CN112006924A - Chitosan-modified vitamin complex nano-liposome, preparation method thereof and application thereof in cosmetics - Google Patents
Chitosan-modified vitamin complex nano-liposome, preparation method thereof and application thereof in cosmetics Download PDFInfo
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Abstract
The invention belongs to the technical field of cosmetic raw materials, and discloses a chitosan-modified vitamin complex nano liposome, a preparation method thereof and application thereof in cosmetics. The method comprises the following steps: weighing 3.5-4.5% of vitamin A, 5.5-6.5% of vitamin E and 0.5-1.5% of caprylic/capric triglyceride by mass percent, and uniformly stirring in a water bath at 65 ℃ to obtain phase A; weighing 1.5-2.5% of lecithin, 0.3-0.6% of chitosan, 70-80% of glycerol and 8-15% of water by mass percent, and uniformly stirring in a water bath at 65 ℃ to obtain a phase B; adding the phase A into the phase B in the water bath heating and stirring process, and continuing to heat and stir in the water bath at 65 ℃ for 1.5-2.5 h to obtain a composite vitamin liposome primary emulsion; and homogenizing the primary emulsion by adopting a high-pressure micro-jet homogenization method to obtain the product.
Description
Technical Field
The invention belongs to the technical field of cosmetic raw materials, and particularly relates to a chitosan-modified vitamin complex nano liposome, a preparation method thereof and application thereof in cosmetics.
Background
The vitamin complex nano liposome is a new skin care product raw material, and the liposome technology is utilized to wrap the vitamin so as to improve the stability, bioavailability, slow release, irritation reduction and the like of the vitamin complex nano liposome. Vitamins (vitamines) are a class of organic substances essential to the maintenance of human vital activities. In the aspect of cosmetic application, due to poor water solubility, stability and low bioavailability of vitamin A and vitamin E, ideal effects in skin care products are difficult to achieve. Liposome (Liposome) is an ultramicro vesicle formed by encapsulating active substance in lipid bilayer, and has the advantages of good biocompatibility, easy degradation in vivo, no toxicity to organism, no antigenicity and the like because of being similar to biomembrane in composition, and can be used as a good active substance carrier. However, the problems of poor stability and low bioavailability of the vitamin complex can only be partially solved by adopting a liposome encapsulation technology at present, the requirements of the modern cosmetic industry can not be completely met, and the main phenomena are that the liposome prepared from natural phospholipid is easy to show physical or chemical instability in storage, and aggregation, oxidation, rancidity, burst release and the like are generated, and the main reason is that ester bonds and unsaturated acyl groups on the structure of phosphatidylcholine which is the main component in the phospholipid are easy to generate hydrolysis reaction or oxidation reaction.
Disclosure of Invention
In order to overcome the defects of oxidative rancidity and burst release of the vitamin complex nanoliposome in the prior art, the invention mainly aims to provide a preparation method of the chitosan modified vitamin complex nanoliposome; the method adopts a double-layer wrapping mode to solve the problem, namely, a chitosan coat is wrapped on the outer side of the liposome, because the chitosan belongs to a natural polysaccharide polymer, the biocompatibility is good, and the skin is well conditioned, when the chitosan is used for wrapping the liposome, the effects of improving the stability, bioavailability, slow release, reducing the irritation and the like of the vitamin complex can be realized while the product effect is not influenced, the problems of oxidative rancidity and burst release of the vitamin complex of the liposome can be solved to the maximum extent, and the stability of the product is further improved.
The invention further aims to provide the chitosan-modified vitamin complex nano-liposome prepared by the preparation method.
The invention also aims to provide application of the chitosan-modified vitamin complex nano-liposome.
