stability of traditional emulsifiers in cosmetics have been solved, achieving a low-irritation and high-stability emulsification effect, and improving the moisturizing, firming and anti-wrinkle performance of cosmetics.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-02-06
- Publication Date
- 2026-04-14
AI Technical Summary
Existing traditional emulsifiers have problems such as skin irritation when added in large quantities in cosmetics, large and uneven emulsion particle size, poor system stability, and poor compatibility with ectoine, which affects its moisturizing and repairing effects.
Ectoin supramolecular emulsifier powder was prepared by dispersing ectoin, polymer, and sodium fatty acid in water, adding fatty acids and alcohol, and then spray drying. This powder forms nanostructured aggregates for use in cosmetics.
It achieves emulsification with low addition amount, low irritation, and high stability, improving the moisturizing, stability, and firming and anti-wrinkle properties of cosmetics, making it suitable for industrial production.
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Figure CN121845958A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to an ectoine supramolecular emulsifier, its preparation method, and its application, belonging to the field of supramolecular emulsifier preparation technology. Background Technology
[0002] Ectoine, scientifically known as tetrahydromethylpyrimidine carboxylic acid, is a naturally occurring water-soluble zwitterionic amino acid derivative synthesized by halophilic extremophiles under extreme conditions such as high salt, high temperature, and ultraviolet radiation. It acts as an osmotic pressure regulator to maintain cell structural stability. Due to its excellent biological activity, it shows broad application prospects in cosmetics, pharmaceuticals, and other fields. Especially in skincare products, it can form a hydrating protective film on the cell surface, binding a large number of water molecules to achieve long-lasting moisturizing. Simultaneously, it stabilizes cell membranes and protein structures, resists external stimuli such as ultraviolet radiation and free radicals, accelerates the repair of damaged skin cells, and reduces transepidermal water loss, exhibiting significant repairing effects on sensitive skin and skin with damaged barriers.
[0003] Emulsification systems form the fundamental framework of cosmetic formulations. Traditional emulsifiers widely used in the industry mainly include ionic emulsifiers (such as sodium cetearyl sulfate), nonionic emulsifiers (such as fatty alcohol polyoxyethylene ethers and polyethylene glycol fatty acid esters), and glycerides. These emulsifiers generally suffer from excessive dosage, and even with increased dosage, many inherent defects remain. Firstly, high dosages of traditional emulsifiers can easily irritate the skin, damaging the skin barrier function and causing discomfort such as redness and dryness. This contradicts the skin-repairing properties of ectoine for sensitive skin, greatly limiting its application in sensitive skin products. Secondly, the emulsions formed by traditional emulsifiers have large and unevenly distributed particles, resulting in poor system stability. During storage and transportation, problems such as layering, flocculation, and demulsification can easily occur, directly leading to the loss or inactivation of active ingredients like ectoine, weakening the product's sustained efficacy. Furthermore, some traditional emulsifiers have poor compatibility with ectoine, potentially altering the molecular structure of ectoine through chemical bonding, further weakening its core biological activities such as moisturizing and repairing.
[0004] To address the inherent drawbacks of traditional emulsifiers, supramolecular emulsification technology has emerged with its unique advantages, offering a new direction for resolving the contradiction between the stability and safety of formulation systems. Unlike traditional emulsifiers that rely on chemical bonds, supramolecular emulsifiers achieve molecular self-assembly based on intermolecular non-covalent bonds (hydrogen bonds, hydrophobic interactions, van der Waals forces, etc.), forming aggregates with unique nanostructures. Therefore, they possess core advantages such as high emulsification efficiency, low addition amount, low irritation, and excellent stability.
[0005] Currently, some studies have explored the use of ectoine in combination with surfactants to reduce irritation, but no supramolecular emulsifiers for ectoine have yet been identified.
