CN114869795A - Preparation method of whitening composition for improving solubility of active components, product and application thereof - Google Patents

Preparation method of whitening composition for improving solubility of active components, product and application thereof Download PDF

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CN114869795A
CN114869795A CN202210322071.8A CN202210322071A CN114869795A CN 114869795 A CN114869795 A CN 114869795A CN 202210322071 A CN202210322071 A CN 202210322071A CN 114869795 A CN114869795 A CN 114869795A
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parts
composition
whitening
lecithin
solubility
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CN114869795B (en
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陈凤凤
杨钰澍
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Shanghai Fulai Biological High Tech Co ltd
Jiangnan University
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Shanghai Fulai Biological High Tech Co ltd
Jiangnan University
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/36Carboxylic acids; Salts or anhydrides thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/34Alcohols
    • A61K8/345Alcohols containing more than one hydroxy group
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/36Carboxylic acids; Salts or anhydrides thereof
    • A61K8/362Polycarboxylic acids
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/37Esters of carboxylic acids
    • A61K8/375Esters of carboxylic acids the alcohol moiety containing more than one hydroxy group
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/55Phosphorus compounds
    • A61K8/553Phospholipids, e.g. lecithin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/60Sugars; Derivatives thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/60Sugars; Derivatives thereof
    • A61K8/602Glycosides, e.g. rutin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/63Steroids; Derivatives thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/02Preparations for care of the skin for chemically bleaching or whitening the skin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/59Mixtures
    • A61K2800/592Mixtures of compounds complementing their respective functions
    • A61K2800/5922At least two compounds being classified in the same subclass of A61K8/18
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/30Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change

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Abstract

The invention discloses a preparation method of a whitening composition for improving the solubility of active components, a product and application thereof, wherein azelaic acid, ferulic acid, dipropylene glycol and glycerol are mixed and heated to obtain a composition 1; mixing and heating glyceryl acetate, hesperidin and aescin to obtain composition 2; slowly adding the composition 1 into the composition 2, and stirring while adding to obtain a composition 3; mixing and heating water, mannosylerythritol lipids, dipalmitoylphosphatidylcholine and lecithin, and homogenizing until the lecithin is completely dissolved to obtain a composition 4; adding the composition 3 into the composition 4, and homogenizing and stirring until complete emulsification; and (3) adding the product obtained in the step (5) into a high-pressure homogenizer, and refluxing under high pressure.

Description

Preparation method of whitening composition for improving solubility of active components, product and application thereof
Technical Field
The invention belongs to the technical field of cosmetics, and particularly relates to a preparation method of a whitening composition for improving the solubility of an active component, a product and application thereof.
Background
At present, whitening raw materials and whitening cosmetics on the market are more and more, many consumers have symptoms of unobvious effect or sensitive skin and the like after using whitening products, and safe and effective whitening still is a problem to be solved urgently.
Ferulic acid is derived from Chinese herbal medicines such as angelica sinensis and the like, is a very safe and effective whitening component, can inhibit the activity of melanocyte B16V and tyrosinase, and has the effects of scavenging oxygen free radicals and good antioxidation. Besides, ferulic acid also has the function of absorbing ultraviolet rays and preventing sunburn. Azelaic acid can competitively inhibit the activity of tyrosinase, and has the effects of directly inhibiting and accelerating keratinocyte metabolism for melanocyte with hyperfunction of structural disorder or proliferation, thereby improving skin pigmentation. Hesperidin can regulate the phosphorylation levels of PI3K and Akt down, and can influence the expression of the most important transcription factor MITF in the melanin synthesis process and finally influence the melanin synthesis. Aescin has good anti-inflammatory effect, and can prevent melanin deposition caused by inflammation, and relieve irritation and erythema caused by whitening agent.
However, although the natural sources of ferulic acid, azelaic acid, hesperidin and aescin have good efficacy, the natural sources are not soluble in water and oil, the use is limited, the emulsion is broken due to precipitation even if the natural sources are made into cream, the product is extremely unstable, and the ferulic acid is easy to oxidize to influence the effect of the ferulic acid.