The purpose of the invention is realized by the following technical scheme:
a preparation method of chitosan modified vitamin complex nano-liposome comprises the following steps:
(1) weighing 3.5-4.5% of vitamin A, 5.5-6.5% of vitamin E and 0.5-1.5% of caprylic/capric triglyceride by mass percent, stirring for 25min in a water bath stirrer at the temperature of 65 ℃, stirring at the speed of 450rpm, and after uniformly stirring, naming the mixture as phase A;
(2) weighing 1.5-2.5% of lecithin, 0.3-0.6% of chitosan, 70-80% of glycerol and 8-15% of water by mass percent, stirring for 25min in a water bath stirrer at the temperature of 65 ℃, stirring at the speed of 450rpm, and after uniformly stirring, naming the mixture as phase B;
(3) adding the phase A into the phase B in the water bath heating and stirring process, and continuing to heat and stir in the water bath at 65 ℃ for 1.5-2.5 h after the phase A is completely added into the phase B to form a vitamin complex liposome primary emulsion;
(4) and (3) homogenizing the vitamin complex liposome primary emulsion obtained in the step (3) by adopting a high-pressure micro-jet homogenization method, so that the dispersity and the stability of the vitamin complex liposome primary emulsion are improved, wherein the homogenization parameters are as follows: homogenizing under 1800bar, and circulating for 3-5 times to obtain chitosan modified vitamin complex nano liposome.
The vitamin A in the step (1) is retinol palmitate or retinol acetate; vitamin E is tocopherol acetate.
The lecithin in the step (2) is soybean lecithin or egg yolk lecithin; the chitosan is chitosan or carboxymethyl chitosan.
The chitosan modified vitamin complex nano-liposome prepared by the preparation method.
The chitosan-modified vitamin complex nano-liposome is applied to cosmetics.
The principle of the invention is as follows:
the reasons for the effect of chitosan on the oxidative rancidity and burst release of nanoliposomes are as follows: chitosan (CTS) is a dephthalyl derivative of chitin extracted from crustacean shell or fungus, and has excellent biological properties such as biomembrane adhesion, promotion of drug absorption, good biocompatibility and antibacterial activity. The liposome is coated by chitosan, so that a layer of compact and certain-thickness membrane is added on the surface of the liposome membrane, the release of the vitamin is slowed, the slow-release effect is achieved, and the problems of sudden release and leakage of the vitamin are solved. Meanwhile, the chitosan wraps the liposome, so that the repulsion among liposome particles can be increased, the particles are prevented from being gathered, a film structure is formed on the surface of the liposome, hydrophobic binding sites are covered, and the stability of the liposome is improved.
The reason that the high-pressure micro-jet homogenization method plays a role in the dispersibility and stability of the chitosan-modified vitamin complex nano-liposome is as follows: the high-pressure micro-jet technology is used as a novel nano liposome preparation technology, achieves the aims of homogenization and refinement through high-speed impact, shearing and cavitation, and has the advantages of simple and convenient operation, cleanness, safety, easiness in large-scale continuous production and the like. In the present invention, the advantages of the high-pressure micro-jet technology are mainly shown in the following aspects: compared with other preparation methods, the liposome prepared by the technology has controllable particle size, can ensure that each part of a material body obtains the same homogenizing effect, has very good reproducibility, and can realize continuous homogeneous production. The material body is processed by the actions of severe shearing, oscillation, collision, cavitation effect, correlation and the like, the physical and chemical properties of the material body can be changed, and finally the homogeneous effects of particle size reduction, narrow distribution, increased stability, uniformity, transparency and the like are achieved; thirdly, the materials are fully mixed, the surface area of the reaction is increased, and the speed of the physical and chemical reactions is accelerated, so that the aims of better improving the dispersibility and the stability of the materials are fulfilled.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the material body proportion, the heating temperature, the stirring time and the speed in the step (1) and the step (2) of the preparation method are results obtained through experimental optimization design, and the optimal synergistic effect between active matters can be exerted by combining the precise proportion between the material bodies under the condition, and the inter-batch difference in the process of producing the liposome in large batch can be solved; under the action of the functions of a protective barrier of chitosan and the like, the vitamin complex nano liposome can prevent the oxidative rancidity and burst release of the nano liposome and improve the slow release and efficacy of the vitamin complex nano liposome.
