CN116098832A - Ascorbyl tetraisopalmitate lyotropic liquid crystal nanoparticle dispersion, preparation method and application thereof, and toning lotion - Google Patents

Ascorbyl tetraisopalmitate lyotropic liquid crystal nanoparticle dispersion, preparation method and application thereof, and toning lotion Download PDF

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CN116098832A
CN116098832A CN202310173488.7A CN202310173488A CN116098832A CN 116098832 A CN116098832 A CN 116098832A CN 202310173488 A CN202310173488 A CN 202310173488A CN 116098832 A CN116098832 A CN 116098832A
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liquid crystal
lyotropic liquid
ascorbyl tetraisopalmitate
nanoparticle dispersion
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邹爱华
高宁
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Shanghai Normal University
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Abstract

The invention belongs to the technical field of carrier systems in cosmetic preparation, and particularly relates to a tetraisopalmitate ascorbate lyotropic liquid crystal nanoparticle dispersion, a preparation method and application thereof, and a toning lotion. The invention provides a ascorbyl tetraisopalmitate lyotropic liquid crystal nanoparticle dispersion, which is prepared from ascorbyl tetraisopalmitate, grease, an emulsifier and a stabilizer aqueous solution, and the invention solves the problem of low solubility of the VC-IP by encapsulating the ascorbyl tetraisopalmitate (VC-IP) in the lyotropic liquid crystal nanoparticle, improves the stability of the VC-IP in the aqueous solution, and simultaneously, the ascorbyl tetraisopalmitate lyotropic liquid crystal nanoparticle in the dispersion has a lipid bilayer structure, is similar to a cell membrane structure, and can promote the absorption of active ingredients And the release speed of VC-IP can be controlled, so that the bioavailability is increased.

Description

Ascorbyl tetraisopalmitate lyotropic liquid crystal nanoparticle dispersion, preparation method and application thereof, and toning lotion
Technical Field
The invention belongs to the technical field of carrier systems in cosmetic preparation, and particularly relates to a tetraisopalmitate ascorbate lyotropic liquid crystal nanoparticle dispersion, a preparation method and application thereof, and a toning lotion.
Background
Ascorbyl tetraisopalmitate (Ascorbyl Tetraisopalmitate, VC-IP) is a fat-soluble derivative of vitamin C, is colorless or pale yellow liquid, is insoluble in water, and has a structural formula shown in formula I. VC-IP has the effects of whitening skin, removing spots, promoting collagen growth and the like, is commonly used as an antioxidant and is applied to a cosmetic skin care product.
Figure BDA0004099988500000011
At present, when VC-IP is applied to cosmetics, most products are products with very high oiliness such as essence, face cream and the like, and the formula has the defects of oily skin feel, difficult absorption and the like. The VC-IP is a fat-soluble compound, is difficult to dissolve in water, is easily oxidized in water, cannot be converted into vitamin C to play an antioxidant role, and cannot be directly applied to water-based products.
Disclosure of Invention
The invention aims at solving the existing problems and provides an ascorbyl tetraisopalmitate lyotropic liquid crystal nanoparticle dispersion, a preparation method and application thereof, and a toning lotion. The ascorbyl tetraisopalmitate lyotropic liquid crystal nanoparticle dispersion provided by the invention increases the solubility of VC-IP in water, improves the stability of VC-IP in water solution, is not easy to oxidize, and can be directly used for preparing toning lotion.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides an ascorbyl tetraisopalmitate lyotropic liquid crystal nanoparticle dispersion which is prepared from the following raw materials in parts by weight: ascorbyl tetraisopalmitate, a lyotropic liquid crystal carrier and an aqueous stabilizer solution; the lyotropic liquid crystal carrier comprises grease and an emulsifying agent; the mass ratio of the ascorbyl tetraisopalmitate to the grease is 1-10:10.
Preferably, the grease comprises one or more of cetyl palmitate, glycerol monolaurate, glyceryl behenate, glyceryl distearate, glycerol monooleate, glycerol monostearate, monoglyceride succinate, glyceryl caprylate, monoglyceride oleate, propylene glycol monostearate, propylene glycol monooleate, propylene glycol monolaurate, sweet almond oil, hazelnut oil, soybean oil, olive oil and grape seed oil.
