CN112220696A - Fullerene nano emulsion and preparation method and application thereof - Google Patents
Fullerene nano emulsion and preparation method and application thereof Download PDFInfo
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- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
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Abstract
The invention discloses fullerene nano-emulsion and a preparation method thereof. The nano emulsion comprises the following components: 0.05-5 parts of fullerene, 15-35 parts of lipid, 3-15 parts of surfactant, 0.1-5 parts of cosurfactant and 45-75 parts of deionized water in balance; stirring and shearing according to the preparation method of the process flow diagram to form fullerene nanoemulsion primary emulsion, and treating the fullerene nanoemulsion primary emulsion by a high-pressure homogenizer at the high-pressure homogenizing pressure of 500-900bar for 1-5 times to obtain the light-purple translucent to transparent fullerene nanoemulsion. The invention wraps unmodified fullerene in the nano emulsion carrier, solves the problems of poor water solubility, poor stability and the like of the fullerene, and has the advantages of high fullerene nano emulsion encapsulation rate (more than 99 percent), good structural stability, simple operation, good repeatability and good transdermal absorption performance.
Description
Technical Field
The invention relates to a chemical material and a preparation method thereof, in particular to fullerene nano-emulsion and a preparation method and application thereof.
Background
Fullerene (C60) is an allotrope of elemental carbon. The structure is a hollow 32-sided body consisting of 12 pentagons and 20 hexagons, and the density is 1.678g/cm3The melting point is > 553K. C60 appears as a dark yellow solid, and can be brown to black in color depending on thickness. Fullerene has high oxidation resistance, 125 times of vitamin C, has a similar action principle as superoxide dismutase (SOD), and has higher capacity and speed of capturing free radical molecules than beta-carotene. In addition, fullerene has high safety, and has been studied to some extent in the fields of medicines, cosmetics, foods and the like.
In the aspect of medicine, fullerene has strong photodynamic activity and free radical scavenging activity, and can be used as a gene carrier and a drug carrier, so that the fullerene can play an important role in the aspects of treating tumors, diseases caused by oxidative stress and the like. The fullerene can be used as an antioxidant to improve the stability of the oleic acid and the food thereof by delaying the autoxidation process of the fatty acid, and prolong the shelf life. The ultra-strong oxidation resistance of the fullerene makes people have a very high interest in the application of the fullerene in the field of skin care of cosmetics. Fullerene mainly has the following effects in the field of cosmetic skin care: resisting aging, removing wrinkle, whitening skin, removing speckle, inhibiting acne, and shrinking follicular orifice. The fullerene can continuously remove skin free radicals which are continuously promoted by ultraviolet rays, haze and other environmental pollution, self pressure, alcohol, nicotine and other external factors, thereby solving various problems of skin aging, relaxation, color spots, acne and the like. Compared with other components, the fullerene has unique electronic characteristics, can adsorb and scavenge free radicals at the source of skin aging chain reaction, and reduces the aging reaction of human bodies. The fullerene has the main effect on free radicals, can provide instant antioxidation like vitamin C, can continuously and effectively adsorb the free radicals like sponge, provides a long-acting protective cover for cells, and improves the damage resistance of the cells.
However, fullerenes have very poor solubility in water, most oils and polar solvents, and are generally soluble only in aromatic solvents such as toluene, chlorobenzene, or non-aromatic solvents such as carbon disulfide. Moreover, fullerene has poor photostability, low bioavailability, and poor skin absorption properties, which results in greatly limited applications of fullerene in cosmetics. At present, the oxidation resistance and other properties of chemically modified fullerenes such as water-soluble fullerenes and oil-soluble fullerenes are greatly affected, and thus, the application defects of fullerenes need to be solved by other better methods.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to provide the nano emulsion with high fullerene content and better water solubility, stability and other properties. The nano emulsion is a transparent or semitransparent homogeneous dispersion system which is composed of water, oil, a surfactant, a cosurfactant and the like. The nanoemulsion can be solubilized by the inner core oil phase and the surfactant, and the nanoemulsion can increase transdermal absorption capacity.
Another object of the present invention is to provide a preparation method and use of the nanoemulsion.