[0006] Therefore, there is an urgent need to develop an ectoine supramolecular emulsifier that can fully leverage the inherent advantages of supramolecular technology—low irritation and high stability—while simultaneously achieving the performance of ectoine itself; and when used in emulsions, it should have high emulsification efficiency, low addition amount, low irritation, and excellent stability. Summary of the Invention
[0007] To address the aforementioned problems, this invention provides an ectoine supramolecular emulsifier, its preparation method, and its application. Specifically, this invention first disperses ectoine, a polymer, and sodium fatty acid in water to obtain a dispersion; then, fatty acids and an alcohol are added to the dispersion to obtain a suspension; finally, the suspension is spray-dried to obtain ectoine supramolecular emulsifier powder. The ectoine supramolecular emulsifier powder prepared by this invention is used to prepare emulsions, exhibiting high emulsification efficiency, low addition amount, low irritation, and excellent stability.
[0008] The first objective of this invention is to provide a method for preparing ectoine supramolecular emulsifier powder, comprising the following steps: (1) Disperse ectoine, polymer, and sodium fatty acid in water to obtain a dispersion; (2) Add fatty acids and alcohol to the dispersion, stir evenly to obtain a suspension; (3) The suspension was dried to obtain ectoine supramolecular emulsifier powder; The mass ratio of ectoine, polymer, sodium fatty acid, fatty acid, alcohol, and water is 4-50:2-18:0-5:4-22:5-90:320.
[0009] Preferably, the polymer in step (1) is one or more of carbomer, sodium polyglutamate, sodium hyaluronate, chitosan, and sugars; wherein, carbomer includes one or two of carbomer 980 and carbomer U20; and sugars include one or more of aloe polysaccharide, tremella polysaccharide, chondrus crispus extract, hydrolyzed sclerotium gum, dextran, xanthan gum, fructooligosaccharide, gum arabic, and starch.
[0010] Preferably, the sodium fatty acid in step (1) is one or more of sodium linoleate, sodium palmitate, sodium myristate, sodium oleate, sodium cocoate, sodium laurylate, sodium palmitate, sodium stearate, and sodium isostearate.
[0011] Preferably, in step (1), the dispersion is ultrasonic dispersion at 25-40℃ and 50-500W for 0.5-2h.
[0012] Preferably, the fatty acid in step (2) is one or more of the following: undecenoic acid, linolenic acid, stearic acid, linoleic acid, palmitoleic acid, myristic acid, tall oil acid, oleic acid, hydrogenated coconut oil acid, coconut oil acid, caprylic acid, capric acid, lauric acid, palmitic acid, isostearic acid, butyloctanoic acid, docosahexaenoic acid, and eicosapentaenoic acid.
[0013] Preferably, the alcohol in step (2) is one or more of butyloctanol, decanol, decyltetradecol, arachidonicol, hexyldecol, cetyl alcohol, cetearyl alcohol, polydimethylsiloxane alcohol, myristol, behenol, octyldodecyl alcohol, lanosterol, lanolin alcohol, cocoyl alcohol, isocetol, isostearol, stearol, oleyl alcohol, lauryl alcohol, and palm oil alcohol.
[0014] Preferably, the stirring in step (2) is carried out at 60-110℃ and 400-650rpm for 3-11 hours.
[0015] Preferably, the drying in step (3) is spray drying, specifically spray drying at 180-200℃ and 0.2-0.5MPa for 3-8 hours.
[0016] The second objective of this invention is to prepare ectoine supramolecular emulsifier powder using the method described herein.
[0017] Preferably, the particle size range of the ectoine supramolecular emulsifier powder is 600-700 nm.
[0018] The third objective of this invention is the application of the ectoine supramolecular emulsifier powder described herein in the preparation of pharmaceuticals or cosmetics.
[0019] Preferably, cosmetics include ointments, creams, lotions, etc.; ectoine supramolecular emulsifier powder can enhance the moisturizing, stability, irritation relief, firming and anti-wrinkle functions of cosmetics; medicines include dressings, creams, etc.
[0020] The fourth objective of this invention is to provide a cosmetic product that uses the ectoine supramolecular emulsifier powder described in this invention.
[0021] Preferably, the preparation method of the cosmetic is as follows: Ectoin supramolecular emulsifier powder was added to the oil phase and mixed evenly, then added to the aqueous phase and homogenized and emulsified to obtain the cosmetic product. The mass concentration of ectoine supramolecular emulsifier powder in the entire cosmetic product is 0.1-2%.
