CN114869795B - Preparation method of whitening composition, product and application thereof - Google Patents
Preparation method of whitening composition, product and application thereof Download PDFInfo
- Publication number
- CN114869795B CN114869795B CN202210322071.8A CN202210322071A CN114869795B CN 114869795 B CN114869795 B CN 114869795B CN 202210322071 A CN202210322071 A CN 202210322071A CN 114869795 B CN114869795 B CN 114869795B
- Authority
- CN
- China
- Prior art keywords
- composition
- parts
- whitening
- portions
- lecithin
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000000203 mixture Substances 0.000 title claims abstract description 81
- 230000002087 whitening effect Effects 0.000 title claims abstract description 68
- 238000002360 preparation method Methods 0.000 title abstract description 17
- BDJRBEYXGGNYIS-UHFFFAOYSA-N nonanedioic acid Chemical compound OC(=O)CCCCCCCC(O)=O BDJRBEYXGGNYIS-UHFFFAOYSA-N 0.000 claims abstract description 66
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 52
- KSEBMYQBYZTDHS-HWKANZROSA-M (E)-Ferulic acid Natural products COC1=CC(\C=C\C([O-])=O)=CC=C1O KSEBMYQBYZTDHS-HWKANZROSA-M 0.000 claims abstract description 34
- KSEBMYQBYZTDHS-HWKANZROSA-N ferulic acid Chemical compound COC1=CC(\C=C\C(O)=O)=CC=C1O KSEBMYQBYZTDHS-HWKANZROSA-N 0.000 claims abstract description 34
- 229940114124 ferulic acid Drugs 0.000 claims abstract description 34
- KSEBMYQBYZTDHS-UHFFFAOYSA-N ferulic acid Natural products COC1=CC(C=CC(O)=O)=CC=C1O KSEBMYQBYZTDHS-UHFFFAOYSA-N 0.000 claims abstract description 34
- 235000001785 ferulic acid Nutrition 0.000 claims abstract description 34
- QURCVMIEKCOAJU-UHFFFAOYSA-N trans-isoferulic acid Natural products COC1=CC=C(C=CC(O)=O)C=C1O QURCVMIEKCOAJU-UHFFFAOYSA-N 0.000 claims abstract description 34
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- QUQPHWDTPGMPEX-UHFFFAOYSA-N Hesperidine Natural products C1=C(O)C(OC)=CC=C1C1OC2=CC(OC3C(C(O)C(O)C(COC4C(C(O)C(O)C(C)O4)O)O3)O)=CC(O)=C2C(=O)C1 QUQPHWDTPGMPEX-UHFFFAOYSA-N 0.000 claims abstract description 27
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- VUYDGVRIQRPHFX-UHFFFAOYSA-N hesperidin Natural products COc1cc(ccc1O)C2CC(=O)c3c(O)cc(OC4OC(COC5OC(O)C(O)C(O)C5O)C(O)C(O)C4O)cc3O2 VUYDGVRIQRPHFX-UHFFFAOYSA-N 0.000 claims abstract description 27
- QUQPHWDTPGMPEX-QJBIFVCTSA-N hesperidin Chemical compound C1=C(O)C(OC)=CC=C1[C@H]1OC2=CC(O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@@H](CO[C@H]4[C@@H]([C@H](O)[C@@H](O)[C@H](C)O4)O)O3)O)=CC(O)=C2C(=O)C1 QUQPHWDTPGMPEX-QJBIFVCTSA-N 0.000 claims abstract description 27
- 229940025878 hesperidin Drugs 0.000 claims abstract description 27
- ARGKVCXINMKCAZ-UHFFFAOYSA-N neohesperidine Natural products C1=C(O)C(OC)=CC=C1C1OC2=CC(OC3C(C(O)C(O)C(CO)O3)OC3C(C(O)C(O)C(C)O3)O)=CC(O)=C2C(=O)C1 ARGKVCXINMKCAZ-UHFFFAOYSA-N 0.000 claims abstract description 27
- KMZHZAAOEWVPSE-UHFFFAOYSA-N 2,3-dihydroxypropyl acetate Chemical compound CC(=O)OCC(O)CO KMZHZAAOEWVPSE-UHFFFAOYSA-N 0.000 claims abstract description 25
- IIZPXYDJLKNOIY-JXPKJXOSSA-N 1-palmitoyl-2-arachidonoyl-sn-glycero-3-phosphocholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCC\C=C/C\C=C/C\C=C/C\C=C/CCCCC IIZPXYDJLKNOIY-JXPKJXOSSA-N 0.000 claims abstract description 24
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- KILNVBDSWZSGLL-KXQOOQHDSA-N 1,2-dihexadecanoyl-sn-glycero-3-phosphocholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCCCCCCCCCCCCCC KILNVBDSWZSGLL-KXQOOQHDSA-N 0.000 claims abstract description 22
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- SZXQTJUDPRGNJN-UHFFFAOYSA-N dipropylene glycol Chemical compound OCCCOCCCO SZXQTJUDPRGNJN-UHFFFAOYSA-N 0.000 claims abstract description 18
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- XHCADAYNFIFUHF-TVKJYDDYSA-N esculin Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC(C(=C1)O)=CC2=C1OC(=O)C=C2 XHCADAYNFIFUHF-TVKJYDDYSA-N 0.000 claims abstract description 14