Disclosure of Invention
This section is for the purpose of summarizing some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. In this section, as well as in the abstract and the title of the invention of this application, simplifications or omissions may be made to avoid obscuring the purpose of the section, the abstract and the title, and such simplifications or omissions are not intended to limit the scope of the invention.
As one aspect of the present invention, the present invention provides a method for preparing a whitening composition for improving the solubility of an active ingredient, which comprises the steps of,
step 1: mixing azelaic acid, ferulic acid, dipropylene glycol and glycerol and heating to provide composition 1;
step 2: mixing and heating glyceryl acetate, hesperidin and aescin to obtain composition 2;
and step 3: slowly adding the composition 1 into the composition 2, and stirring while adding to obtain a composition 3;
and 4, step 4: mixing and heating water, mannosylerythritol lipids, dipalmitoylphosphatidylcholine and lecithin, and homogenizing until the lecithin is completely dissolved to obtain a composition 4;
and 5: adding the composition 3 into the composition 4, and homogenizing and stirring until complete emulsification;
step 6: adding the product obtained in the step (5) into a high-pressure homogenizer, and performing high-pressure reflux for 8-9 times under the pressure of 800-900 bar to obtain the whitening nano emulsion;
the feed additive comprises, by mass, 5-32 parts of azelaic acid, 1-14 parts of ferulic acid, 0.5-5 parts of hesperidin, 1-2 parts of aescin, 1-5 parts of dipalmitoyl phosphatidylcholine, 1-4 parts of soybean lecithin, 0.1-1 part of mannosylerythritol ester, 4-6 parts of glycerol acetate, 5-12 parts of glycerol, 1-7 parts of dipropylene glycol and the balance of water to 100 parts.
As a preferred embodiment of the method for preparing the whitening composition for improving the solubility of the active ingredient according to the present invention: in the step 1, heating is carried out until the temperature is 60-70 ℃.
As a preferred embodiment of the method for preparing the whitening composition for improving the solubility of the active ingredient according to the present invention: in the step 2, heating is carried out until the temperature is 60-70 ℃.
As a preferred embodiment of the method for preparing the whitening composition for improving the solubility of the active ingredient according to the present invention: in the step 5, heating is carried out until the temperature is 60 ℃.
As a preferred embodiment of the method for preparing the whitening composition for improving the solubility of the active ingredient according to the present invention: in step 6, the pressure is 850 bar.
As a preferred embodiment of the method for preparing the whitening composition for improving the solubility of the active ingredient according to the present invention: in step 5, the homogenizing time is 3-5 min, and the rotating speed is 10000-15000 r/s.
As a preferred embodiment of the method for preparing the whitening composition for improving the solubility of the active ingredient according to the present invention: the lecithin is soybean lecithin, and the phosphatidylcholine content of the lecithin is 40%.
As a preferred embodiment of the method for preparing the whitening composition for improving the solubility of the active ingredient according to the present invention: the feed additive comprises, by mass, 27-30 parts of azelaic acid, 13-14 parts of ferulic acid, 3-5 parts of hesperidin, 1-2 parts of aescin, 4-5 parts of dipalmitoylphosphatidylcholine, 2-3 parts of lecithin, 0.5-1 part of mannosylerythritol ester, 4-5 parts of glycerol acetate, 10-12 parts of glycerol, 6-7 parts of dipropylene glycol and the balance of water to 100 parts.
As another aspect of the invention, the invention provides an application of the whitening composition in preparing whitening masks, essences, emulsions and creams.
The invention has the beneficial effects that: according to the invention, a nano-emulsification technology is adopted, a proper solvent, an emulsifier and the like are searched for to completely dissolve functional raw materials, and the nano-emulsion with uniform particle size is prepared, so that the nano-emulsion can be added into an aqueous product and an emulsified body, and meanwhile, the slow release permeation of the nano-emulsion in skin is increased by adopting hydrogenated phosphatidylcholine, lecithin (PC40) and mannitol erythritol lipid obtained by biological fermentation, and the effects of mildness, safety and high efficiency whitening are achieved. The compound of the dipalmitoyl phosphatidylcholine and the soybean lecithin (PC40) emulsifier not only improves the emulsification effect, but also can assist in solubilizing azelaic acid, ferulic acid and hesperidin, so that the emulsion is stable and does not break emulsion while the solubility of the azelaic acid, the ferulic acid and the hesperidin is improved.