[0022] Preferably, preservatives and some functional ingredients can be added at appropriate times as needed in the preparation method of cosmetics.
[0023] Preferably, cosmetics include lotions, creams, and lotions; different aqueous and oil phases can be selected as needed.
[0024] The fifth objective of this invention is to provide a method for improving the storage stability and multifunctionality of emulsions, which employs the ectoine supramolecular emulsifier powder described in this invention.
[0025] Preferably, multifunctionality refers to enhancing properties such as moisturizing, relieving irritation, skin repair, firming and anti-wrinkle effects.
[0026] The technical effects of this invention are as follows: (1) The ectoin supramolecular emulsifier powder prepared in this invention is used to prepare emulsions, which have high emulsification efficiency, low addition amount, low irritation and excellent stability.
[0027] (2) The method for preparing ectoin supramolecular emulsifier powder by the present invention is simple, low in cost, and suitable for industrial production; it can be used in the fields of medicine and cosmetics.
[0028] (3) The ectoin supramolecular emulsifier powder of the present invention has a particle size of 600-700 nm and an EAI index of 91 nm. 2 The emulsion has a concentration of ≥ / g, an ESI index of ≥82%, and a cell viability retention rate of ≥91%. The prepared emulsion is homogeneous and stable without stratification after being placed in a high temperature and high humidity environment for 1 month; it is also homogeneous and stable without stratification after a freeze-thaw cycle for 1 month. Furthermore, the prepared cosmetic has excellent firming and anti-wrinkle properties, and is homogeneous and stable without stratification after being placed in a high temperature and high humidity environment for 1 month; it is also homogeneous and stable without stratification after a freeze-thaw cycle for 1 month. Attached Figure Description
[0029] Figure 1 The infrared spectrum of the ectoin supramolecular emulsifier powder prepared in Example 1.
[0030] Figure 2 The images show actual test results for the stability of Examples 1-3, 17, 18 and Comparative Examples 1-5. Detailed Implementation
[0031] The preferred embodiments of the present invention are described below. It should be understood that the embodiments are for better explanation of the present invention and are not intended to limit the present invention.
[0032] Test method: 1. Emulsifying activity and stability (EAI / ESI index) test: Add the emulsifier powder to water to prepare an emulsifier aqueous solution with a mass concentration of 1%; weigh the emulsifier aqueous solution and liquid paraffin at a mass ratio of 1:4, vortex mix for 30 s to form an emulsion; take 0.1 mL of the emulsion and dilute it with distilled water to 10 mL (dilution factor N=100).
[0033] After standing for 10 min, using distilled water as a blank, measure the absorbance A0 at 500 nm. Substitute the absorbance into the formula to calculate EAI; EAI(m) 2 / g)={(2×2.303) / [C×(1-φ)×10 4 ]}×A 500 × dilution factor; where φ is 0.2; Transfer the emulsion to centrifuge tubes and let it stand for 4 hours. Take 0.1 mL of the upper layer of emulsion each time, dilute it, and measure the absorbance A. t ; Calculate ESI using the formula:
[0034] The emulsion was subjected to accelerated aging tests under two conditions: a high temperature and high humidity (40℃ / 75% RH) constant temperature and humidity chamber and a freeze-thaw cycle (alternating between -20℃ and 25℃, with one cycle completed every 24 hours). After one month, the emulsion was observed to determine whether it was uniform and stable and whether it separated into layers.
[0035] 2. In vitro hyaluronidase activity inhibition test: (1) Take four clean test tubes and label them A, B, C and D respectively. Add 50 μL of the sample to be tested (the emulsion obtained in Example 17, Comparative Example 7 and Comparative Example 8) to each of test tubes A and B. Add 50 μL of distilled water to each of test tubes C and D. Add 50 μL of 500 U / mL hyaluronidase solution to each of test tubes A and C. Add 50 μL of pH=5.6 acetate buffer to each of test tubes B and D. Place the test tubes in a 37 ℃ incubator for 20 min.
[0036] (2) Add 10 μL of 2.5 mol / L CaCl2 solution to each of the four test tubes, and then place them in a 37 ℃ incubator for 20 min.