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- JLPULHDHAOZNQI-ZTIMHPMXSA-N 1-hexadecanoyl-2-(9Z,12Z-octadecadienoyl)-sn-glycero-3-phosphocholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCCCCCC\C=C/C\C=C/CCCCC JLPULHDHAOZNQI-ZTIMHPMXSA-N 0.000 claims description 11
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- 239000004480 active ingredient Substances 0.000 claims description 7
- WTJKGGKOPKCXLL-RRHRGVEJSA-N phosphatidylcholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCCCCCCC=CCCCCCCCC WTJKGGKOPKCXLL-RRHRGVEJSA-N 0.000 claims description 4
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- 238000004945 emulsification Methods 0.000 abstract description 3
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- XUMBMVFBXHLACL-UHFFFAOYSA-N Melanin Chemical compound O=C1C(=O)C(C2=CNC3=C(C(C(=O)C4=C32)=O)C)=C2C4=CNC2=C1C XUMBMVFBXHLACL-UHFFFAOYSA-N 0.000 description 10
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- 206010067484 Adverse reaction Diseases 0.000 description 2
- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 description 2
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- 230000008859 change Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- UNXHWFMMPAWVPI-ZXZARUISSA-N erythritol Chemical compound OC[C@H](O)[C@H](O)CO UNXHWFMMPAWVPI-ZXZARUISSA-N 0.000 description 2
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- UFTFJSFQGQCHQW-UHFFFAOYSA-N triformin Chemical compound O=COCC(OC=O)COC=O UFTFJSFQGQCHQW-UHFFFAOYSA-N 0.000 description 1
Classifications
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/36—Carboxylic acids; Salts or anhydrides thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/34—Alcohols
- A61K8/345—Alcohols containing more than one hydroxy group
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- A—HUMAN NECESSITIES
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- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/36—Carboxylic acids; Salts or anhydrides thereof
- A61K8/362—Polycarboxylic acids
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/37—Esters of carboxylic acids
- A61K8/375—Esters of carboxylic acids the alcohol moiety containing more than one hydroxy group
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- A—HUMAN NECESSITIES
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- A61Q19/02—Preparations for care of the skin for chemically bleaching or whitening the skin
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- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Landscapes
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- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Veterinary Medicine (AREA)
- Public Health (AREA)
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- Emergency Medicine (AREA)
- Dermatology (AREA)
- Biophysics (AREA)
- Molecular Biology (AREA)
- Cosmetics (AREA)
- Medicinal Preparation (AREA)
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 glycerin are mixed and heated to obtain a composition 1; mixing glycerol acetate, hesperidin and aesculin, and heating to obtain composition 2; slowly adding the composition 1 into the composition 2, and stirring while adding to obtain a composition 3; mixing water, mannose erythritol lipid, dipalmitoyl phosphatidylcholine and lecithin, heating, homogenizing until lecithin is completely dissolved to obtain composition 4; adding the composition 3 into the composition 4, and uniformly stirring until the mixture is completely emulsified; the product obtained in the step 5 is added into a high-pressure homogenizer for high-pressure reflux, the nano-emulsification technology is adopted, and proper solvents, emulsifying agents and the like are searched for to completely dissolve functional raw materials, and nano-emulsion with uniform particle size is prepared, so that the nano-emulsion can be added into water aqua products or emulsifying bodies.