Preferably, the emulsifier comprises one or more of decyl glucoside, lauryl glucoside, sucrose monostearate, cetyl palmitate, tween 80 and coco glucoside.
Preferably, the stabilizer in the aqueous solution of the stabilizer comprises one or more of carbomer, sodium alginate, hyaluronic acid, magnesium stearate, xanthan gum and calcium stearate.
The invention also provides a preparation method of the ascorbyl tetraisopalmitate lyotropic liquid crystal nanoparticle dispersion, which comprises the following steps:
mixing ascorbyl tetraisopalmitate, an emulsifier and grease to obtain a grease mixture;
emulsifying the oil mixture and a stabilizer aqueous solution to obtain nanoparticle colostrum;
and dispersing the nanoparticle colostrum to obtain the ascorbyl tetraisopalmitate lyotropic liquid crystal nanoparticle dispersion.
Preferably, the ratio of the oil mixture to the aqueous stabilizer solution is 1-10 g/50 mL, and the concentration of the stabilizer in the aqueous stabilizer solution is 0.1-3 wt%.
Preferably, the emulsifying mode comprises shearing, wherein the rotating speed of the shearing is 6000-12000 rpm, and the time is 1-10 min.
Preferably, the dispersing mode comprises homogenizing, wherein the homogenizing pressure is 400-1000 bar, and the times are 3-9 times.
The invention also provides application of the ascorbyl tetraisopalmitate lyotropic liquid crystal nanoparticle dispersion in toning lotion.
The invention also provides a toning lotion which comprises the following components in percentage by mass: 1-3% of ascorbyl tetraisopalmitate lyotropic liquid crystal nanoparticle dispersion, 80-93.37% of water, 0.03-1% of chelating agent, 0.3-0.1% of anti-inflammatory agent, 5-15% of humectant and 0.3-1% of preservative, wherein the ascorbyl tetraisopalmitate lyotropic liquid crystal nanoparticle dispersion is the ascorbyl tetraisopalmitate lyotropic liquid crystal nanoparticle dispersion according to the technical scheme or the ascorbyl tetraisopalmitate lyotropic liquid crystal nanoparticle dispersion obtained by the preparation method.
The invention provides an ascorbyl tetraisopalmitate lyotropic liquid crystal nanoparticle dispersion, which is prepared from ascorbyl tetraisopalmitate, grease, an emulsifier and a stabilizer aqueous solution.
The invention also provides a preparation method of the ascorbyl tetraisopalmitate lyotropic liquid crystal nanoparticle dispersion, which is simple and easy to implement, wherein the ascorbyl tetraisopalmitate lyotropic liquid crystal nanoparticle has uniform particle size, the particle size range is 80-200 nm, and the dispersion is good, and the method is suitable for industrial mass production.
The invention also provides application of the ascorbyl tetraisopalmitate lyotropic liquid crystal nanoparticle dispersion in the toning lotion, and the ascorbyl tetraisopalmitate lyotropic liquid crystal nanoparticle dispersion can be directly used as a raw material of cosmetics to prepare the toning lotion, is comfortable in skin feel and good in biocompatibility, does not have layering or precipitation after being subjected to stability test, and has good stability.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a flow chart of a preparation process of the toning lotion of the present invention;
FIG. 2 is a graph showing the chemical stability of VC-IP lyotropic liquid crystal nanoparticles of example 1;
FIG. 3 is an electron microscope image of lyotropic liquid crystal nanoparticles, wherein a) is blank lyotropic liquid crystal nanoparticles, b) is VC-IP lyotropic liquid crystal nanoparticles of example 1;
FIG. 4 is a freshly prepared toning lotion in example 1;
FIG. 5 is a view of the lotion after being left at room temperature for thirty days;
FIG. 6 is a view of the lotion after thirty days of oven high temperature placement at 50 ℃;
FIG. 7 shows the lotion after being left at a low temperature of 4℃for thirty days;
FIG. 8 shows the lotion after freeze-thaw cycle.
