CN110585061A - Method for stabilizing Pickering emulsion by using regenerated chitin - Google Patents
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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
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/04—Dispersions; Emulsions
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- 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
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- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
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Abstract
The invention discloses a method for preparing Pickering emulsion by using regenerated chitin, which comprises the following steps: mixing the water phase and the oil phase by taking the regenerated chitin suspension as the water phase and GTCC as the oil phase, wherein the mass concentration of the oil phase in the obtained mixed solution is 10-50%; in the regenerated chitin suspension, the mass concentration of the regenerated chitin is 0.2-1.2%; dispersing the obtained mixed solution to obtain Pickering emulsion. The emulsion obtained by the invention has good stability, and solves the problems of environment and skin irritation caused by using a large amount of the surfactant in the prior art.
Description
Technical Field
The invention belongs to the field of cosmetic emulsion, and particularly relates to a method for preparing emulsion by stabilizing cosmetic oil with regenerated chitin suspension, namely a method for stabilizing Pickering (Pickering) emulsion by utilizing regenerated chitin.
Background
At present, a great deal of research has been conducted to show that solid particles have a positive effect in cosmetics as an emulsifier. The solid particles are used as an emulsifier instead of the traditional surfactant and applied to cosmetics, so that the irritation of the product to the human skin caused by the self property of part of the surfactant is reduced. Besides the emulsification effect as a stabilizer, some solid particles also have certain properties such as ultraviolet resistance, oxidation resistance, bacteria resistance and the like, and the additional functions enable the product to have better efficacy.
Pickering emulsion refers to an emulsion obtained by using ultrafine solid particles as an emulsifier, and is also called Pickering emulsion.
Solid particles currently used as emulsifiers for cosmetics include titanium dioxide, zinc oxide, and the like.
Chitin is the only natural polymer with positive charges in the world developed by human to date, and is the only biological nitrogenous polysaccharide macromolecule in nature. The chitin can directly participate in carbon and nitrogen circulation after being degraded by biological enzymes such as chitinase, lysozyme, chitosanase and the like in an ecological system, and plays an indispensable regulation and control role on the earth ecological system. And the biomass fuel is a cheap, biodegradable, renewable, nontoxic and environment-friendly sustainable resource, and is a natural resource treasure house which can be fully utilized by human beings. However, the application of the solid particles in cosmetics has not been reported at present.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for regenerating a stable Pickering (Pickering) emulsion of chitin, wherein the obtained emulsion has good stability, and solves the problems of environment and skin irritation caused by using a large amount of surfactant in the prior art.
In order to solve the technical problems, the invention provides a method for preparing Pickering emulsion by using regenerated chitin, which comprises the following steps:
mixing the water phase and the oil phase by taking the regenerated chitin suspension as the water phase and GTCC (caprylic/capric triglyceride) as the oil phase, wherein the mass concentration of the oil phase in the obtained mixed solution is 10-50%;
in the regenerated chitin suspension, the mass concentration of the regenerated chitin is 0.2-1.2%;
the resulting mixture was dispersed to obtain Pickering (Pickering) emulsion.
As an improvement of the method for preparing Pickering emulsion by using regenerated chitin, the preparation method of the regenerated chitin suspension comprises the following steps in sequence:
adding chitin into phosphoric acid solution with volume concentration of (85 +/-5)% according to a material-liquid ratio of 1g/(50 +/-5) ml, and stirring at a low temperature of (3 +/-1) ° C until the chitin is dissolved;
adding deionized water into the solution obtained in the step I, wherein the obtained precipitate is regenerated chitin;
the deionized water: phosphoric acid solution of step (i) (50 ± 5): 1 in a volume ratio;
repeatedly washing the regenerated chitin obtained in the step II with deionized water until the pH value is constant, and then adding deionized water for dispersing and homogenizing to obtain a regenerated chitin suspension; in the regenerated chitin suspension, the mass concentration of the regenerated chitin is 0.2-1.2%.
As a further improvement of the method for preparing Pickering emulsion by using regenerated chitin, in the step III, a dispersion machine is used for dispersion and homogenization (30 +/-5) min under the condition of (12,000 +/-1000) rpm.