[0037] (3) Add 50 μL of 0.5 mg / mL sodium hyaluronate solution to test tubes A and C, and add 50 μL of pH 5.6 acetate buffer to test tubes B and D. Place the test tubes in an incubator at 37 ℃ for 40 min, and then take them out and let them stand at room temperature for 10 min.
[0038] (4) Add 50 μL of distilled water, 10 μL of 5 mol / L NaOH solution and 50 μL of acetylacetone solution to the four test tubes respectively. Place the test tubes in a water bath for 30 min of boiling water, then in an ice bath for 10 min, and finally at room temperature for 10 min.
[0039] (5) Add 100 μL of P-DAB reagent to each test tube, and then measure the absorbance at 530 nm using an ELISA reader. Calculate the hyaluronic acid phytase inhibition rate using the following formula: Hyaluronidase inhibition rate (%) = [(CD) - (AB)] / (CD) × 100% In the formula: A is the OD value of the sample solution; B is the OD value of the blank sample; C is the OD value of the control sample solution; and D is the OD value of the blank control sample.
[0040] 3. In vitro elastase activity inhibition test: (1) Take 4 clean test tubes and label them A, B, C and D respectively. Add 25 μL of the sample to be tested (the emulsion obtained in Example 17, Comparative Example 7 and Comparative Example 8) to each of test tubes A and B. Add 25 μL of distilled water to each of test tubes C and D. Add 25 μL of 0.171 U / mL porcine pancreatic elastase solution to each of test tubes A and C. Add 25 μL of Tris-HCl buffer solution with pH=8.0 to each of test tubes B and D.
[0041] (2) Add 50 μL of 1 mmol / L AAAPVN (N-succinyl-alanine-alanine-p-nitroaniline) solution to each of the four test tubes, mix well, and incubate at room temperature for 15 min. Then, measure the absorbance at 420 nm using a microplate reader. Calculate the elastase inhibition rate according to the following formula: Elastase inhibition rate (%) = (1 - (AB) / (CD)) × 100% In the formula: A is the OD value of the sample solution; B is the OD value of the blank sample; C is the OD value of the control sample solution; and D is the OD value of the blank control sample.
[0042] 4. Cell compatibility test: The MTT (3-(4,5-dimethylthiazolyl-2-yl)-2,5-diphenyltetrazolium bromide) method is a classic cell proliferation / toxicity assay that indirectly reflects cell number and viability by detecting the ability of mitochondrial dehydrogenases in living cells to reduce MTT to formazan.
[0043] Take fibroblasts in the logarithmic growth phase and adjust the density (1×10⁻⁶). 4 (cells / well, 96-well plate); add 100 μL of complete culture medium to each well and incubate for 24 h to allow the cells to adhere; Experimental Groups: Blank control group (culture medium only, no cells); Negative control group (untreated cells); Experimental group (0.5% emulsifier aqueous solution); Positive control group (10% PDGF stimulation); Add 10 μL of MTT solution (5 mg / mL, prepared in PBS) to each well (final concentration 0.5 mg / mL); incubate at 37 °C for 4 h, then discard the supernatant; add 150 μL of DMSO to each well and shake slowly for 10 min to dissolve the crystals; measure the absorbance at 490 nm using a microplate reader.
[0044] The formula for calculating cell viability retention rate is as follows: Cell viability (%) = (OD value of experimental group - OD value of blank group) / (OD value of control group - OD value of blank group) × 100% Raw materials used in the examples: Ectocin: 99%; Carbomer 980: 99%; Sodium palmitate: 99%; Cocolate acid: 99%; Coconut oil alcohol: 99%; Sodium polyglutamate: 98%; molecular weight 50-100 kDa; Sodium myristate: 98%; Eicosapentaenoic acid: 98%; Palm oil alcohol: 98% Sodium hyaluronate: molecular weight 5K-2000KDa; Sodium lauryl var.: 97%; Cetearyl alcohol: 99% Chitosan: Deacetylation degree 95%; Sodium stearate: 98%; Hydrogenated coconut oil acid: 99%; Polydimethylsiloxane alcohol: 99%; Aloe polysaccharides: BR, 60%; Sodium palmitate: 99%; Betaine alcohol: 98%; Carbomer U20: 100%; Sodium isostearate: 98% Hexanoic acid: 99%; Lanolin alcohol: 99%; Hydrolyzed sclerotium gum: 98%; Chondrus crispus extract: 98%; Polyaspartic acid: molecular weight 10 kDa.