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In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without inventive exercise. Wherein:
FIG. 1 is a graph showing the particle size distribution of the product of example 1.
Fig. 2 is a transdermal fluorescence image of the whitening nanoemulsion of the control group and the embodiment 1 of the invention.
FIG. 3 is a graph of MI values tested in example 1.
FIG. 4 is the melanin reduction rate over 3 weeks tested in example 1.
FIG. 5 is the ITA ° test value within 21 days of the test of example 1.
FIG. 6 is the gloss enhancement rate over 3 weeks tested in example 1.
Fig. 7 is a skin penetration test chart of the whitening combination emulsion of the control example 1.
Fig. 8 is MI values measured within 21 days of the whitening combination emulsion of comparative example 1.
Fig. 9 is a melanin reduction rate of the whitening combination emulsion of comparative example 1 for 3 weeks.
Fig. 10 is an ITA ° measured within 21 days of the whitening combination emulsion of comparative example 1.
Fig. 11 is a graph showing the brightness improvement rate of the whitening combination emulsion of comparative example 1 in 3 weeks.
FIG. 12 is a graph showing the particle size distribution of the product of comparative example 1.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with examples are described in detail below.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described and will be readily apparent to those of ordinary skill in the art without departing from the spirit of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.
Furthermore, the references herein to "one embodiment" or "an embodiment" refer to a particular feature, structure, or characteristic that may be included in at least one implementation of the present invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
The whitening nano-emulsion disclosed by the invention comprises the following raw materials in parts by weight: 5-30 parts of azelaic acid, 1-14 parts of ferulic acid, 0.5-5 parts of hesperidin, 1-2 parts of aescin, 1-5 parts of dipalmitoylphosphatidylcholine, 1-4 parts of soybean lecithin (PC40), 0.1-1 part of mannosylerythritol ester, 4-6 parts of glycerol acetate, 5-12 parts of glycerol and dipropylene glycol (C) 6 H 14 O 3 )1-7 parts of water to 100 parts.
The preparation method of the whitening composition comprises the following steps:
1. mixing azelaic acid, ferulic acid, dipropylene glycol and glycerol, and heating to 60-70 deg.C for complete dissolution to obtain composition 1;
2. mixing glyceryl acetate, hesperidin and aescin, and heating to 60-70 deg.C for completely dissolving to obtain composition 2;
3. slowly adding composition 1 into composition 2 at 60-70 deg.C under stirring to obtain composition 3;
4. mixing water, mannosylerythritol lipid, dipalmitoylphosphatidylcholine and lecithin, heating to 60 deg.C, and homogenizing until lecithin is completely dissolved to obtain composition 4;
5. adding the composition 3 into the composition 4, homogenizing at 10000-15000 r/s for 3-5 minutes until complete emulsification;
6. and adding the emulsified emulsion into a high-pressure homogenizer, and performing high-pressure reflux for 8-9 times under the pressure of 850bar to obtain the whitening nano emulsion.
Example 1:
the whitening nano-emulsion disclosed by the invention comprises the following raw materials in parts by weight: 31 parts of azelaic acid, 14 parts of ferulic acid, 5 parts of hesperidin, 2 parts of aescin, 5 parts of dipalmitoyl phosphatidylcholine, 3 parts of lecithin (PC40), 1 part of mannosylerythritol ester, 5 parts of glycerol acetate, 12 parts of glycerol, and dipropylene glycol (C) 6 H 14 O 3 )7 parts of water to 100 parts.