Description
Technical Field
The invention belongs to the technical field of cosmetics, and particularly relates to a preparation method of a whitening composition for improving solubility of active components, a product and application thereof.
Background
At present, more and more whitening raw materials and whitening cosmetics in the market are available, and a safe and effective whitening problem is still a problem to be solved after a plurality of consumers use the whitening products and have symptoms such as unobvious effect or skin sensitivity.
The ferulic acid is derived from Chinese herbal medicines such as angelica, 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 resisting oxidation. In addition, ferulic acid has the effect of absorbing ultraviolet rays and preventing sunburn. Azelaic acid can competitively inhibit tyrosinase activity, and has effects of directly inhibiting and accelerating cutin metabolism of structurally disordered and hyperplastic melanocytes, thereby improving skin pigmentation. Hesperidin can down regulate the phosphorylation level of PI3K and Akt, and can influence the expression of the most important transcription factor MITF in the melanin synthesis process, and finally influence the melanin synthesis. The aesculin has good anti-inflammatory effect, and can prevent melanin deposition caused by inflammation, and relieve irritation and erythema caused by whitening agent.
However, although these natural sources of ferulic acid, azelaic acid, hesperidin and aesculin are effective, they are not soluble in water nor oil, and are limited in use, and even if they are in the form of cream, they are precipitated to break emulsion, which results in extremely unstable products, and ferulic acid is easily oxidized to affect its own functions.
Disclosure of Invention
This section is intended to outline some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. Some simplifications or omissions may be made in this section as well as in the description summary and in the title of the application, to avoid obscuring the purpose of this section, the description summary and the title of the invention, which should not be used 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 obtain composition 1;
step 2: mixing glycerol acetate, hesperidin and aesculin, and heating to obtain composition 2;
step 3: slowly adding the composition 1 into the composition 2, and stirring while adding to obtain a composition 3;
step 4: mixing water, mannose erythritol lipid, dipalmitoyl phosphatidylcholine and lecithin, heating, homogenizing until lecithin is completely dissolved to obtain composition 4;
step 5: adding the composition 3 into the composition 4, and uniformly stirring until the mixture is completely emulsified;
step 6: adding the product obtained in the step 5 into a high-pressure homogenizer, and refluxing for 8-9 times under the pressure of 800-900 bar to obtain the whitening nano emulsion;
wherein, the weight portions of the raw materials are 5 to 32 portions of azelaic acid, 1 to 14 portions of ferulic acid, 0.5 to 5 portions of hesperidin, 1 to 2 portions of aesculin, 1 to 5 portions of dipalmitoyl phosphatidylcholine, 1 to 4 portions of soybean lecithin, 0.1 to 1 portion of mannitol erythritol ester, 4 to 6 portions of glycerol acetate, 5 to 12 portions of glycerol, 1 to 7 portions of dipropylene glycol and the balance of water to 100 portions.
As a preferred scheme of the preparation method of the whitening composition for improving the solubility of the active component, the invention is as follows: in the step 1, heating to 60-70 ℃.
As a preferred scheme of the preparation method of the whitening composition for improving the solubility of the active component, the invention is as follows: in the step 2, heating to 60-70 ℃.
As a preferred scheme of the preparation method of the whitening composition for improving the solubility of the active component, the invention is as follows: in the step 5, the temperature is heated to 60 ℃.
As a preferred scheme of the preparation method of the whitening composition for improving the solubility of the active component, the invention is as follows: in the step 6, the pressure is 850bar.