The invention is further improved by the method for preparing Pickering emulsion by using regenerated chitin:
dispersing with ultrasonic cell pulverizer for (2 + -0.5) min.
The invention is further improved by the method for preparing Pickering emulsion by using regenerated chitin:
in the regenerated chitin suspension, the mass concentration of the regenerated chitin is 1.0%.
The invention is further improved by the method for preparing Pickering emulsion by using regenerated chitin: the mass concentration of the oil phase in the mixed solution obtained in the step 1) is 10-30%.
Compared with solid particle emulsifiers such as titanium dioxide, zinc oxide and the like, the chitin has better biocompatibility, belongs to functional biomass materials, is a food-grade material, is nontoxic and harmless to human bodies, has the functions of moisture preservation, oxidation resistance, ultraviolet resistance and the like, and can be directly used as solid particles to stabilize an oil phase to prepare emulsion.
Chitin has high radiation resistance, disinfection, sterilization and oxidation resistance, and is an ideal raw material for hair care, skin care and cosmetics. Chitin has the functions of activating cells, forming films and keeping moisture, can be used for manufacturing high-grade skin care and skin care cosmetics, keeps skin glossy, moist and elastic, can enhance the metabolic function of skin cells, inhibit free radical oxidation, eliminate senile plaque and lipofuscin, inhibit mites, maintain skin injury and the like, prevent rough skin, repair DNA injury, keep skin young, improve the blood flow rate and blood flow volume of the skin and have the advantages which are not possessed by other cosmetic raw materials. In the traditional cosmetic emulsion, a surfactant is often used as an emulsifier, however, part of the surfactant has certain toxicity and certain irritation to eyes and skin of people, and the regenerated chitin is non-toxic, harmless, renewable and excellent in efficacy performance as a biomass material.
The invention uses the regenerated chitin solid particles as the emulsifier to emulsify the oil phase, thereby preparing the emulsion which is stable and not layered and has uniform emulsion drop size distribution.
In conclusion, the regenerated chitin solid particles are used as the emulsifier, so that a series of emulsions with stable emulsions and uniformly dispersed droplet sizes are successfully prepared; namely, the invention uses the regenerated chitin solid particles as the emulsifier to emulsify GTCC to form stable O/W type Pickering emulsion. The method is simple to operate, is easy to control, uses non-toxic, harmless, renewable and biodegradable regenerated chitin as emulsifying particles to replace the traditional surfactant as an emulsifying agent, has low emulsifier dosage, forms emulsion with good stability and uniform dispersion of emulsion droplet size, and simultaneously avoids the environmental problem caused by using a large amount of surfactant.
Drawings
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
FIG. 1 shows the stability of Pickering emulsion emulsified by regenerated chitin suspensions of different concentrations after standing for 0, 7, 30, 90 days at room temperature (the upper graph is the standing condition of the emulsions of examples 1-15 from left to right, and the lower graph is the standing condition of the emulsions of examples 16-30 from left to right);
FIG. 2 is a microscope photograph of Pickering emulsions formed at different concentrations of the regenerated chitin suspension and different oil-water ratios (from left to right, the first row is examples 1-5 from top to bottom, the second row is examples 6-10 from top to bottom, the third row is examples 11-15 from top to bottom, the fourth row is examples 16-20 from top to bottom, the fifth row is examples 21-25 from top to bottom, and the sixth row is examples 26-30 from top to bottom);
FIG. 3 is a graph of the average particle size of Pickering emulsions formed by different concentrations of regenerated chitin suspensions and different oil-water ratios;
the first column from left to right corresponds to example 1, example 6, example 11, example 16, example 21;
the rest of the columns are analogized.
Detailed Description
The invention will be further described with reference to specific examples, but the scope of the invention is not limited thereto:
case 1, a method for preparing a suspension of regenerated chitin, chitin being a powder extracted from shrimp shells; can be prepared according to the methods disclosed in Stabilizing oil-in-water with regenerated peptides from the publications in Food Chemistry.