1. Mixing azelaic acid, ferulic acid, dipropylene glycol and glycerol, and heating to 65 deg.C for complete dissolution to obtain composition 1;
2. mixing glyceryl acetate, hesperidin and aescin, and heating to 65 deg.C to completely dissolve to obtain composition 2;
3. slowly adding composition 1 to composition 2 while maintaining at 65 deg.C, and stirring to obtain composition 3;
4. mixing water, mannosylerythritol lipids, dipalmitoylphosphatidylcholine and lecithin, heating to 60 deg.C, and homogenizing until the lecithin is completely dissolved to obtain composition 4;
5. adding the composition 3 into the composition 4, and homogenizing and stirring for 4 minutes until complete emulsification;
6. and adding the emulsified emulsion into a high-pressure homogenizer, and performing high-pressure reflux for 8 times under the pressure of 850bar to obtain the whitening nano emulsion.
The experimental results are as follows: the obtained nano-emulsion is transparent viscous liquid, and the particle size of the nano-emulsion is measured by adopting a Zeta potential and nano-particle size analyzer; and placing the mixture in a high-low temperature circulating (-15 ℃ -48 ℃) thermostat to determine the high-low temperature stability of the mixture. Fig. 1 is a particle size distribution diagram measured by a Zeta potential and nano-particle size analyzer, and it can be seen that the nanoemulsion has a more concentrated particle size distribution and a better dispersity. From the figure, it can be seen that the average particle size of the nanoemulsion ranges from 40 to 50 nm.
The stability test results are as follows: the cycle did not change significantly one month.
Transdermal experiment: the skin penetration depth of the whitening nanoemulsion added with a fat-soluble fluorescent agent, namely nile red (the mass fraction of 0.0001 percent) is observed by adopting a fluorescence microscope. The two samples were cut into strips after transdermal penetration and coated with SAKURA cryo-embedding medium. And after freezing for 24 hours, placing the pigskin on a freezing microtome for slicing, wherein the thickness is controlled to be 20-40 mu m. Setting the fluorescence type to the excitation wavelength: 488nm, emission wavelength: 571-741 nm, and observing the transdermal effect of the whitening nanoemulsion under the fluorescent condition. Fig. 2 is a transdermal fluorescence image of a control group and the whitening nanoemulsion of the invention. Fig. 2 shows that a-1 is a transdermal experimental white light channel diagram of a control group whitening emulsion, a-2 is a transdermal experimental fluorescence diagram of the control group whitening emulsion, b-1 is a transdermal experimental white light channel diagram of the whitening nanoemulsion of the present invention, and b-2 is a transdermal experimental fluorescence diagram of the whitening nanoemulsion of the present invention, so that the whitening nanoemulsion of the present invention has good transdermal properties. Spot-pasting experiment: the spot test method comprises the following steps: selecting qualified spot test equipment, placing 0.020-0.025 mL (0.020-0.025 g) of a test object in a spot tester by a closed spot test method, externally applying a hypoallergenic adhesive tape to the curved side of the forearm of the test object, removing the test object after 24 hours, removing the spot tester of the test object for 30min, and observing skin reaction after the indentation disappears. If the result is negative, the test is observed once more at 24h and 48h after the patch test. The results were recorded according to the skin adverse reaction grading criteria (table below).
TABLE 1 skin closed Patch test skin response grading Standard
Figure BDA0003570533080000051
Figure BDA0003570533080000061
Through detection, 30 people do not have adverse skin reactions in 30 closed skin patch tests, which are detailed in table 2.
TABLE 2 cosmetic body Patch test results
Figure BDA0003570533080000062
Evaluation experiment of human whitening efficacy: the skin melanin content (MI value) was measured using the german CK skin tester Mexameter MX18 probe, and higher measured values indicate higher melanin content in the skin. Skin brightness (dark yellowness) was measured with a Colormeter probe (ITA ° value), the ITA ° value being the individual type angle of the skin, the greater the ITA ° value, the brighter the skin, and vice versa the darker the skin. After the test subject cleans the face every day, the whitening nano-emulsion is added at 1.25 mu L/cm 2 The test part was coated with uniform coating density 1 time each day in the morning and evening for 21 days. FIG. 3 shows MI values measured in 21 days, and FIG. 4 shows melanin reduction rate in 3 weeks. As can be seen from the figure, the whitening nanoemulsion can well reduce the melanin content of the skin and improve the brightness. Fig. 5 is the ITA ° test value in 21 days, and fig. 6 is the gloss improvement rate in 3 weeks.