Detailed Description
The invention provides an ascorbyl tetraisopalmitate lyotropic liquid crystal nanoparticle dispersion which is prepared from the following raw materials in parts by weight: ascorbyl tetraisopalmitate, a lyotropic liquid crystal carrier and an aqueous stabilizer solution; the lyotropic liquid crystal carrier comprises grease and an emulsifying agent; the mass ratio of the ascorbyl tetraisopalmitate to the grease is 1-10:10.
In the present invention, all materials used are commercial products in the art unless otherwise specified.
In the invention, the mass ratio of the ascorbyl tetraisopalmitate to the grease is preferably 5-10:10.
In the present invention, the grease preferably comprises one or more of cetyl palmitate, glycerol monolaurate, glyceryl behenate, glyceryl distearate, glyceryl monooleate, glyceryl monostearate, monoglyceride succinate, glyceryl caprylate, monoglyceride oleate, propylene glycol monostearate, propylene glycol monooleate, propylene glycol monolaurate, sweet almond oil, hazelnut oil, soybean oil, olive oil and grapeseed oil; more preferably a mixture of glycerol monostearate and hazelnut oil, a mixture of glycerol monostearate and olive oil, or a mixture of glycerol monostearate and soybean oil, wherein the mass ratio of glycerol monostearate to hazelnut oil in the mixture of glycerol monostearate and hazelnut oil is preferably 500:500, the mass ratio of glycerol monostearate to olive oil in the mixture of glycerol monostearate and olive oil is preferably 500:500, and the mass ratio of glycerol monostearate to soybean oil in the mixture of glycerol monostearate and soybean oil is preferably 500:500.
In the present invention, the emulsifier preferably includes one or more of decyl glucoside, lauryl glucoside, sucrose monostearate, cetyl palmitate, tween 80 and coco glucoside, more preferably lauryl glucoside, coco glucoside or cetyl palmitate.
In the present invention, the mass ratio of the grease to the emulsifier is preferably 1000:150.
In the present invention, the stabilizer in the aqueous stabilizer solution preferably includes one or more of carbomer, sodium alginate, hyaluronic acid, magnesium stearate, xanthan gum and calcium stearate.
In the invention, the particle size of the ascorbyl tetraisopalmitate lyotropic liquid crystal nanoparticles in the ascorbyl tetraisopalmitate lyotropic liquid crystal nanoparticle dispersion is preferably 80-200 nm.
The invention also provides a preparation method of the ascorbyl tetraisopalmitate lyotropic liquid crystal nanoparticle dispersion, which comprises the following steps:
mixing ascorbyl tetraisopalmitate, an emulsifier and grease to obtain a grease mixture;
emulsifying the oil mixture and a stabilizer aqueous solution to obtain nanoparticle colostrum;
and dispersing the nanoparticle colostrum to obtain the ascorbyl tetraisopalmitate lyotropic liquid crystal nanoparticle dispersion.
The invention mixes the ascorbyl tetraisopalmitate, the emulsifier and the grease to obtain the grease mixture.
In the present invention, the mass ratio of the ascorbyl tetraisopalmitate to the fat is preferably 1 to 10:10, more preferably 5 to 10:10.
In the present invention, the temperature of the mixing is preferably 40 to 70 ℃, more preferably 60 ℃, and the manner of maintaining the temperature of the mixing is preferably a thermostatic water bath.
After the oil and fat mixture is obtained, the oil and fat mixture and the aqueous solution of the stabilizing agent are emulsified to obtain the nanoparticle colostrum.
In the present invention, the oil-and-fat mixture is preferably first mixed with the aqueous stabilizer solution and then emulsified. The temperature of the aqueous stabilizer solution is preferably the same as the temperature of the fat and oil mixture when the first mixing is performed, and the temperature of the first mixing is preferably 40 to 70 ℃, more preferably 60 ℃.
In the present invention, the ratio of the fat/oil mixture to the aqueous stabilizer solution is preferably 1 to 10 g/50 mL, more preferably 1.65 to 2.15 g/50 mL, and the concentration of the stabilizer in the aqueous stabilizer solution is preferably 0.1 to 3wt%.