The technical scheme is as follows: the fullerene nano emulsion provided by the invention comprises the following raw materials in parts by weight:
further, the lipid is one or more of caprylic/capric triglyceride, triolein, octyldodecanol, cetyl alcohol, cetearyl alcohol, macadamia nut oil, camellia oleosa seed oil, olive oil and jojoba oil.
Further, the surfactant is one or a mixture of more of tween 80, tween 60, tween 20, glyceryl monostearate, glycerol monolaurate, steareth-21, steareth-2, polyglycerol 10-stearate and polyglycerol 6-stearate.
Further, the cosurfactant is one or a mixture of propylene glycol, glycerol, dipropylene glycol, butanediol and methyl propylene glycol.
The preparation method of the fullerene nano-emulsion comprises the following steps:
(1) weighing fullerene, lipid, surfactant and cosurfactant according to a formula proportion, and mixing and dissolving under a heating condition to obtain an oil phase;
(2) weighing deionized water, and heating to obtain a water phase;
(3) injecting the water phase into the oil phase, and stirring to obtain fullerene nanoemulsion primary emulsion;
(4) homogenizing the fullerene nanoemulsion primary emulsion to obtain the fullerene nano emulsion.
Further, the homogenization conditions are as follows: the pressure is 500-900bar, and the discharge temperature is controlled as follows: 15-45 ℃.
The application of the fullerene nano-emulsion in the preparation of cosmetics.
Has the advantages that: the preparation of the high content nanoemulsions of the invention is controllable. By adjusting the formula of the nano emulsion, the addition amount of the fullerene, the high-pressure homogenization cycle times, the temperature and other conditions, the fullerene nano emulsion with the content of 0.05-5% can be prepared; has a very high fullerene content; according to the invention, the nano emulsion is adopted to wrap the fullerene, so that the water solubility and stability of the fullerene are obviously improved, and the fullerene is not separated out when the nano emulsion is applied to cosmetics; the fullerene nano-emulsion prepared by the invention has good affinity with the skin cuticle, and the fullerene for the skin can achieve multiple effects of aging resistance, repair and the like; the fullerene nanoemulsion prepared by the high-pressure homogenization method has uniform particle size and good stability, has higher encapsulation rate (> 99%) and better slow release effect, and improves the transdermal absorption capacity of fullerene.
Drawings
FIG. 1 is a schematic flow diagram of the process of the present invention;
FIG. 2 is an electron micrograph of a fullerene nanoemulsion of the present invention;
FIG. 3 is a graph showing the temperature stability of the fullerene nanoemulsion of the present invention;
FIG. 4 is a graph showing the measurement of the stability of fullerene nanoemulsion according to the present invention;
fig. 5 is a test chart of the transdermal behavior of the fullerene nanoemulsion of the present invention.
Detailed Description
Example 1
The formula of the nanoemulsion of this example is as follows:
the preparation procedure for this example is as follows:
1. accurately weighing 0.1g of fullerene, 10.0g of caprylic/capric triglyceride, 5.0g of olive oil, 802.5 g of tween, 208.0 g of tween and 3.5g of glycerol, and magnetically stirring at 40 ℃ and 300rpm for 1h until the fullerene is completely dissolved to form an oil phase;
2. putting 70.9g of deionized water into a water bath at 40 ℃ for heating to form a water phase;
3. pouring the water phase into the oil phase at one time, stirring at 40 ℃ and 400rpm for 10min to form fullerene nanoemulsion primary emulsion;
4. homogenizing the primary emulsion with high pressure of 700bar for 1 cycle, and controlling the final discharge temperature to 25 + -3 deg.C;
5. and (3) collecting the material after homogenizing to obtain the fullerene nanoemulsion, wherein the average particle size of the fullerene nanoemulsion is 70.33 +/-2.12 nm and the PDI is 0.062 +/-0.048 as determined by a particle size potential analyzer.