The following steps are carried out in sequence:
adding 5g of chitin into 250ml of 85% phosphoric acid solution according to the material-liquid ratio of 1g/50ml, and stirring at the low temperature of 3 ℃ until the chitin is dissolved;
adding deionized water into the solution obtained in the step I, wherein the obtained precipitate is regenerated chitin;
the deionized water: the phosphoric acid solution of step (i) is 50: 1 in a volume ratio;
repeatedly washing the regenerated chitin obtained in the step two with deionized water until the pH value is stable, adding deionized water, and dispersing and homogenizing for 30min at 12,000rpm by using a dispersion machine to obtain regenerated chitin suspension; in the regenerated chitin suspension, the mass concentration of the regenerated chitin is 0.2-1.2%.
In the following examples 1 to 30, the ultrasonic treatment was carried out by using an ultrasonic cell disruptor model JY 92-II DN manufactured by Ningbo New Zealand Biotech Co., Ltd. The aqueous phase and the oil phase may be first mixed in a vortex apparatus and then treated ultrasonically.
Example 1
0.7g GTCC was added to a glass bottle containing 6.3g regenerated chitin suspension with a concentration of 0.2 wt%, mixed and sonicated for 2min at 80% pressure amplitude to prepare O/W Pickering emulsion.
Example 2
Adding 1.4g GTCC into a regenerated chitin suspension glass bottle with the concentration of 5.6g being 0.2 wt%, mixing, and carrying out ultrasonic treatment for 2min under the pressure amplitude of 80% to prepare O/W type Pickering emulsion.
Example 3
2.1g GTCC was added into a glass bottle containing 0.2 wt% regenerated chitin suspension containing 4.9g GTCC, and after mixing, the mixture was subjected to ultrasonic treatment for 2min at 80% pressure amplitude to prepare O/W type Pickering emulsion.
Example 4
2.8g GTCC was added into a glass bottle containing 0.2 wt% regenerated chitin suspension containing 4.2g GTCC, and after mixing, the mixture was subjected to ultrasonic treatment for 2min at 80% pressure amplitude to prepare O/W type Pickering emulsion.
Example 5
Adding 3.5g GTCC into a regenerated chitin suspension glass bottle with the concentration of 3.5g being 0.2 wt%, mixing, and carrying out ultrasonic treatment for 2min under the pressure amplitude of 80% to prepare O/W type Pickering emulsion.
Example 6
Adding 0.7g GTCC into a regenerated chitin suspension glass bottle with the concentration of 6.3g being 0.4 wt%, mixing, and carrying out ultrasonic treatment for 2min under the pressure amplitude of 80% to prepare O/W type Pickering emulsion.
Example 7
Adding 1.4g GTCC into a regenerated chitin suspension glass bottle with the concentration of 5.6g being 0.4 wt%, mixing, and carrying out ultrasonic treatment for 2min under the pressure amplitude of 80% to prepare O/W type Pickering emulsion.
Example 8
2.1g GTCC was added into a regenerated chitin suspension glass bottle containing 4.9g 0.4 wt% of chitin, and after mixing, the mixture was subjected to ultrasonic treatment for 2min at 80% pressure amplitude to prepare an O/W Pickering emulsion.
Example 9
2.8g GTCC was added into a glass bottle containing 0.4 wt% regenerated chitin suspension containing 4.2g GTCC, and after mixing, the mixture was subjected to ultrasonic treatment for 2min at 80% pressure amplitude to prepare O/W type Pickering emulsion.
Example 10
Adding 3.5g GTCC into a regenerated chitin suspension glass bottle with the concentration of 3.5g being 0.4 wt%, mixing, and carrying out ultrasonic treatment for 2min under the pressure amplitude of 80% to prepare O/W type Pickering emulsion.
Example 11
Adding 0.7g GTCC into a regenerated chitin suspension glass bottle with the concentration of 6.3g being 0.6 wt%, mixing, and carrying out ultrasonic treatment for 2min under the pressure amplitude of 80% to prepare O/W type Pickering emulsion.
Example 12
Adding 1.4g GTCC into a regenerated chitin suspension glass bottle with the concentration of 5.6 wt%, mixing, and performing ultrasonic treatment for 2min under the pressure amplitude of 80% to prepare O/W type Pickering emulsion.