In the present invention, the emulsification means preferably includes shearing at a rotation speed of 6000 to 12000rpm, more preferably 10000rpm, and a time of preferably 1 to 10min. The shear rate can enable the oil phase and the water phase to be rapidly emulsified to form nanoparticle colostrum.
After nanoparticle colostrum is obtained, the nanoparticle colostrum is dispersed to obtain the ascorbyl tetraisopalmitate lyotropic liquid crystal nanoparticle dispersion.
In the present invention, the dispersing means preferably includes homogenization, and the pressure of the homogenization is preferably 400 to 1000bar, more preferably 750bar, and the number of times is preferably 3 to 9, more preferably 6. The homogenization pressure and the times can lead the particle size of the nanoparticle colostrum to be more uniform, and improve the dispersibility of the nanoparticles.
The preparation method of the ascorbyl tetraisopalmitate lyotropic liquid crystal nanoparticle dispersion is simple, and the prepared ascorbyl tetraisopalmitate lyotropic liquid crystal nanoparticle has uniform particle size and good dispersibility, and is suitable for mass production. The ascorbate tetraisopalmitate lyotropic liquid crystal nanoparticle prepared by the invention has a lipid bilayer structure. According to the electron microscope image in the embodiment, the nanoparticles are all of vesicle structures, long chains of VC-IP and an oil phase are self-assembled to promote the structure to change, and the VC-IP is successfully loaded into a carrier.
The invention also provides application of the ascorbyl tetraisopalmitate lyotropic liquid crystal nanoparticle dispersion in toning lotion.
The invention also provides a toning lotion which comprises the following components in percentage by mass: 1 to 3 percent of ascorbyl tetraisopalmitate lyotropic liquid crystal nanoparticle dispersion, 80 to 93.37 percent of water, 0.03 to 1 percent of chelating agent, 0.3 to 0.1 percent of anti-inflammatory agent, 5 to 15 percent of humectant and 0.3 to 1 percent of preservative, wherein the ascorbyl tetraisopalmitate lyotropic liquid crystal nanoparticle dispersion is the ascorbyl tetraisopalmitate lyotropic liquid crystal nanoparticle dispersion according to the technical scheme.
In the invention, the mass fraction of the ascorbyl tetraisopalmitate lyotropic liquid crystal nanoparticle dispersion in the cosmetic water is preferably 2-3%.
In the invention, the mass fraction of water in the toning lotion is preferably 83-89%.
In the present invention, the chelating agent in the cosmetic water is preferably 0.05 to 0.07% by mass.
In the present invention, the chelating agent preferably includes one or more of diethanolamine, sorbitol, EDTA-2Na, carboxymethyl chitosan and citric acid monohydrate.
In the invention, the mass fraction of the anti-inflammatory agent in the toning lotion is preferably 0.3-0.5%.
In the present invention, the anti-inflammatory agent preferably includes one or more of dipotassium glycyrrhizinate, allantoin, aloe vera extract, calendula extract, curcumin and bisabolol.
In the invention, the mass fraction of the humectant in the toning lotion is preferably 8-12%.
In the present invention, the humectant preferably includes one or more of glycerin, butylene glycol, polyethylene glycol, propylene glycol, xylitol, sodium lactate, sodium hyaluronate and panthenol, more preferably a mixture of glycerin and propylene glycol, and the mass ratio of glycerin to propylene glycol in the mixture of glycerin and propylene glycol is preferably 3-7:5, more preferably 5:5.
In the present invention, the mass fraction of the preservative in the cosmetic water is preferably 0.5%.
In the present invention, the preservative preferably includes one or more of phenoxyethanol, benzyl alcohol, propylparaben, pentanediol, and hexanediol.
In the present invention, the toning lotion is preferably prepared by a method comprising the steps of:
carrying out second mixing on the ascorbyl tetraisopalmitate lyotropic liquid crystal nanoparticle dispersion and water to obtain a phase A;
thirdly mixing the chelating agent, the anti-inflammatory agent and the humectant to obtain a phase B;
and (3) fourth mixing the phase A and the phase B, and then fifth mixing with a preservative (phase C) to obtain the toning lotion.