Example 2
The formula of the nanoemulsion of this example is as follows:
the preparation procedure for this example is as follows:
1. accurately weighing 0.05g of fullerene, 23.0g of triolein, 808.5 g of tween, 1.5g of glyceryl monostearate and 1.0g of propylene glycol, and magnetically stirring at 65 ℃ and 400rpm for 1h until the fullerene is completely dissolved to form an oil phase;
2. putting 65.95g of deionized water into a 65 ℃ water bath for heating to form a water phase;
3. pouring the water phase into the oil phase at one time, stirring at 65 ℃ and 500rpm for 15min to form fullerene nanoemulsion primary emulsion;
4. homogenizing the primary emulsion with high pressure at 400bar for 3 times, and controlling the final discharge temperature at 25 + -3 deg.C;
5. and (3) receiving the material after homogenizing, namely obtaining the fullerene nanoemulsion, wherein the average particle size of the fullerene nanoemulsion is 62.45 +/-3.01 nm and the PDI is 0.123 +/-0.009 as determined by a particle size potential analyzer.
Example 3
The formula of the nanoemulsion of this example is as follows:
the preparation procedure for this example is as follows:
1. accurately weighing 0.2g of fullerene, 18.5g of triolein, 7.0g of caprylic/capric triglyceride, 2010.0 g of tween, 2.5g of polyglycerol 10-stearate and 2.5g of butanediol, and magnetically stirring at 55 ℃ and 400rpm for 1h until the fullerene is completely dissolved to form an oil phase;
2. placing 59.3g of deionized water in a water bath at 55 ℃ for heating to form a water phase;
3. pouring the water phase into the oil phase at one time, stirring at 55 ℃ and 600rpm for 10min to form fullerene nanoemulsion primary emulsion;
4. homogenizing the primary emulsion with high pressure of 600bar for 4 times of circulation, and controlling the final discharge temperature to 25 +/-3 ℃;
5. and (3) collecting the material after homogenizing to obtain the fullerene nanoemulsion, wherein the average particle size of the fullerene nanoemulsion is 103.33 +/-4.79 nm and the PDI is 0.205 +/-0.081 as determined by a particle size potential analyzer.
Example 4
The formula of the nanoemulsion of this example is as follows:
the preparation procedure for this example is as follows:
1. accurately weighing 2.3g of fullerene, 10.0g of jojoba oil, 17.5g of caprylic/capric triglyceride, 215.0 g of steareth-215.0 g, 1.5g of glycerol and 2.0g of propylene glycol, and magnetically stirring at 70 ℃ and 600rpm for 1h until the lipid fullerene is completely dissolved to form an oil phase;
2. 51.7g of deionized water is placed in a 70 ℃ water bath for heating to form a water phase;
3. pouring the water phase into the oil phase at one time, stirring at 70 ℃ and 700rpm for 8min to form fullerene nanoemulsion primary emulsion;
4. homogenizing the primary emulsion with high pressure homogenizing at 550bar for 2 times, and controlling the final discharge temperature at 25 + -3 deg.C;
5. and (3) collecting the material after homogenizing, namely obtaining the fullerene nanoemulsion, wherein the average particle size of the fullerene nanoemulsion is 153.08 +/-2.11 nm and the PDI is 0.241 +/-0.032 as determined by a particle size potential analyzer.
And (3) performance testing:
the temperature stability, the illumination stability and the percutaneous behavior effect of the product are tested by adopting a conventional method:
as shown in fig. 3: the grain diameter of the fullerene nano emulsion changes with the storage time at different temperatures, and the grain diameter of the fullerene nano emulsion is maintained at about 55nm at 4 ℃ and 25 ℃. It can be shown that the fullerene nanoemulsion has good storage stability at both low and normal temperatures. While there was a slight change in particle size after 4 weeks of storage at 40 ℃ probably due to accelerated particle-to-particle collisions under high temperature conditions, resulting in C60The particle size of NE is increased. This is achieved by
As shown in fig. 4: the change relation of the grain diameter of the fullerene nano-emulsion with different dilution times along with the time is investigated, and the grain diameter of the diluent of the fullerene nano-emulsion with different concentrations along with the increase of the time is not changed greatly. Therefore, the fullerene nanoemulsion has good dilution stability.