The combination of the glycerol and the dipropylene glycol ensures that the oil-water distribution coefficient is just proper, and the emulsion is stable and does not break. Meanwhile, the two emulsifiers, namely dipalmitoyl phosphatidylcholine and soybean lecithin, are compounded, so that the emulsifying effect is improved, and the solubilization of azelaic acid, ferulic acid and hesperidin can be assisted, so that the emulsion is stable and does not break emulsion while the solubility of azelaic acid, ferulic acid and hesperidin is improved. The invention adopts the soybean lecithin with 40 wt% of phosphatidylcholine content to be compounded with dipalmitoyl phosphatidylcholine, probably because the mixture of phosphoric acid, choline, fatty acid, glycolipid, triglyceride and the like in the soybean lecithin can promote the dissolution of azelaic acid and ferulic acid after being compounded with other components, and the compounding of the two emulsifiers improves the stability of the emulsion.
Comparative example 1:
the whitening nano-emulsion disclosed by the invention comprises the following raw materials in parts by weight: 31 parts of azelaic acid, 14 parts of ferulic acid, 5 parts of hesperidin, 2 parts of aescin, 5 parts of dipalmitoyl phosphatidylcholine, 3 parts of lecithin (PC40), 1 part of mannosylerythritol ester, 5 parts of glycerol acetate, 12 parts of glycerol, and dipropylene glycol (C) 6 H 14 O 3 )7 parts of water to 100 parts.
The preparation method comprises the following steps:
1. mixing azelaic acid, ferulic acid, dipropylene glycol and glycerol, and heating to 65 deg.C for complete dissolution to obtain composition 1;
2. mixing glyceryl acetate, hesperidin and aescin, and heating to 65 deg.C for completely dissolving to obtain composition 2;
3. slowly adding composition 1 to composition 2 while maintaining at 65 deg.C, and stirring to obtain composition 3;
4. mixing water, mannosylerythritol lipids, dipalmitoylphosphatidylcholine and lecithin, heating to 60 deg.C, and homogenizing until the lecithin is completely dissolved to obtain composition 4;
5. adding the composition 3 into the composition 4, homogenizing and stirring for 3-5 minutes until complete emulsification;
6. and adding the emulsified emulsion into a high-pressure homogenizer, and performing high-pressure reflux for 3 times under the pressure of 400bar to obtain the whitening nano emulsion.
The experimental results are as follows: the appearance is opaque emulsion, the particle size is about 100-120nm, and the graph is shown in figure 12.
The stability test results are as follows: the sample is placed in a high-low temperature constant temperature box for circulation experiment, and no obvious change is caused within 1 month.
Fig. 7 is a graph of a transdermal experiment of the whitening combined emulsion of the embodiment, c-1 is a graph of a transdermal experiment white light channel of the whitening nanoemulsion of the embodiment, and c-2 is a graph of a transdermal experiment fluorescence of the whitening nanoemulsion of the embodiment. Fig. 8 shows MI values measured within 21 days of the whitening combination emulsion. Fig. 9 is the melanin reduction rate of the whitening combination emulsion for 3 weeks. Fig. 10 is the ITA ° measured over 21 days for the whitening combination emulsion. Fig. 11 shows the brightness improvement rate of the whitening combination emulsion within 3 weeks.
The factors that cause emulsion instability are mainly the following: layering, flocculation, phase inversion, polymerization, and austenite ripening. The austenite curing means that small particles in a system gradually become smaller and are attached to large particles, and finally the phenomenon that the small particles are smaller and the large particles are larger is caused, and the pressure and the reflux frequency for preparing the nano emulsion influence the particle size distribution, the transdermal effect and the whitening effect of a product. The nano emulsion prepared by the method has larger and uneven grain diameter and can cause austenite curing because the force for breaking the emulsion is smaller with smaller pressure and reflux times; the excessive reflux times caused by excessive pressure can cause re-agglomeration of the nano emulsion after excessive scattering; the large particle size causes the active substance not to easily permeate into the skin, thereby affecting the whitening effect, so that it is very important to obtain a stable product having excellent skin penetration and whitening effects by optimizing a proper pressure and adjusting an optimal number of times of reflux.