The manner of the second mixing and the third mixing is not particularly limited in the present invention, and may be any manner known to those skilled in the art.
In the present invention, the volume ratio of the A phase to the B phase is preferably 6 to 10:1 to 4.
In the present invention, the mass ratio of the A phase to the B phase is preferably 88.95:10.55.
In the present invention, the fourth and fifth mixing means are preferably magnetic stirring, the magnetic stirring is preferably performed at normal temperature, the rotation speed of the magnetic stirring is independently preferably 200 to 500rpm, more preferably 400rpm, and the time is independently preferably 10 to 60min, more preferably 20 to 30min.
After the toning lotion is obtained, the invention preferably further comprises a finished product canning mode, the invention has no special requirement on the finished product canning mode, and the toning lotion can be prepared by adopting a mode well known to a person skilled in the art, and a preparation process flow chart of the toning lotion is shown in figure 1.
The cosmetic water contains the ascorbyl tetraisopalmitate lyotropic liquid crystal nanoparticles, the water content of the VC-IP lyotropic liquid crystal nanoparticle dispersion reaches more than 85 percent, and the cosmetic water has the effects of whitening and moisturizing.
For further explanation of the present invention, the ascorbyl tetraisopalmitate lyotropic liquid crystal nanoparticle dispersion, the preparation method and application thereof, and the cosmetic water provided by the present invention are described in detail below with reference to the accompanying drawings and examples, but they should not be construed as limiting the scope of the present invention.
Example 1
1. Mixing 500mg glycerol monostearate, 500mg hazelnut oil and 150mg lauryl glucoside uniformly in water bath at 60deg.C, adding 1000mg VC-IP, and mixing with oil in water bath at 60deg.C to obtain oil mixture.
2. The lipid mixture was mixed with 50mL of 0.1wt% aqueous hyaluronic acid at 60℃and sheared at high speed at 10000rpm for 1min to obtain nanoparticle colostrum.
3. Pouring the nanoparticle colostrum into a material cup of a high-pressure homogenizer, and circulating for 6 times under the pressure of 750bar to obtain the VC-IP lyotropic liquid crystal nanoparticle dispersoid.
4. According to the formula of the cosmetic water in Table 1, magnetically stirring the phase A and the phase B at normal temperature and 400rpm for 30min, adding phenoxyethanol (phase C) into the system, magnetically stirring at normal temperature for 30min, and uniformly mixing the cosmetic water to obtain the VC-IP lyotropic liquid crystal nanoparticle cosmetic water.
Table 1 example 1 lotion formulation
Figure BDA0004099988500000071
Example 2
1. Mixing 500g of glycerol monostearate, 500g of olive oil and 150g of coco glucoside uniformly in a water bath at 60 ℃, adding 500g of VC-IP, and mixing with grease in the water bath at 60 ℃ to obtain a grease mixture.
2. The fat mixture was mixed with 50L of 0.1wt% sodium alginate aqueous solution (containing 50g of sodium alginate) at the same temperature, and sheared at a high speed of 10000rpm for 1min, to obtain nanoparticle colostrum.
The subsequent preparation was the same as in example 1.
The formula and the preparation method of the VC-IP lyotropic liquid crystal nanoparticle cosmetic water are the same as those of the example 1.
Example 3
1. Mixing 500g of glycerol monostearate, 500g of soybean oil and 150g of cetyl palmitate uniformly in a water bath at 60 ℃, adding 1000g of VC-IP, and mixing with grease in the water bath at 60 ℃ to obtain a grease mixture.
2. The fat mixture was mixed with 50L of a 0.1wt% magnesium stearate aqueous solution (50 g containing magnesium stearate) at the same temperature, and sheared at a high speed of 10000rpm for 1min, to obtain nanoparticle colostrum.
The subsequent preparation was the same as in example 1.
The formula and the preparation method of the VC-IP lyotropic liquid crystal nanoparticle cosmetic water are the same as those of the example 1.