[0045] Example 1 A method for preparing ectoine supramolecular emulsifier powder includes the following steps: (1) Disperse ectoine, carbomer 980 and sodium palmitate in water and ultrasonically disperse at 30°C and 350W for 1 hour to obtain a dispersion. (2) Add coconut oil acid and coconut oil alcohol to the dispersion, stir at 80°C and 500 rpm for 6 h to obtain a suspension; (3) The suspension was spray-dried at 190℃ and 0.3MPa for 5h to obtain ectoine supramolecular emulsifier powder; The mass ratio of ectoine, carbomer 980, sodium palmitate, cocoacid, cocoa alcohol, and water is 30:10:3:13:44:320.
[0046] Figure 1 Infrared spectrum of the ectoine supramolecular emulsifier powder prepared in Example 1. Figure 1 It can be seen that: compared to ectoine, the emulsifier at 3426 cm -1 The presence of a broad absorption peak indicates the presence of numerous hydrogen bonds in the system, confirming the formation of a supramolecular system.
[0047] Example 2 A method for preparing ectoine supramolecular emulsifier powder includes the following steps: (1) Disperse ectoine, sodium polyglutamate and sodium myristate in water and ultrasonically disperse at 35°C and 400W for 1.5h to obtain a dispersion; (2) Add eicosapentaenoic acid and palm oil alcohol to the dispersion, and stir at 70°C and 500 rpm for 8 hours to obtain a suspension; (3) The suspension was spray-dried at 200℃ and 0.2MPa for 7h to obtain ectoine supramolecular emulsifier powder; The mass ratio of ectoine, sodium polyglutamate, sodium myristate, eicosapentaenoic acid, palmitole alcohol, and water is 40:15:5:20:80:320.
[0048] Example 3 A method for preparing ectoine supramolecular emulsifier powder includes the following steps: (1) Disperse ectoine, sodium hyaluronate and sodium laurylate in water and ultrasonically disperse at 25°C and 400W for 1.5h to obtain a dispersion; (2) Add palmitoleic acid and cetearyl alcohol to the dispersion, and stir at 75°C and 500 rpm for 8 hours to obtain a suspension; (3) The suspension was spray-dried at 200℃ and 0.2MPa for 7h to obtain ectoine supramolecular emulsifier powder; The mass ratio of ectoine, sodium hyaluronate, sodium laurate, palmitoleic acid, cetearyl alcohol, and water is 20:13:4:18:45:320.
[0049] Example 4 A method for preparing ectoine supramolecular emulsifier powder includes the following steps: (1) Disperse ectoine, chitosan and sodium stearate in water and ultrasonically disperse at 40℃ and 300W for 1.5h to obtain a dispersion; (2) Add hydrogenated coconut oil acid and polydimethylsiloxane alcohol to the dispersion, and stir at 90°C and 400 rpm for 8 hours to obtain a suspension; (3) The suspension was spray-dried at 180℃ and 0.5MPa for 5h to obtain ectoine supramolecular emulsifier powder; The mass ratio of ectoine, chitosan, sodium stearate, hydrogenated coconut oil acid, polydimethylsiloxane alcohol, and water is 50:18:2:22:8:320.
[0050] Example 5 A method for preparing ectoine supramolecular emulsifier powder includes the following steps: (1) Disperse ectoine, aloe polysaccharide and sodium palmitate in water and ultrasonically disperse at 35°C and 300W for 1 hour to obtain a dispersion; (2) Add eicosapentaenoic acid and behenol to the dispersion, and stir at 100°C and 400 rpm for 5 h to obtain a suspension; (3) The suspension was spray-dried at 190℃ and 0.5MPa for 8h to obtain ectoine supramolecular emulsifier powder; The mass ratio of ectoine, aloe polysaccharide, sodium palmitate, eicosapentaenoic acid, behenol, and water is 45:12:1:6:36:320.