As a preferred scheme of the preparation method of the whitening composition for improving the solubility of the active component, the invention is as follows: in the step 5, the homogenizing time is 3-5 min, and the rotating speed is 10000-15000 r/s.
As a preferred scheme of the preparation method of the whitening composition for improving the solubility of the active component, the invention is as follows: the lecithin is soybean lecithin, and the phosphatidylcholine content of the lecithin is 40%.
As a preferred scheme of the preparation method of the whitening composition for improving the solubility of the active component, the invention is as follows: the weight portions of the raw materials are 27 to 30 portions of azelaic acid, 13 to 14 portions of ferulic acid, 3 to 5 portions of hesperidin, 1 to 2 portions of aesculin, 4 to 5 portions of dipalmitoyl phosphatidylcholine, 2 to 3 portions of lecithin, 0.5 to 1 portion of mannitol erythritol ester, 4 to 5 portions of glyceroacetate, 10 to 12 portions of glycerol, 6 to 7 portions of dipropylene glycol and the balance of water to 100 portions.
As another aspect of the invention, the invention provides application of the whitening composition in preparing whitening facial masks, essences, emulsions and creams.
The invention has the beneficial effects that: the invention adopts nanoemulsion technology to find out proper solvents, emulsifying agents and the like to completely dissolve functional raw materials and prepare nanoemulsion with uniform particle size, thus not only being capable of being added into water aqua products but also being added into an emulsifying body, and simultaneously adopting hydrogenated phosphatidylcholine, lecithin (PC 40) and mannitol erythritol fat obtained by biological fermentation to increase the slow release permeation of the mannitol erythritol fat in skin, thereby achieving the effects of mildness, safety and high efficiency and whitening. The combination of two emulsifying agents, namely dipalmitoyl phosphatidylcholine and soybean lecithin (PC 40), not only improves the emulsifying effect, but also assists in solubilizing azelaic acid, ferulic acid and hesperidin, so that the solubility of azelaic acid, ferulic acid and hesperidin is improved, and meanwhile, the emulsion is stable and does not break.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the description of the embodiments will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art. Wherein:
FIG. 1 is a graph showing the particle size distribution of the product of example 1.
Fig. 2 is a transdermal fluorescence map of the whitening nanoemulsion of the control group and example 1 of the present invention.
FIG. 3 shows MI values tested in example 1.
Fig. 4 is a graph showing melanin reduction rates within 3 weeks of the test of example 1.
Fig. 5 is the ITA ° test values over 21 days tested in example 1.
Fig. 6 is a graph of the gloss rise rate over 3 weeks for the test of example 1.
Fig. 7 is a transdermal experimental view of the whitening combination emulsion of comparative example 1.
Fig. 8 shows the MI values measured within 21 days of the whitening composition emulsion of comparative example 1.
Fig. 9 shows the melanin reduction rate of the whitening composition emulsion of comparative example 1 for 3 weeks.
Fig. 10 is the ITA ° measured within 21 days of the whitening combined emulsion of comparative example 1.
Fig. 11 is a luminance improvement rate within 3 weeks of the whitening composition emulsion of comparative example 1.
FIG. 12 is a graph showing the particle size distribution of the product of comparative example 1.
Detailed Description
In order that the above-recited objects, features and advantages of the present invention will become more apparent, a more particular description of the invention will be rendered by reference to specific embodiments thereof.
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 other than those described herein, and persons skilled in the art will readily appreciate that the present invention is not limited to the specific embodiments disclosed below.
Further, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic can be included in at least one implementation of the 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 nanoemulsion is prepared from the following raw materials in parts by mass: 5-30 parts of azelaic acid, 1-14 parts of ferulic acid, 0.5-5 parts of hesperidin, 1-2 parts of aesculin, 1-5 parts of dipalmitoyl phosphatidylcholine, 1-4 parts of soybean lecithin (PC 40), 0.1-1 part of mannitol erythritol ester, 4-6 parts of glyceroacetate, 5-12 parts of glycerol and dipropylene glycol (C) 6 H 14 O 3 ) 1-7 parts of water to 100 parts of water.