Example 13
2.1g GTCC was added into a glass bottle containing 0.6 wt% regenerated chitin suspension containing 4.9g GTCC, and after mixing, the mixture was subjected to ultrasonic treatment for 2min at 80% pressure amplitude to prepare O/W type Pickering emulsion.
Example 14
2.8g GTCC was added into a glass bottle containing 0.6 wt% regenerated chitin suspension containing 4.2g GTCC, and after mixing, the mixture was subjected to ultrasonic treatment for 2min at 80% pressure amplitude to prepare O/W type Pickering emulsion.
Example 15
Adding 3.5g GTCC into a regenerated chitin suspension glass bottle with the concentration of 3.5g being 0.6 wt%, mixing, and carrying out ultrasonic treatment for 2min under the pressure amplitude of 80% to prepare O/W type Pickering emulsion.
Example 16
Adding 0.7g GTCC into a regenerated chitin suspension glass bottle with the concentration of 6.3g being 0.8 wt%, mixing, and carrying out ultrasonic treatment for 2min under the pressure amplitude of 80% to prepare O/W type Pickering emulsion.
Example 17
Adding 1.4g GTCC into a regenerated chitin suspension glass bottle with the concentration of 5.6g being 0.8 wt%, mixing, and carrying out ultrasonic treatment for 2min under the pressure amplitude of 80% to prepare O/W type Pickering emulsion.
Example 18
2.1g GTCC was added into a glass bottle containing 0.8 wt% regenerated chitin suspension containing 4.9g GTCC, and after mixing, the mixture was subjected to ultrasonic treatment for 2min at 80% pressure amplitude to prepare O/W type Pickering emulsion.
Example 19
2.8g GTCC was added into a glass bottle containing 0.8 wt% regenerated chitin suspension containing 4.2g GTCC, and after mixing, the mixture was subjected to ultrasonic treatment for 2min at 80% pressure amplitude to prepare O/W type Pickering emulsion.
Example 20
Adding 3.5g GTCC into a regenerated chitin suspension glass bottle with the concentration of 3.5g being 0.8 wt%, mixing, and carrying out ultrasonic treatment for 2min under the pressure amplitude of 80% to prepare O/W type Pickering emulsion.
Example 21
Adding 0.7g GTCC into a regenerated chitin suspension glass bottle with the concentration of 6.3g being 1.0 wt%, mixing, and carrying out ultrasonic treatment for 2min under the pressure amplitude of 80% to prepare O/W type Pickering emulsion.
Example 22
Adding 1.4g GTCC into a regenerated chitin suspension glass bottle with the concentration of 5.6g being 1.0 wt%, mixing, and carrying out ultrasonic treatment for 2min under the pressure amplitude of 80% to prepare O/W type Pickering emulsion.
Example 23
2.1g GTCC was added into a glass bottle containing a regenerated chitin suspension of 4.9g 1.0 wt%, mixed, and subjected to ultrasonic treatment for 2min at a pressure amplitude of 80% to prepare an O/W Pickering emulsion.
Example 24
2.8g GTCC was added to a glass bottle containing a regenerated chitin suspension of 4.2g 1.0 wt%, mixed and sonicated for 2min at 80% pressure amplitude to prepare an O/W Pickering emulsion.
Example 25
Adding 3.5g GTCC into a regenerated chitin suspension glass bottle with the concentration of 3.5g being 1.0 wt%, mixing, and carrying out ultrasonic treatment for 2min under the pressure amplitude of 80% to prepare O/W type Pickering emulsion.
Example 26
Adding 0.7g GTCC into a regenerated chitin suspension glass bottle with the concentration of 6.3g being 1.2 wt%, mixing, and carrying out ultrasonic treatment for 2min under the pressure amplitude of 80% to prepare O/W type Pickering emulsion.
Example 27
Adding 1.4g GTCC into a regenerated chitin suspension glass bottle with the concentration of 5.6g being 1.2 wt%, mixing, and carrying out ultrasonic treatment for 2min under the pressure amplitude of 80% to prepare O/W type Pickering emulsion.