Test example 1
Table 2 shows the particle size of the ascorbyl tetraisopalmitate lyotropic liquid crystal nanoparticles in the VC-IP lyotropic liquid crystal nanoparticle dispersions of examples 1 to 3.
TABLE 2 particle size of the ascorbyl tetraisopalmitate lyotropic liquid Crystal nanoparticles in examples 1 to 3
Examples Example 1 Example 2 Example 3
Particle size (nm) 152.5 157.7 173.2
As can be seen from Table 2, the particle size of the ascorbyl tetraisopalmitate lyotropic liquid crystal nanoparticles is in the range of 80-200 nm, and the particle size of the ascorbyl tetraisopalmitate lyotropic liquid crystal nanoparticles in the VC-IP lyotropic liquid crystal nanoparticle dispersion of example 1 is the smallest, and is more suitable for transdermal and absorption of the nanoparticles.
Example 4
The raw material composition and the preparation method of the VC-IP lyotropic liquid crystal nanoparticle dispersion are the same as in example 1.
The VC-IP lyotropic liquid crystal nanoparticle toning lotion comprises the following raw materials:
allantoin is used as an anti-inflammatory agent, the addition amount is 0.5% of the mass of the toning lotion, EDTA-2Na is used as a chelating agent, and the addition amount is 0.05% of the mass of the toning lotion; glycerin and propylene glycol are used as moisturizers, and the addition amounts are respectively 3% and 5% of the mass of the toning lotion; the phenoxyethanol is used as a preservative, the addition amount is 0.5% of the mass of the toning lotion, and the balance is water. The method for preparing the toning lotion is the same as in example 1.
Example 5
The raw material composition and the preparation method of the VC-IP lyotropic liquid crystal nanoparticle dispersion are the same as in example 1.
The VC-IP lyotropic liquid crystal nanoparticle toning lotion comprises the following raw materials:
allantoin is used as anti-inflammatory agent, and the addition amount is 0.5% of the quality of the toning lotion; EDTA-2Na is used as a chelating agent, and the addition amount is 0.05% of the mass of the toning lotion; glycerin and propylene glycol are used as moisturizers, and the addition amounts are respectively 7% and 5% of the mass of the toning lotion; the phenoxyethanol is used as a preservative, the addition amount is 0.5% of the mass of the toning lotion, and the balance is water. The method for preparing the toning lotion is the same as in example 1.
Test example 2
The moisture retention testing method comprises the following steps: the breathable adhesive tape with the length of 20-30 cm is stuck on a glass plate, and the weight of the breathable adhesive tape is called M0. 0.15g of a toning lotion sample (M sample) was weighed, uniformly smeared on a breathable adhesive tape, placed in a constant temperature dryer for 24 hours, taken out and weighed as M1, and the moisture retention was calculated according to formula II, and the results are shown in Table 3.
Figure BDA0004099988500000091
TABLE 3 variation of moisture retention of lotions of various examples
Examples Example 1 Example 4 Example 5
Moisture retention (%) 14.93 12.32 10.59
The glycerol contains a plurality of hydroxyl groups in the molecular structure, so that the glycerol can absorb moisture with one time of the volume of the glycerol and has good moisturizing performance. And (3) taking the moisturizing rate as a standard, screening the final content of the glycerol, and under the condition that the content of other components is not changed and the content of the glycerol is only changed, when the mass content of the glycerol in the toning lotion is 5%, the moisturizing rate of the toning lotion is the maximum.
Test example 3 chemical stability determination
An aqueous VC-IP solution having a concentration of 100ppm was prepared and the VC-IP lyotropic liquid crystal nanoparticle dispersion prepared in example 1 was diluted to contain an aqueous solution having a concentration of 100ppm of VC-IP (VC-IP LCNPs). Sealing the sample in a transparent penicillin bottle, placing the sample in a room temperature condition, measuring the absorbance of the sample by an ultraviolet-visible spectrophotometer on the first day, the seventh day, the fifteenth day and the thirty th day respectively to obtain the content change of VC-IP at different times, and comparing the difference of the stability of VC-IP load in solute liquid crystal nano particles and pure VC-IP in aqueous solution, wherein the chemical stability result is shown in figure 2.