The preparation method of the whitening composition comprises the following steps:
1. mixing azelaic acid, ferulic acid, dipropylene glycol and glycerol, and heating to 60-70deg.C for complete dissolution to obtain composition 1;
2. mixing glycerol acetate, hesperidin and aesculin, and heating to 60-70deg.C for complete dissolution to obtain composition 2;
3. slowly adding composition 1 into composition 2 at 60-70deg.C under stirring to obtain composition 3;
4. mixing water, mannose erythritol lipid, dipalmitoyl phosphatidylcholine and lecithin, heating to 60deg.C, homogenizing until lecithin is completely dissolved to obtain composition 4;
5. adding the composition 3 into the composition 4, homogenizing for 3-5 minutes to completely emulsify at 10000-15000 r/s;
6. and (3) adding the emulsified emulsion into a high-pressure homogenizer, and refluxing for 8-9 times under the pressure of 850bar to obtain the whitening nano emulsion.
Example 1:
the whitening nanoemulsion is prepared from 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 horse chestnut saponin, 5 parts of dipalmitoyl phosphatidylcholine, 3 parts of lecithin (PC 40), 1 part of mannitol erythritol ester, 5 parts of glyceryl acetate, 12 parts of glycerin, and dipropylene glycol (C) 6 H 14 O 3 ) 7 parts of water to 100 parts of water.
1. Azelaic acid, ferulic acid, dipropylene glycol and glycerin are mixed and heated to 65 ℃ to be completely dissolved to obtain a composition 1;
2. mixing glycerol acetate, hesperidin and aesculin, and heating to 65deg.C for dissolving completely to obtain composition 2;
3. slowly adding composition 1 into composition 2 at 65deg.C under stirring to obtain composition 3;
4. mixing water, mannose erythritol lipid, dipalmitoyl phosphatidylcholine and lecithin, heating to 60 ℃, and homogenizing until the lecithin is completely dissolved to obtain a composition 4;
5. adding the composition 3 into the composition 4, and uniformly stirring for 4 minutes to completely emulsify;
6. and (3) adding the emulsified emulsion into a high-pressure homogenizer, and refluxing for 8 times under the pressure of 850bar to obtain the whitening nano emulsion.
Experimental results: the obtained nanoemulsion is transparent viscous liquid, and the particle size is measured by using a Zeta potential and nano particle size analyzer; the high and low temperature stability is measured in a constant temperature box with high and low temperature circulation (-15 ℃ to 48 ℃). Fig. 1 shows the Zeta potential and the particle size distribution diagram measured by the 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 mean particle size of the nanoemulsion is between 40 and 50nm.
Stability test results: there was no significant change in circulation for one month.
Transdermal experiments: the depth of penetration of the whitening nanoemulsion with the addition of the liposoluble fluorescent agent nile red (mass fraction 0.0001%) was observed by using a fluorescence microscope. The pig skin after transdermal of both samples was cut into strips and wrapped with SAKURA frozen embedding medium. Freezing for 24h, and slicing the pigskin on a frozen slicer, wherein the thickness is controlled to be 20-40 mu m. The fluorescence type is set 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 present invention. A-1 of fig. 2 is a transdermal experimental white light channel diagram of the whitening emulsion of the control group, a-2 is a transdermal experimental fluorescent diagram of the whitening emulsion of the control group, 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 fluorescent diagram of the whitening nanoemulsion of the present invention, which shows that the whitening nanoemulsion of the present invention has good transdermal properties. Spot-mapping experiments: plaque test method: selecting qualified spot test equipment, placing 0.020-0.025 mL (0.020-0.025 g) of test object into a spot tester by a closed spot test method, applying a low-sensitization adhesive tape externally on the curved side of the forearm of a subject, removing the test object after 24 hours, removing the spot tester for 30 minutes, and observing skin reaction after the indentation disappears. If the result is negative, the spot test is observed again 24h and 48h after the spot test. The reaction results were recorded according to the skin adverse reaction grading standard table (table below).