[0051] Example 6 In step (1) of Example 1, Carbomer 980 was changed to Carbomer U20, while the rest remained the same as in Example 1, to obtain Ectoin supramolecular emulsifier powder.
[0052] Example 7 In step (1) of Example 1, sodium palmitate was replaced with sodium isostearate, while other steps remained the same as in Example 1, resulting in ectoine supramolecular emulsifier powder.
[0053] Example 8 In step (2) of Example 1, coconut oil acid was replaced with lauric acid, while other steps remained the same as in Example 1, resulting in ectoine supramolecular emulsifier powder.
[0054] Example 9 In step (2) of Example 1, coconut oil alcohol was changed to lanolin alcohol, while the rest remained the same as in Example 1, to obtain ectoin supramolecular emulsifier powder.
[0055] Example 10 In step (1) of Example 1, Carbomer 980 was changed to hydrolyzed sclerotium gum, while the rest remained the same as in Example 1, resulting in ectoine supramolecular emulsifier powder.
[0056] Example 11 In step (1) of Example 1, Carbomer 980 was changed to Carrageenan extract, while the rest remained the same as in Example 1, resulting in Ectoin supramolecular emulsifier powder.
[0057] Example 12 The mass ratio of ectoine, carbomer 980, sodium palmitate, cocoacid, cocoa alcohol, and water in Example 1 was adjusted to 50:18:5:22:90:320, while other aspects remained the same as in Example 1, to obtain ectoine supramolecular emulsifier powder.
[0058] Example 13 The mass ratio of ectoine, carbomer 980, sodium palmitate, cocoacid, cocoa alcohol, and water in Example 1 was adjusted to 4:2:5:20:5:320, while other aspects remained the same as in Example 1, to obtain ectoine supramolecular emulsifier powder.
[0059] Example 14 The reaction temperature in step (2) of Example 1 was adjusted to 110°C, while other steps remained the same as in Example 1, to obtain ectoine supramolecular emulsifier powder.
[0060] Example 15 The reaction temperature in step (2) of Example 1 was adjusted to 60°C, while other steps remained the same as in Example 1, to obtain ectoine supramolecular emulsifier powder.
[0061] Example 16 The reaction time in step (2) of Example 1 was adjusted to 11h, while other steps remained the same as in Example 1, to obtain ectoine supramolecular emulsifier powder.
[0062] The obtained emulsifier was subjected to performance testing, and the test results are as follows: Table 1
[0063] Comparative Example 1 A method for preparing ectoine supramolecular emulsifier powder includes the following steps: Ectoin, carbomer 980, sodium palmitate, cocoacid, cocoyl alcohol, and water were dispersed by ultrasonication at 30°C and 350W for 1 hour in a mass ratio of 30:10:3:13:44:320, followed by stirring at 80°C and 500rpm for 6 hours to obtain a suspension. The suspension was then spray-dried at 190°C and 0.3MPa for 5 hours to obtain ectoin supramolecular emulsifier powder.
[0064] Comparative Example 2 In Example 1, carbomer 980 was replaced with polyaspartic acid, while other aspects remained the same as in Example 1, resulting in ectoine supramolecular emulsifier powder.
[0065] Comparative Example 3 The sodium palmitate in Example 1 was replaced with sodium octanoate, while other aspects remained the same as in Example 1, resulting in ectoine supramolecular emulsifier powder.
[0066] Comparative Example 4 In Example 1, coconut oil acid was replaced with hexanoic acid, while other aspects remained the same as in Example 1, resulting in ectoine supramolecular emulsifier powder.
[0067] Comparative Example 5 In Example 1, coconut oil alcohol was replaced with octanol, while other aspects remained the same as in Example 1, resulting in ectoine supramolecular emulsifier powder.
[0068] Comparative Example 6 Adjust step (2) of Example 1 as follows: A dispersion was added to a mixture of coconut oil acid and coconut oil alcohol, and the mixture was stirred at 80°C and 500 rpm for 6 hours to obtain a suspension. Everything else remained the same as in Example 1, resulting in ectoine supramolecular emulsifier powder.