(2) The high-pressure microjet homogenization parameters in the step (4) of the preparation method are the results obtained through experimental optimization design, and under the homogenization parameters, the composite vitamin nano liposome can be protected from being influenced by the dispersibility and stability of the liposome due to overlarge pressure or overlarge circulation times; the vitamin complex nano liposome can only exert an extremely synergistic effect under the mutual action of the high-pressure micro jet and the chitosan, thereby achieving the optimal effect of the vitamin complex nano liposome.
(3) Compared with the common vitamin complex liposome on the market, the chitosan-modified vitamin complex nano liposome prepared by the technical scheme has better stability, is not easy to oxidize, has a more lasting sustained-release effect, and has lower irritation and sensitivity to skin. The main reason is that the chitosan combines the high-pressure micro-jet technology under the vitamin complex liposome system, so that the chitosan exerts an extremely good effect, not only plays a role in protecting the oxidative rancidity and burst release of the liposome, but also can improve the effect of the vitamin complex liposome.
Drawings
Fig. 1 is a result of wrinkle removal efficacy test of the sample obtained in example 2.
Fig. 2 is a result of wrinkle removal efficacy test of the sample obtained in example 1.
FIG. 3 is a graph of the in vitro drug release profiles of the samples obtained in examples 1, 2 and 3.
FIG. 4 is a graph showing a particle size distribution of a sample obtained in example 1.
Detailed description of the invention
The invention is further described in the following description with reference to the figures and specific examples, which should not be construed as limiting the invention. Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art. Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated.
Example 1
The embodiment is a preparation method of chitosan-modified vitamin complex nano-liposome, and the process comprises the following steps:
(1) weighing 4% of retinol palmitate, 6% of tocopheryl acetate and 1% of caprylic/capric triglyceride by mass percent, stirring for 25min in a water bath stirrer at 65 ℃, wherein the stirring speed is 450rpm, and after the mixture is uniformly stirred, the mixture is named as phase A;
(2) weighing 2% of soybean lecithin, 0.5% of chitosan, 75% of glycerol and 11.5% of water by mass percent, stirring for 25min in a water bath stirrer at 65 ℃, wherein the stirring speed is 450rpm, and after the materials are uniformly stirred, the material is named as phase B;
(3) slowly adding the phase A into the phase B during water bath heating and stirring, and continuing to heat and stir in the water bath at 65 ℃ for 2h after the phase A is completely added into the phase B to form a composite vitamin liposome primary emulsion;
(4) and (3) homogenizing the vitamin complex liposome primary emulsion obtained in the step (3) by adopting a high-pressure micro-jet homogenization method, so that the dispersibility and stability of the vitamin complex liposome primary emulsion are improved, and the homogenizing parameters are as follows: homogenizing under 1800bar, and circulating for 4 times to obtain chitosan-modified vitamin complex nano liposome. The particle size distribution diagram of the obtained chitosan-modified vitamin complex nanoliposome is shown in figure 4.
The chitosan-modified vitamin complex nanoliposome prepared in the embodiment is yellow semitransparent liquid in appearance and has characteristic smell.
Example 2
This example is the preparation of a vitamin complex nanoliposome with formulation bias, the process of which is as follows:
(1) weighing 4% of retinol palmitate, 6% of tocopheryl acetate and 1% of caprylic/capric triglyceride by mass percent, stirring for 25min in a water bath stirrer at 65 ℃, wherein the stirring speed is 450rpm, and after the mixture is uniformly stirred, the mixture is named as phase A;
(2) weighing 2% of soybean lecithin, 75% of glycerol and 12% of water by mass, stirring for 25min in a water bath stirrer at 65 ℃, wherein the stirring speed is 450rpm, and after the materials are uniformly stirred, the material is named as phase B;
(3) slowly adding the phase A into the phase B during water bath heating and stirring, and continuing to heat and stir in the water bath at 65 ℃ for 2h after the phase A is completely added into the phase B to form a composite vitamin liposome primary emulsion;
(4) and (3) homogenizing the vitamin complex liposome primary emulsion obtained in the step (3) by adopting a high-pressure micro-jet homogenization method, so that the dispersibility and stability of the vitamin complex liposome primary emulsion are improved, and the homogenizing parameters are as follows: homogenizing under 1800bar, and circulating for 4 times to obtain vitamin complex nanoliposome.