TABLE 1 skin response grading Standard for skin seal Patch test
According to detection, in the 30-person human body closed type skin patch test, 30 persons do not have skin adverse reaction, and the details are shown in Table 2.
TABLE 2 summary of cosmetic body Patch test results
Human whitening efficacy evaluation experiment: skin melanin content (MI value) was measured using a germany CK skin tester mexametemx 18 probe, with higher measurement values indicating higher melanin content in the skin. Skin brightness (darkness) was measured with a colorimeter probe (ITA value): the value of ITA is the individual type angle of the skin, the greater the value of ITA, the brighter the skin, and conversely the darker the skin. The subjects cleaned their faces daily, and the whitening nanoemulsion was used at 1.25. Mu.L/cm 2 The test parts are uniformly coated with the coating density, and the coating is continuously coated for 21 days, wherein the coating density is 1 time in the morning and evening each day. Fig. 3 shows the MI values tested within 21 days, and fig. 4 shows the melanin reduction rate within 3 weeks. From the figure, the whitening nanoemulsion can well reduce the melanin content of skin and improve the brightness. Fig. 5 shows the ITA ° test value over 21 days, and fig. 6 shows the gloss rise over 3 weeks.
The glycerin and dipropylene glycol are compounded, so that the oil-water distribution coefficient is just suitable, and the emulsion is stable and does not break. Meanwhile, the combination of two emulsifying agents, namely dipalmitoyl phosphatidylcholine and soybean lecithin, not only improves the emulsifying effect, but also assists in solubilizing azelaic acid, ferulic acid and hesperidin, so that the solubility of azelaic acid, ferulic acid and hesperidin is improved, and meanwhile, the emulsion is stable and does not break. The invention adopts the soybean lecithin with the phosphatidylcholine content of 40wt% to compound with the 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 simultaneously the compounding of the two emulsifying agents improves the stability of emulsion.
Comparative example 1:
the whitening nanoemulsion is prepared from 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 horse chestnut saponin, 5 parts of dipalmitoyl phosphatidylcholine, 3 parts of lecithin (PC 40), 1 part of mannitol erythritol 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 of water.
The preparation method comprises the following steps:
1. azelaic acid, ferulic acid, dipropylene glycol and glycerin are mixed and heated to 65 ℃ to be completely dissolved to obtain a composition 1;
2. mixing glycerol acetate, hesperidin and aesculin, and heating to 65deg.C for dissolving completely to obtain composition 2;
3. slowly adding composition 1 into composition 2 at 65deg.C under stirring to obtain composition 3;
4. mixing water, mannose erythritol lipid, dipalmitoyl phosphatidylcholine and lecithin, heating to 60deg.C, homogenizing until lecithin is completely dissolved to obtain composition 4;
5. adding the composition 3 into the composition 4, and uniformly stirring for 3-5 minutes until the composition is completely emulsified;
6. and adding the emulsified emulsion into a high-pressure homogenizer, and refluxing for 3 times under the pressure of 400bar to obtain the whitening nano emulsion.
Experimental results: the appearance is opaque emulsion, and the particle size is about 100-120nm, as shown in figure 12.
Stability test results: the sample is placed in a high-low temperature incubator for cyclic experiment, and no obvious change is generated within 1 month.
Fig. 7 is a transdermal experimental graph of the whitening combination emulsion of the present embodiment, c-1 is a transdermal experimental white light channel graph of the whitening nanoemulsion of the present embodiment, and c-2 is a transdermal experimental fluorescence graph of the whitening nanoemulsion of the present embodiment. Figure 8 shows the MI measured within 21 days of the whitening composition emulsion. Fig. 9 shows the melanin reduction rate of the whitening composition emulsion for 3 weeks. Fig. 10 is the ITA ° measured within 21 days of the whitening combination emulsion. Fig. 11 is a luminance improvement rate within 3 weeks of the whitening composition emulsion.