As shown in fig. 5: compared with fullerene water solution, the fullerene nano emulsion has higher percutaneous absorption capability and can be slowly controlled to release. This shows that the penetration ability of fullerene is obviously enhanced by the nano emulsion carrier, which is beneficial to the accumulation of fullerene in skin and maintains higher concentration for a longer time, thereby improving the bioavailability of fullerene. Provides a new idea for the application of fullerene in skin care cosmetics.
Claims (7)
1. A fullerene nanoemulsion characterized by: the composite material comprises the following raw materials in parts by weight:
2. a fullerene nanoemulsion according to claim 1, characterised in that: the lipid is one or more of caprylic/capric triglyceride, triolein, octyldodecanol, cetyl alcohol, cetearyl alcohol, macadamia nut oil, camellia oleosa seed oil, olive oil, and jojoba oil.
3. A fullerene nanoemulsion according to claim 1, characterised in that: the surfactant is one or more of Tween 80, Tween 60, Tween 20, glyceryl monostearate, glycerol monolaurate, steareth-21, steareth-2, polyglycerol 10-stearate and polyglycerol 6-stearate.
4. A fullerene nanoemulsion according to claim 1, characterised in that: the cosurfactant is one or a mixture of propylene glycol, glycerin, dipropylene glycol, butanediol and methyl propylene glycol.
5. A method of producing a fullerene nanoemulsion as claimed in any one of claims 1-4, characterized in that: the method comprises the following steps:
(1) weighing fullerene, lipid, surfactant and cosurfactant according to a formula proportion, and mixing and dissolving under a heating condition to obtain an oil phase;
(2) weighing deionized water, and heating to obtain a water phase;
(3) injecting the water phase into the oil phase, and stirring to obtain fullerene nanoemulsion primary emulsion;
(4) homogenizing the fullerene nanoemulsion primary emulsion to obtain the fullerene nano emulsion.
6. A method of preparing a fullerene nanoemulsion as claimed in claim 5, wherein the homogenization conditions are: the pressure is 500-900bar, and the discharge temperature is controlled as follows: 15-45 ℃.
7. Use of a fullerene nanoemulsion according to any one of claims 1-4 in the preparation of cosmetics.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115177539A (en) * | 2022-08-05 | 2022-10-14 | 赤峰福纳康生物技术有限公司 | Preparation method of water-soluble fullerene nano solution |
| CN115429712A (en) * | 2022-09-02 | 2022-12-06 | 广东粤港澳大湾区国家纳米科技创新研究院 | Polypeptide and fullerene co-delivery nano composition, preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018180009A1 (en) * | 2017-03-30 | 2018-10-04 | ビタミンＣ６０バイオリサーチ株式会社 | Fullerene-containing cosmetic composition |
| CN109481463A (en) * | 2017-09-12 | 2019-03-19 | 北京福纳康生物技术有限公司 | A kind of oral fullerene emulsion, preparation method and application |
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- 2020-09-25 CN CN202011029786.1A patent/CN112220696A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018180009A1 (en) * | 2017-03-30 | 2018-10-04 | ビタミンＣ６０バイオリサーチ株式会社 | Fullerene-containing cosmetic composition |
| CN109481463A (en) * | 2017-09-12 | 2019-03-19 | 北京福纳康生物技术有限公司 | A kind of oral fullerene emulsion, preparation method and application |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115177539A (en) * | 2022-08-05 | 2022-10-14 | 赤峰福纳康生物技术有限公司 | Preparation method of water-soluble fullerene nano solution |
| CN115177539B (en) * | 2022-08-05 | 2024-06-07 | 赤峰福纳康生物技术有限公司 | Preparation method of water-soluble fullerene nano solution |
| CN115429712A (en) * | 2022-09-02 | 2022-12-06 | 广东粤港澳大湾区国家纳米科技创新研究院 | Polypeptide and fullerene co-delivery nano composition, preparation method and application thereof |
| CN115429712B (en) * | 2022-09-02 | 2024-01-23 | 广东粤港澳大湾区国家纳米科技创新研究院 | Polypeptide and fullerene co-delivery nano composition, and preparation method and application thereof |
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Application publication date: 20210115 |