Example 28
2.1g GTCC was added into a glass bottle containing a regenerated chitin suspension of 4.9g 1.2 wt%, mixed, and subjected to ultrasonic treatment for 2min at a pressure amplitude of 80% to prepare an O/W Pickering emulsion.
Example 29
2.8g GTCC was added into a glass bottle containing a regenerated chitin suspension of 4.2g 1.2 wt%, mixed, and subjected to ultrasonic treatment for 2min at a pressure amplitude of 80% to prepare an O/W Pickering emulsion.
Example 30
Adding 3.5g GTCC into a regenerated chitin suspension glass bottle with the concentration of 3.5g being 1.2 wt%, mixing, and carrying out ultrasonic treatment for 2min under the pressure amplitude of 80% to prepare O/W type Pickering emulsion.
The stability test was carried out according to the static method in examples 1 to 30, and the results are shown in FIG. 1; from fig. 1, the following conclusive conclusions can be drawn: as can be seen from figure 1, when the concentration of the regenerated chitin suspension is low, the emulsion is easy to delaminate, because the dosage of the stabilizer is small, the physical stability of the emulsion is poor, and a certain density difference exists between oil and water phases, the deionized water is settled under the action of gravity, and a water layer appears. The layering is relieved with the increase of the concentration of the regenerated chitin suspension, because the emulsion has stronger stability with the increase of the dosage of the regenerated chitin. Under the condition of the same concentration of the regenerated chitin suspension, the layering condition of the emulsion is less and less obvious along with the increase of the mass fraction of the oil phase. Apart from the appearance of the aqueous layer, the emulsion showed no further instability.
On the 30 th day of standing, each sample had different degrees of delamination. Example 30 water layer separation was minimal.
The results of the microscopic examination of the emulsion using an optical microscope in examples 1 to 30 are shown in FIG. 2; from fig. 2, the following conclusive conclusions can be drawn: along with the increase of the oil phase, the particle size of emulsion droplets under the same concentration of the regenerated chitin suspension is also obviously increased. With the increase of the concentration of the regenerated chitin suspension, the particle size of emulsion droplets with the same oil phase mass fraction is reduced, the particle size of emulsion droplets formed by the regenerated chitin suspension with the concentration of 0.2 wt% is obviously larger than that of emulsion droplets formed by other concentrations, and the particle size of emulsion droplets stabilized by the regenerated chitin suspension with the concentration of 0.4 wt% -1.2 wt% has a tendency of gradually reducing but is not obviously changed. It is probably because the viscosity of the emulsion becomes higher and the efficiency of homogeneous dispersion of the emulsion is lowered when the concentration of the regenerated chitin is increased. The emulsion droplets formed in each ratio are regularly spherical and have a uniform size distribution.
The average particle size of emulsion droplets was measured using a laser particle size analyzer in examples 1 to 30, and the results are shown in fig. 3; from fig. 3, the following conclusive conclusions can be drawn: along with the increase of the concentration of the regenerated chitin suspension, the particle size of the emulsion droplets is smaller and gradually tends to be stable, the particle sizes of the Pickering emulsion droplets with the stable suspension with the concentration of 1.0 wt% and the stable suspension with the concentration of 1.2 wt% are almost the same, and meanwhile, the larger the specific gravity of GTCC is, the larger the particle size of the emulsion droplets is.
The three graphs are combined to obtain that when the concentration of the regenerated chitin reaches 1.0 wt%, the stability and the particle size of the emulsion show similar results along with the increase of the concentration of the regenerated chitin. Furthermore, the fluidity of the emulsion is deteriorated as the amount of the regenerated chitin is increased, so that the regenerated chitin with the concentration of 1.0 wt% is the optimal amount of the solid particles in the emulsion system.
In the course of the invention, the inventors also carried out the following comparative experiments: directly adding deionized water into chitin according to the step III of the example 1 for dispersing and homogenizing for 30min to obtain chitin suspension; the emulsion preparation as described in examples 1 to 30 was carried out by using this chitin suspension instead of the regenerated chitin suspension, and as a result, it was found that: the stability under the same conditions is far less than that of the present invention.