The factors that lead to instability of the emulsion are mainly the following: layering, flocculation, phase inversion, polymerization, oryza sativa maturation. Wherein the Orshi ripening means that small particles in the system become smaller and adhere to large particles, and finally the phenomenon that the small particles are smaller and the large particles are bigger is caused, and the pressure and the reflux times for preparing the nano emulsion can influence the particle size distribution, the transdermal effect and the whitening effect of the product. The pressure and the reflux times are smaller, the force for breaking the emulsion is smaller, so that the particle size of the prepared nano emulsion is larger and uneven, and the Oryza curing can be caused; too large pressure and too many times of reflux can cause re-agglomeration of the nano emulsion particle size after excessive scattering; the large particle size makes the active substance not easily penetrate into the skin to affect the whitening effect, so that the preferable proper pressure and the adjustment of the optimal number of reflux times are important for obtaining a stable product with excellent transdermal and whitening effects.
Comparative example 2:
31 parts of azelaic acid, 14 parts of ferulic acid, 5 parts of hesperidin, 2 parts of horse chestnut saponin, 5 parts of dipalmitoyl phosphatidylcholine, 3 parts of lecithin (PC 40), 1 part of mannitol erythritol 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 of water.
The preparation method is the same as in example 1.
Experimental results: it was found that if glycerol and dipropylene glycol were replaced with butanediol and propylene glycol (C 3 H 8 O 2 ) Can cause azelaic acid and ferulic acidCan not be completely dissolved, crystals are separated out after cooling, and emulsion is broken.
Azelaic acid and ferulic acid have solubilities between water and oil, and it is difficult to find suitable solvents which are not soluble in oil nor water, and glycerol or propylene glycol alone, although being soluble at high temperatures, can precipitate from the system when the temperature is lowered to room temperature, and the product is eventually unstable. While it is more difficult to dissolve azelaic acid and ferulic acid simultaneously and to find a solvent which can be suitable for them simultaneously, the prior art has not solved this technical problem.
Comparative example 3:
31 parts of azelaic acid, 14 parts of ferulic acid, 5 parts of hesperidin, 2 parts of horse chestnut saponin, 3 parts of caprylic/capric triglyceride, 1 part of mannitol erythritol lipid, 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 of water.
The preparation method is the same as in example 1.
Experimental results: the emulsion is demulsified after being cooled, the emulsification effect is poor, and the experimental requirements cannot be met.
Comparative example 4:
the whitening nanoemulsion is composed of 31 parts of azelaic acid, 14 parts of ferulic acid, 5 parts of hesperidin, 2 parts of aesculin, 8 parts of dipalmitoyl phosphatidylcholine, 1 part of mannitol erythritol 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 of water.
The preparation method is the same as in example 1.
Experimental results: after the emulsion is cooled, more precipitate is separated out. The combination of two emulsifying agents, namely dipalmitoyl phosphatidylcholine and soybean lecithin (PC 40), not only improves the emulsifying effect, but also assists in solubilizing azelaic acid, ferulic acid and hesperidin, so that the solubility of azelaic acid, ferulic acid and hesperidin is improved, and meanwhile, the emulsion is stable and does not break. The dipalmitoyl phosphatidylcholine alone has poor effect, the solubility of azelaic acid, ferulic acid and hesperidin is obviously reduced, and the simultaneous requirements of emulsification and solubilization cannot be met.
Comparative example 5:
the whitening nanoemulsion is prepared from 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 horse chestnut saponin, 5 parts of dipalmitoyl phosphatidylcholine, 3 parts of lecithin (PC 80), 1 part of mannitol erythritol 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 of water.
The preparation method is the same as in example 1.
Experimental results: after the emulsion is cooled, precipitation is formed. The invention discovers that the soybean lecithin with the phosphatidylcholine content of 80wt% and dipalmitoyl phosphatidylcholine are compounded to cause poor solubility of azelaic acid and ferulic acid, and emulsion is precipitated and separated, so that the emulsion is unstable.