Comparative example 2:
31 parts of azelaic acid, 14 parts of ferulic acid, 5 parts of hesperidin, 2 parts of aescin, 5 parts of dipalmitoyl phosphatidylcholine, 3 parts of lecithin (PC40), 1 part of mannosylerythritol ester, 5 parts of glycerol acetate, 12 parts of butanediol and propylene glycol (C) 3 H 8 O 2 )7 parts of water to 100 parts.
The preparation method is the same as that of example 1.
The experimental results are as follows: it was found that if glycerin and dipropylene glycol were replaced with butylene glycol and propylene glycol (C) 3 H 8 O 2 ) Can cause that azelaic acid and ferulic acid can not be completely dissolved, crystal is separated out after cooling, and emulsion is broken by emulsion.
The solubility of azelaic acid and ferulic acid is between that of water and oil, and it is difficult to find suitable solvents, which are neither soluble in oil nor soluble in water, and glycerin or propylene glycol alone, although high temperature can dissolve it, will precipitate out of the system when the temperature is reduced to room temperature, and the product will eventually be unstable. While it is more difficult to dissolve azelaic acid and ferulic acid simultaneously and to find a solvent that is compatible with them simultaneously, this technical problem is not solved in the prior art.
Comparative example 3:
31 parts of azelaic acid, 14 parts of ferulic acid, 5 parts of hesperidin, 2 parts of aescin, 805 parts of tween, 3 parts of caprylic/capric triglyceride, 1 part of mannosylerythritol ester, 5 parts of glycerol acetate, 12 parts of glycerol and dipropylene glycol (C) 6 H 14 O 3 )7 parts of water to 100 parts.
The preparation method is the same as that of example 1.
The experimental results are as follows: the emulsion is demulsified after being cooled, the emulsification effect is not good, and the experimental requirements can not be met.
Comparative example 4:
the combination of the whitening nano-emulsion of the invention is nonane II31 parts of acid, 14 parts of ferulic acid, 5 parts of hesperidin, 2 parts of aescin, 8 parts of dipalmitoyl phosphatidylcholine, 1 part of mannosylerythritol, 5 parts of glycerol acetate, 12 parts of glycerol and dipropylene glycol (C) 6 H 14 O 3 )7 parts of water to 100 parts.
The preparation method is the same as that of example 1.
The experimental results are as follows: more precipitate is separated out after the emulsion is cooled. The compound of the dipalmitoyl phosphatidylcholine and the soybean lecithin (PC40) emulsifier not only improves the emulsification effect, but also can assist in solubilizing azelaic acid, ferulic acid and hesperidin, so that the emulsion is stable and does not break emulsion while the solubility of the azelaic acid, the ferulic acid and the hesperidin is improved. And the effect is poor when dipalmitoyl phosphatidylcholine is used alone, the solubility of azelaic acid, ferulic acid and hesperidin is obviously reduced, and the requirements of emulsification and solubilization can not be met.
Comparative example 5:
the whitening nano-emulsion disclosed by the invention comprises the following raw materials in parts by weight: 31 parts of azelaic acid, 14 parts of ferulic acid, 5 parts of hesperidin, 2 parts of aescin, 5 parts of dipalmitoyl phosphatidylcholine, 3 parts of lecithin (PC80), 1 part of mannosylerythritol ester, 5 parts of glycerol acetate, 12 parts of glycerol, and dipropylene glycol (C) 6 H 14 O 3 )7 parts of water to 100 parts.
The preparation method is the same as that of example 1.
The experimental results are as follows: the emulsion is cooled and precipitates. The invention discovers that the poor solubility of azelaic acid and ferulic acid, the precipitation of the emulsion and the instability of the emulsion are caused after the soybean lecithin with 80 wt% of phosphatidylcholine content and dipalmitoyl phosphatidylcholine are compounded.