Finally, it is also noted that the above-mentioned lists merely illustrate a few specific embodiments of the invention. It is obvious that the invention is not limited to the above embodiments, but that many variations are possible. All modifications which can be derived or suggested by a person skilled in the art from the disclosure of the present invention are to be considered within the scope of the invention.
Claims (6)
1. The method for preparing Pickering emulsion by using regenerated chitin is characterized by comprising the following steps:
mixing the water phase and the oil phase by taking the regenerated chitin suspension as the water phase and GTCC as the oil phase, wherein the mass concentration of the oil phase in the obtained mixed solution is 10-50%;
in the regenerated chitin suspension, the mass concentration of the regenerated chitin is 0.2-1.2%;
dispersing the obtained mixed solution to obtain Pickering emulsion.
2. The method for preparing Pickering emulsion by using regenerated chitin according to claim 1, wherein the preparation method of the regenerated chitin suspension comprises the following steps in sequence:
adding chitin into phosphoric acid solution with volume concentration of (85 +/-5)% according to a material-liquid ratio of 1g/(50 +/-5) ml, and stirring at a low temperature of (3 +/-1) ° C until the chitin is dissolved;
adding deionized water into the solution obtained in the step I, wherein the obtained precipitate is regenerated chitin;
the deionized water: phosphoric acid solution of step (i) (50 ± 5): 1 in a volume ratio;
repeatedly washing the regenerated chitin obtained in the step II with deionized water until the pH value is constant, and then adding deionized water for dispersing and homogenizing to obtain a regenerated chitin suspension; in the regenerated chitin suspension, the mass concentration of the regenerated chitin is 0.2-1.2%.
3. The method for preparing Pickering emulsion by using regenerated chitin according to claim 2, wherein: in the third step, a dispersion machine is used for dispersion and homogenization (30 +/-5) min under the condition of (12,000 +/-1000) rpm.
4. The method for preparing Pickering emulsion by using regenerated chitin according to any one of claims 1-3, wherein the method comprises the following steps:
dispersing with ultrasonic cell pulverizer for (2 + -0.5) min.
5. The method for preparing Pickering emulsion by using regenerated chitin according to claim 4, wherein:
in the regenerated chitin suspension, the mass concentration of the regenerated chitin is 1.0%.
6. The method for preparing Pickering emulsion by using regenerated chitin according to claim 5, wherein: the mass concentration of the oil phase in the mixed solution obtained in the step 1) is 10-30%.
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| CN113527712A (en) * | 2021-06-17 | 2021-10-22 | 广州大学 | Corn peptide-microcrystalline chitin compound and preparation method of double pickering emulsion thereof |
| CN115517339A (en) * | 2022-09-22 | 2022-12-27 | 河南南街村清真食品有限公司 | Preparation and controlled-release method of low-viscosity emulsion coagulant suitable for bean curd processing |
| CN115678041A (en) * | 2022-11-21 | 2023-02-03 | 东北林业大学 | Preparation method of nano chitin-based environmental change resistant HIPPES (chitin pentapeptides) |
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2019
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| YONGMEI XIAO等: "In Vitro Digestion of Oil-in-Water Emulsions Stabilized by Regenerated Chitin", 《JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY》 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113527712A (en) * | 2021-06-17 | 2021-10-22 | 广州大学 | Corn peptide-microcrystalline chitin compound and preparation method of double pickering emulsion thereof |
| CN113527712B (en) * | 2021-06-17 | 2023-07-07 | 广州大学 | Corn peptide-microcrystalline chitin compound and preparation method of double pickering emulsion thereof |
| CN115517339A (en) * | 2022-09-22 | 2022-12-27 | 河南南街村清真食品有限公司 | Preparation and controlled-release method of low-viscosity emulsion coagulant suitable for bean curd processing |
| CN115678041A (en) * | 2022-11-21 | 2023-02-03 | 东北林业大学 | Preparation method of nano chitin-based environmental change resistant HIPPES (chitin pentapeptides) |
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Application publication date: 20191220 |