In summary, the invention adopts the nanoemulsion technology to find out proper solvents, emulsifiers and the like to completely dissolve functional raw materials and prepare nanoemulsion with uniform particle size, the invention can realize the simultaneous dissolution of 32% azelaic acid, 14% ferulic acid, 5% hesperidin and 2% horse chestnut saponin, the emulsion is very stable and not demulsified, the emulsion is not precipitated, the components are directly mixed and dissolved, the complex steps of ethanol re-drying and the like are not required to be introduced in the dissolution process, the solvents and the emulsifiers are the whitening and moisturizing functional components, the emulsifying and moisturizing functions are realized, the solvent is used for dissolving the azelaic acid, the ferulic acid and other active components, the process is simplified and safer, the composition can be added into aqueous products, and the emulsifying body is also added, so that the slow release permeation of the aqueous emulsion in skin is enhanced by adopting hydrogenated phosphatidylcholine, soybean lecithin (PC 40) and mannose erythritol lipid obtained by biological fermentation, and the effects of mild, safety and high efficiency are achieved.
It should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same, 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 the technical solution of the present invention may be modified or substituted without departing from the spirit and scope of the technical solution of the present invention, which is intended to be covered in the scope of the claims of the present invention.
Claims (7)
1. A method for preparing a whitening composition for improving the solubility of active ingredients, which is characterized in that: is composed of the following steps of the method,
step 1: mixing azelaic acid, ferulic acid, dipropylene glycol and glycerol, and heating to obtain composition 1;
step 2: mixing glycerol acetate, hesperidin and aesculin, and heating to obtain composition 2;
step 3: slowly adding the composition 1 into the composition 2, and stirring while adding to obtain a composition 3;
step 4: mixing water, mannose erythritol lipid, dipalmitoyl phosphatidylcholine and lecithin, heating, and homogenizing until lecithin is completely dissolved to obtain composition 4;
step 5: adding the composition 3 into the composition 4, and uniformly stirring until the mixture is completely emulsified;
step 6: adding the product obtained in the step 5 into a high-pressure homogenizer, and refluxing at a high pressure of 800-900 bar for 8-9 times to obtain a whitening nano emulsion;
wherein, according to the mass parts of raw materials, 5-32 parts of azelaic acid, 1-14 parts of ferulic acid, 0.5-5 parts of hesperidin, 1-2 parts of aesculin, 1-5 parts of dipalmitoyl phosphatidylcholine, 1-4 parts of lecithin, 0.1-1 part of mannitol erythritol ester, 4-6 parts of glyceroacetate, 5-12 parts of glycerol, 1-7 parts of dipropylene glycol and the balance of water to 100 parts;
the lecithin is soybean lecithin, and the phosphatidylcholine content of the lecithin is 40%.
2. The method for preparing a whitening composition for improving the solubility of active ingredients according to claim 1, characterized in that: in the step 1, heating to 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 to 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 6, the pressure is 850bar.
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 the step 5, the homogenization time is 3-5 min.
6. The method for preparing a whitening composition for improving the solubility of active ingredients according to claim 1 or 2, characterized in that: the weight portions of the raw materials are 27-30 portions of azelaic acid, 13-14 portions of ferulic acid, 3-5 portions of hesperidin, 1-2 portions of aesculin, 4-5 portions of dipalmitoyl phosphatidylcholine, 2-3 portions of lecithin, 0.5-1 portion of mannitol erythritol ester, 4-5 portions of glyceroacetate, 10-12 portions of glycerol, 6-7 portions of dipropylene glycol and the balance of water to 100 portions.
7. Use of the whitening composition according to claim 1 for preparing whitening mask, essence, emulsion and cream.
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| CN109481319A (en) * | 2018-11-22 | 2019-03-19 | 杭州千岛湖天鑫有限公司 | A kind of micro-nano lotion of camellia oil and preparation method thereof |
| CN110946796A (en) * | 2019-12-23 | 2020-04-03 | 苏州绿叶日用品有限公司 | Whitening composition containing endothelin antagonist and preparation method and application thereof |
| CN111956637A (en) * | 2020-09-02 | 2020-11-20 | 谢志辉生物医药研究院(广州)有限公司 | Acne-removing ointment and preparation method thereof |
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