As shown in FIG. 2, the solubility of VC-IP in water is low, and the VC-IP can be oxidized rapidly within 4 hours, so that the content of VC-IP is reduced rapidly, and the solubility and stability of VC-IP coated by the lyotropic liquid crystal nanoparticles in water are improved greatly, which means that the VC-IP is well protected after being loaded on the lyotropic liquid crystal nanoparticles, the stability in water is improved, and the utilization rate and the storage rate of the VC-IP are improved obviously.
Test example 4 physical stability determination
Stability of VC-IP lyotropic liquid crystal nanoparticles
1) Centrifugal stability
2mL of the freshly prepared VC-IP lyotropic liquid crystal nanoparticle dispersion in example 1 is taken and placed in a 10mL centrifuge tube, and centrifuged at 25 ℃ for 0min, 10min, 20 min, 30min and 40min respectively, the centrifugation speed is 4000rpm, and the state of the centrifuged sample is observed. If not provided withWhen layering occurs, the average particle size and PDI are measured, and the centrifugal stability parameter K is calculated E The centrifugal stability was evaluated, the formula is shown in formula III, and the result of the centrifugal stability is shown in Table 4.
Figure BDA0004099988500000101
Wherein R is 0 The particle size before centrifugation, and R is the particle size after centrifugation.
Table 4 centrifugal stability results
Time (min) Particle size (nm) PDI K E (%) Status of
0 126.0 0.16 --- Not layered
10 126.7 0.15 0.58 Not layered
20 129.0 0.14 2.41 Not layered
30 127.0 0.13 0.83 Not layered
40 125.1 0.13 0.65 Not layered
The VC-IP lyotropic liquid crystal nanoparticles have no layering or precipitation phenomenon under the conditions of the same rotating speed and different centrifugation time, the particle size and PDI have no obvious change, and the centrifugation stability parameter K E The VC-IP lyotropic liquid crystal nanoparticles in the VC-IP lyotropic liquid crystal nanoparticle dispersion have good stability, and the VC-IP lyotropic liquid crystal nanoparticles are maintained below 5%.
2) Freeze thawing stability
The VC-IP lyotropic liquid crystal nanoparticle dispersion of example 1 was placed at-20 ℃ to take out samples at intervals of 0, 0.5, 1, 1.5 and 2 hours, and the samples were thawed at room temperature, and the average particle size and PDI value of the thawed samples frozen for different times were measured, and the results are shown in Table 5.
TABLE 5 freeze-thaw stability results
Time (h) Particle size (nm) PDI
0 148.6 0.2
0.5 147.5 0.2
1 145.0 0.2
1.5 144.1 0.2
2 142.2 0.2
As can be seen from Table 5, under different freeze thawing times, the particle size and PDI of the VC-IP lyotropic liquid crystal nanoparticles are not changed significantly, which indicates that the VC-IP lyotropic liquid crystal nanoparticles can be stored in an environment of-20 ℃ for a short period of time without affecting the stability of the sample. The result of combining centrifugal stability shows that the VC-IP lyotropic liquid crystal nanoparticles have good stability and can be used as raw materials of cosmetics to be added into the cosmetics.
3) Freezing etching electron microscope experiment (Cryo-TEM)
The VC-IP lyotropic liquid crystal nanoparticle dispersion of example 1 was dropped on a copper mesh, the copper mesh with the dropped sample was rapidly immersed in liquid ethane at-180 ℃, vitrified, and then stored in liquid nitrogen, and the sample was observed and photographed using a 200KV transmission electron microscope.
The electron microscope image of the blank lyotropic liquid crystal nanoparticle carrier is a nanoparticle with an obvious cauliflower-shaped structure, as shown in a) in fig. 3, belongs to the classical morphology of a sponge phase, and simultaneously has a plurality of smaller vesicle structures dispersed at the periphery, which indicates that the blank carrier is a system in which the sponge phase and vesicles coexist. The nanoparticles in the frozen electron microscope image of the VC-IP lyotropic liquid crystal nanoparticles are all vesicle structures, as shown in b) in fig. 3, and the fact that the self-assembly of long chains of VC-IP and an oil phase causes the structure to change is considered, which also proves that the VC-IP is successfully loaded into the carrier.