In summary, the invention adopts the nano-emulsification technology, finds the proper solvent, emulsifier and the like to completely dissolve the functional raw materials and prepare the nano-emulsion with uniform particle size, can simultaneously dissolve 32% azelaic acid, 14% ferulic acid, 5% hesperidin and 2% aescin, ensures that the emulsion is very stable and does not break emulsion, has no precipitation and is directly mixed and dissolved, does not need to introduce ethanol and blow-dry and other complicated steps in the dissolving process, the solvent and the emulsifier are the functional components for whitening and moisturizing, and can be used as the solvent to dissolve the active components of azelaic acid, ferulic acid and the like while realizing emulsification and moisturizing, thereby simplifying the process and being safer, the composition of the invention can be added into water aqua products or emulsified bodies, and simultaneously adopts hydrogenated phosphatidylcholine, soybean lecithin (PC40) and mannose erythritol ester obtained by biological fermentation to increase the slow-release permeation of the composition in skin, the effects of mildness, safety and high-efficiency whitening are achieved.
It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.

Claims (9)

1. A preparation method of a whitening composition for improving the solubility of an active component is characterized by comprising the following steps: the method comprises the following steps of (1),
step 1: mixing azelaic acid, ferulic acid, dipropylene glycol and glycerol and heating to obtain composition 1;
step 2: mixing and heating glyceryl acetate, hesperidin and aescin to obtain composition 2;
and step 3: slowly adding the composition 1 into the composition 2, and stirring while adding to obtain a composition 3;
and 4, step 4: mixing and heating water, mannosylerythritol lipids, dipalmitoylphosphatidylcholine and lecithin, and homogenizing until the lecithin is completely dissolved to obtain a composition 4;
and 5: adding the composition 3 into the composition 4, and homogenizing and stirring until complete emulsification;
step 6: adding the product obtained in the step (5) into a high-pressure homogenizer, and performing high-pressure reflux for 8-9 times under the pressure of 800-900 bar to obtain the whitening nano emulsion;
the feed additive comprises, by mass, 5-32 parts of azelaic acid, 1-14 parts of ferulic acid, 0.5-5 parts of hesperidin, 1-2 parts of aescin, 1-5 parts of dipalmitoyl phosphatidylcholine, 1-4 parts of soybean lecithin, 0.1-1 part of mannosylerythritol ester, 4-6 parts of glycerol acetate, 5-12 parts of glycerol, 1-7 parts of dipropylene glycol and the balance of water to 100 parts.
2. The method for preparing a whitening composition according to claim 1, characterized in that: in the step 1, heating is carried out until the temperature is 60-70 ℃.
3. The method for preparing a whitening composition for improving the solubility of active ingredients according to claim 1 or 2, characterized in that: in the step 2, heating is carried out until the temperature is 60-70 ℃.
4. The method for preparing a whitening composition for improving the solubility of active ingredients according to claim 1 or 2, characterized in that: in the step 5, heating is carried out until the temperature is 60 ℃.
5. The method for preparing a whitening composition for improving the solubility of active ingredients according to claim 1 or 2, characterized in that: in step 6, the pressure is 850 bar.
6. The method for preparing a whitening composition for improving the solubility of active ingredients according to claim 1 or 2, characterized in that: in step 5, the homogenizing time is 3-5 min, and the rotating speed is 10000-15000 r/s.
7. The method for preparing a whitening composition for improving the solubility of active ingredients according to claim 1 or 2, characterized in that: the lecithin is soybean lecithin, and the phosphatidylcholine content of the lecithin is 40%.
8. The method for preparing a whitening composition for improving the solubility of active ingredients according to claim 1 or 2, characterized in that: the feed additive comprises, by mass, 27-30 parts of azelaic acid, 13-14 parts of ferulic acid, 3-5 parts of hesperidin, 1-2 parts of aescin, 4-5 parts of dipalmitoylphosphatidylcholine, 2-3 parts of lecithin, 0.5-1 part of mannosylerythritol ester, 4-5 parts of glycerol acetate, 10-12 parts of glycerol, 6-7 parts of dipropylene glycol and the balance of water to 100 parts.
9. Use of the whitening composition of claim 1 in the preparation of whitening masks, essences, lotions and creams.
CN202210322071.8A 2022-03-29 2022-03-29 Preparation method of whitening composition, product and application thereof Active CN114869795B (en)

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