[0069] The obtained emulsifier was subjected to performance testing, and the test results are as follows: Table 2
[0070] Example 17 A method for preparing an emulsion based on the ectoine supramolecular emulsifier powder of Example 1 includes the following steps: Cetyl ethylhexanoate (7506), caprylic / capric triglyceride (gtcc), squalane, and polydimethylsiloxane were added to an oil pan and heated and stirred at 85°C and 600 rpm until completely dissolved. Ectoin supramolecular emulsifier powder from Example 1 was added, mixed evenly, and kept warm to obtain the oil phase. Add glycerin, 980 (carbomer), and water to an emulsifying vessel, heat at 85°C and 600 rpm and stir until completely dissolved to obtain the aqueous phase; Add the oil phase to the aqueous phase, homogenize at 2600 rpm for 5 min, and keep warm at 85℃ for 20 min; Then, the temperature was lowered to 55°C, arginine was added, and stirring and cooling continued. When the temperature reached 40°C, preservative (PE9010) was added. After the temperature dropped to room temperature, the finished emulsion was obtained. The emulsion contains, by mass percentage, 4% cetyl ethylhexanoate (7506), 3% caprylic / capric triglyceride (GTCC), 3% squalane, 1% polydimethylsiloxane, 5% glycerol, 0.3% 980 (carbomer), 1% ectoine supramolecular emulsifier powder from Example 1, 0.3% arginine, 0.5% preservatives, and the remainder is water.
[0071] The obtained emulsion was subjected to performance testing, and the test results are as follows: Table 3
[0072] Example 18 A method for preparing a cream based on the ectoine supramolecular emulsifier powder of Example 1 includes the following steps: Cetyl ethylhexanoate (7506), caprylic / capric triglyceride (gtcc), squalane, cetearyl alcohol, and polydimethylsiloxane were added to an oil pan and heated and stirred at 85°C and 450 rpm until completely dissolved. Ectoin supramolecular emulsifier powder from Example 1 was added, mixed evenly, and kept warm to obtain the oil phase. Add glycerin and water to an emulsifying pot, heat and stir at 85°C and 450 rpm until completely dissolved to obtain the aqueous phase; Add the oil phase to the aqueous phase, homogenize at 3000 rpm for 2 min, add Clariant Aristoflex AVC, homogenize at 2500 rpm for 5 min, and keep warm at 85℃ for 20 min. Then, the temperature is lowered to 40°C, preservatives (PE9010) are added, and the finished cream is obtained after the temperature drops to room temperature. The cream contains, by weight percentage, 10% cetyl ethylhexanoate (7506), 7% caprylic / capric triglyceride (GTCC), 4.5% squalane, 1.5% cetearyl alcohol, 2% polydimethylsiloxane, 3% glycerin, 0.5% Clariant Aristoflex AVC, 1.5% ectoine supramolecular emulsifier powder from Example 1, 0.5% preservatives, and the remainder is water.
[0073] The obtained cream was subjected to performance testing, and the test results are as follows: Table 4
[0074] Example 19 A method for preparing a cream based on the ectoine supramolecular emulsifier powder of Example 1 includes the following steps: Add meadowfoam seed oil, caprylic / capric triglyceride (gtcc), squalane, cetearyl alcohol, polydimethylsiloxane, and shea butter to an oil pan, heat and stir at 85°C and 500 rpm until completely dissolved, add ectoine supramolecular emulsifier powder from Example 1, mix evenly, keep warm, and obtain the oil phase; Add glycerin and water to an emulsifying pot, heat and stir at 85°C and 450 rpm until completely dissolved to obtain the aqueous phase; Add the oil phase to the aqueous phase, homogenize at 3000 rpm for 2 min, add Clariant Aristoflex AVC, homogenize at 2500 rpm for 5 min, and keep warm at 85℃ for 20 min. Then, the temperature is lowered to 40°C, preservative (PE9010) is added, and the finished cream is obtained after the temperature drops to room temperature. The cream, by weight percentage, contains: meadowfoam seed oil 5%, caprylic / capric triglyceride (GTCC) 8%, squalane 3%, cetearyl alcohol 2.5%, polydimethylsiloxane 2%, shea butter 3%, glycerin 3%, Clariant Aristoflex AVC 0.8%, ectoine supramolecular emulsifier powder from Example 1 2%, preservatives 0.5%, and the remainder is water.