The vitamin complex nanoliposome prepared in the embodiment is yellow semitransparent liquid in appearance and has characteristic smell.
Example 3
This example is a process for preparing a multivitamin liposome primary emulsion with process variation, which comprises the following steps:
(1) weighing 4% of retinol palmitate, 6% of tocopheryl acetate and 1% of caprylic/capric triglyceride by mass percent, stirring for 25min in a water bath stirrer at 65 ℃, wherein the stirring speed is 450rpm, and after the mixture is uniformly stirred, the mixture is named as phase A;
(2) weighing 2% of soybean lecithin, 0.5% of chitosan, 75% of glycerol and 11.5% of water by mass percent, stirring for 25min in a water bath stirrer at 65 ℃, wherein the stirring speed is 450rpm, and after the materials are uniformly stirred, the material is named as phase B;
(3) slowly adding the phase A into the phase B during water bath heating and stirring, and continuing to heat and stir in the water bath at 65 ℃ for 2h after the phase A is completely added into the phase B to finally form the vitamin complex liposome primary emulsion.
The vitamin complex liposome primary emulsion prepared in the embodiment is yellow suspension in appearance and has characteristic smell.
Example 4
This example is a particle size test and a heat stability test of the samples prepared in examples 1, 2 and 3.
The test method comprises the following steps:
(1) the test was carried out using a malvern Nano ZS90 particle size potential detector, and the test sample was diluted 500 times with ultrapure water at a test angle of 90 ° and a test temperature of 25 ℃, and repeated 3 times.
(2) The samples of examples 1, 2 and 3 were prepared and placed under a heat-resistant condition of 45 c, and their particle size, PDI, appearance state and odor were measured on the day of preparation, after one month, after two months and after three months, respectively. And (3) testing results:
TABLE 1 stability test results for the sample of example 1
TABLE 2 stability test results for the samples of example 2
TABLE 3 stability test results for the samples of example 3
As can be seen from tables 1, 2 and 3 above, the three-month heat stability of the sample of example 1 is better than the particle size, dispersion index (PDI), appearance state and odor of examples 2 and 3. Therefore, the chitosan can play a better role in protecting a barrier for a vitamin complex nano liposome system under the action of combining high-pressure micro jet, and has a good stability effect on indexes such as particle size, dispersion index (PDI), appearance and smell.
Example 5
This example is a test of the efficacy of the samples prepared in examples 1 and 2.
The test method comprises the following steps:
the test is carried out according to the human body efficacy evaluation test method and the requirements in section 1 of chapter eight in the cosmetic safety technical specification 2015 edition.
The test results are shown in fig. 1 and 2.
As can be seen from the above fig. 1 and 2, the wrinkle removal rate of the sample of example 1 is 90%, and the wrinkle removal rate of the sample of example 2 is 71.4%. Therefore, the chitosan modified vitamin complex nano liposome can improve the efficacy of the vitamin complex nano liposome, and the wrinkle removal rate is improved by 18.6%.
Example 6
This example is a safety test of the samples prepared in examples 1, 2 and 3.
The test method comprises the following steps:
the test was performed according to the skin irritation test method and requirements in chapter sixth, section 4, in the cosmetic safety specifications 2015 edition.
The test results are shown in table 4 below:
TABLE 4 safety test results for samples of examples 1, 2 and 3
As can be seen from Table 4, the skin irritation was more alleviated for the sample of example 1 than for the samples of examples 2 and 3. Therefore, the chitosan-modified vitamin complex nanoliposome can reduce the irritation of a vitamin complex nanoliposome system under the action of combining high-pressure microfluidics.
Example 7
This example is an in vitro drug release assay test of the samples prepared in examples 1, 2 and 3.
The test method comprises the following steps:
the in vitro drug release experiment was performed by dialysis bag method. A cellulose semipermeable membrane (with a molecular weight cut-off of 10KDa) is selected as a permeable membrane, and is boiled in ultrapure water for half an hour before use. The drug release medium is 5% Labrasol-20% ethanol-PBS solution. Samples of examples 1, 2 and 3 were taken and put into a dialysis bag, both ends were tied up with a rope, the dialysis bag was placed in a 100mL Erlenmeyer flask containing 5% Labrasol-20% ethanol-PBS release medium, shaken on a shaker at 0.5 (37 f) deg.C and placed at a speed of 100r/min, 2mL samples were taken at 0.5h, 1h, 1.5h, 2h, 3h, 4h, 6h, 8h, 10h, 12h and 24h, and then 2mL of blank release medium at the same temperature was rapidly supplemented. The samples were analyzed by HPLC to measure their concentrations and the cumulative release of the drug over time was calculated.
The test results are shown in fig. 3.
As can be seen from FIG. 3, the samples of example 1 showed better in vitro sustained release effects than the samples of examples 2 and 3. Therefore, the chitosan-modified vitamin complex nanoliposome can obviously improve the slow release effect of the vitamin complex nanoliposome under the action of combining high-pressure microfluidics.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (5)
1. A preparation method of chitosan modified vitamin complex nano-liposome is characterized by comprising the following steps:
(1) weighing 3.5-4.5% of vitamin A, 5.5-6.5% of vitamin E and 0.5-1.5% of caprylic/capric triglyceride by mass percent, stirring for 25min in a water bath stirrer at the temperature of 65 ℃, stirring at the speed of 450rpm, and after uniformly stirring, naming the mixture as phase A;
(2) weighing 1.5-2.5% of lecithin, 0.3-0.6% of chitosan, 70-80% of glycerol and 8-15% of water by mass percent, stirring for 25min in a water bath stirrer at the temperature of 65 ℃, stirring at the speed of 450rpm, and after uniformly stirring, naming the mixture as phase B;
(3) adding the phase A into the phase B in the water bath heating and stirring process, and continuing to heat and stir in the water bath at 65 ℃ for 1.5-2.5 h after the phase A is completely added into the phase B to form a vitamin complex liposome primary emulsion;
(4) and (3) homogenizing the vitamin complex liposome primary emulsion obtained in the step (3) by adopting a high-pressure micro-jet homogenization method, so that the dispersity and the stability of the vitamin complex liposome primary emulsion are improved, wherein the homogenization parameters are as follows: homogenizing under 1800bar, and circulating for 3-5 times to obtain chitosan modified vitamin complex nano liposome.
2. The method for preparing the chitosan-modified vitamin complex nanoliposome as claimed in claim 1, wherein the method comprises the following steps: the vitamin A in the step (1) is retinol palmitate or retinol acetate; vitamin E is tocopherol acetate.
3. The method for preparing the chitosan-modified vitamin complex nanoliposome as claimed in claim 1, wherein the method comprises the following steps: the lecithin in the step (2) is soybean lecithin or egg yolk lecithin; the chitosan is chitosan or carboxymethyl chitosan.
4. A chitosan-modified vitamin complex nanoliposome prepared by the preparation method of any one of claims 1 to 3.
5. The use of chitosan-modified vitamin complex nanoliposomes of claim 4 in cosmetics.
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| CN114652636A (en) * | 2022-03-10 | 2022-06-24 | 广东丸美生物技术股份有限公司 | Anti-wrinkle repair composition, preparation method thereof and cosmetic containing composition |
| CN114652636B (en) * | 2022-03-10 | 2023-11-17 | 广东丸美生物技术股份有限公司 | Anti-wrinkle repair composition, preparation method thereof and cosmetic containing composition |
| CN116350537A (en) * | 2023-05-04 | 2023-06-30 | 肽源（广州）生物科技有限公司 | Collagen nanoparticle, preparation method thereof and application thereof in cosmetics |
| CN116350537B (en) * | 2023-05-04 | 2024-03-29 | 肽源（广州）生物科技有限公司 | Collagen nanoparticle, preparation method thereof and application thereof in cosmetics |
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