[0075] The obtained frost was subjected to performance testing, and the test results are as follows: Table 5
[0076] Comparative Example 7 In Example 17, the supramolecular emulsifier powder of ectoine was changed to ectoine, while the rest remained the same as in Example 17.
[0077] Comparative Example 8 In Example 17, the ectoine supramolecular emulsifier powder was changed to the ectoine supramolecular emulsifier powder in Comparative Example 1, while everything else remained the same as in Example 17.
[0078] The emulsions obtained in Example 17, Comparative Example 7, and Comparative Example 8 were subjected to in vitro hyaluronidase activity inhibition tests and in vitro elastase activity inhibition tests. The results are as follows: Table 6
[0079] Although the present invention has been disclosed above with reference to preferred embodiments, it is not intended to limit the present invention. Anyone skilled in the art can make various modifications and alterations without departing from the spirit and scope of the present invention. Therefore, the scope of protection of the present invention should be determined by the claims.
Claims
1. A method for preparing ectoine supramolecular emulsifier powder, characterized in that, Includes the following steps: (1) Disperse ectoine, polymer, and sodium fatty acid in water to obtain a dispersion; (2) Add fatty acids and alcohol to the dispersion, stir evenly to obtain a suspension; (3) The suspension was dried to obtain ectoine supramolecular emulsifier powder; The mass ratio of ectoine, polymer, sodium fatty acid, fatty acid, alcohol, and water is 4-50:2-18:0-5:4-22:5-90:
320.
2. The method according to claim 1, characterized in that, In step (1), the polymer is one or more of the following: carbomer, sodium polyglutamate, sodium hyaluronate, chitosan, and sugars; among which, carbomer includes one or two of carbomer 980 and carbomer U20; and sugars include one or more of the following: aloe polysaccharide, tremella polysaccharide, chondrus crispus extract, hydrolyzed sclerotium gum, dextran, xanthan gum, fructooligosaccharide, gum arabic, and starch.
3. The method according to claim 1, characterized in that, In step (1), the sodium fatty acid is one or more of sodium linoleate, sodium palmitate, sodium myristate, sodium oleate, sodium cocoate, sodium laurylate, sodium palmitate, sodium stearate, and sodium isostearate.
4. The method according to claim 1, characterized in that, In step (1), dispersion is performed at 25-40℃ and 50-500W ultrasonic dispersion for 0.5-2h; in step (2), uniform stirring is performed at 60-110℃ and 400-650rpm for 3-11h.
5. The method according to claim 1, characterized in that, In step (2), the fatty acids are one or more of the following: undecenoic acid, linolenic acid, stearic acid, linoleic acid, palmitoleic acid, myristic acid, tall oil acid, oleic acid, hydrogenated coconut oil acid, coconut oil acid, caprylic acid, capric acid, lauric acid, palmitic acid, isostearic acid, butyloctanoic acid, docosahexaenoic acid, and eicosapentaenoic acid; and in step (2), the alcohols are one or more of the following: butyloctanol, decanol, decyltetradecyl alcohol, arachidonic acid, hexyldecyl alcohol, cetyl alcohol, cetearyl alcohol, polydimethylsiloxane alcohol, myristol, behenol, octyldodecyl alcohol, lanosterol, lanolin alcohol, coconut oil alcohol, isocetol, isostearyl alcohol, stearyl alcohol, oleyl alcohol, lauryl alcohol, and palm oil alcohol.
6. The method according to claim 1, characterized in that, The drying process is spray drying, specifically spray drying at 180-200℃ and 0.2-0.5MPa for 3-8 hours.
7. The ectoin supramolecular emulsifier powder prepared by the method according to any one of claims 1-6.
8. The use of the ectoine supramolecular emulsifier powder according to claim 7 in the preparation of pharmaceuticals or cosmetics.
9. A cosmetic product, characterized in that, The ectoine supramolecular emulsifier powder described in claim 7 was used.
10. A method for improving the storage stability and multifunctionality of emulsions, characterized in that, The ectoine supramolecular emulsifier powder described in claim 7 was used.