Stability of VC-IP lyotropic liquid crystal nanoparticle cosmetic water
1) Storage stability
The toning lotion prepared in example 1 was placed in an oven at normal temperature and 50 ℃ and a low-temperature environment at 4 ℃ respectively, and whether the appearance of the sample was changed or not and whether delamination occurred or not was observed after thirty days.
2) Freeze thawing cycle stability
The toning lotion prepared in example 1 was placed in a 50 ℃ oven, taken out after 12 hours, placed in a 4 ℃ refrigerator, placed in a 50 ℃ oven after 12 hours, repeated 3 times, and the sample was returned to room temperature to see if it delaminated.
Fig. 4 is a freshly prepared lotion in example 1, fig. 5 is a lotion after being left at normal temperature for thirty days, fig. 6 is a lotion after being left at an oven at 50 ℃ for thirty days, fig. 7 is a lotion after being left at a low temperature of 4 ℃ for thirty days, and fig. 8 is a lotion after freeze thawing cycle, and as can be seen from fig. 4 to 8, the lotion still has good uniformity after being subjected to storage stability tests under different conditions, and no delamination or precipitation appears, indicating that the lotion has good stability.
While the foregoing embodiments have been described in some, but not all embodiments of the invention, other embodiments of the invention can be obtained from the embodiments of the invention without departing from the scope of the invention.

Claims (10)

1. A tetraisopalmitate ascorbate lyotropic liquid crystal nanoparticle dispersion, characterized in that it is prepared from the following raw materials: ascorbyl tetraisopalmitate, a lyotropic liquid crystal carrier and an aqueous stabilizer solution; the lyotropic liquid crystal carrier comprises grease and an emulsifying agent, wherein the mass ratio of the ascorbyl tetraisopalmitate to the grease is 1-10:10.
2. The lyotropic liquid crystal nanoparticle dispersion of claim 1, wherein the grease comprises one or more of cetyl palmitate, glycerol monolaurate, glycerol behenate, glycerol distearate, glycerol monooleate, glycerol monostearate, monoglyceride succinate, glyceryl caprylate, monoglyceride oleate, propylene glycol monostearate, propylene glycol monooleate, propylene glycol monolaurate, sweet almond oil, hazelnut oil, soybean oil, olive oil, and grapeseed oil.
3. The lyotropic liquid crystal nanoparticle dispersion of claim 1, wherein the emulsifier comprises one or more of decyl glucoside, lauryl glucoside, sucrose monostearate, cetyl palmitate, tween 80, and coco glucoside.
4. The lyotropic liquid crystal nanoparticle dispersion of claim 1, wherein the stabilizer in the aqueous solution of stabilizers comprises one or more of carbomers, sodium alginate, hyaluronic acid, magnesium stearate, xanthan gum, and calcium stearate.
5. The method for preparing the ascorbyl tetraisopalmitate lyotropic liquid crystal nanoparticle dispersion according to any one of claims 1 to 4, comprising the following steps:
mixing ascorbyl tetraisopalmitate, an emulsifier and grease to obtain a grease mixture;
emulsifying the oil mixture and a stabilizer aqueous solution to obtain nanoparticle colostrum;
and dispersing the nanoparticle colostrum to obtain the ascorbyl tetraisopalmitate lyotropic liquid crystal nanoparticle dispersion.
6. The method according to claim 5, wherein the ratio of the oil mixture to the aqueous stabilizer solution is 1-10 g/50 mL, and the concentration of the stabilizer in the aqueous stabilizer solution is 0.1-3 wt%.
7. The method according to claim 5, wherein the emulsifying means comprises shearing at a rotation speed of 6000 to 12000rpm for 1 to 10min.
8. The method according to claim 5, wherein the dispersing means comprises homogenizing at a pressure of 400 to 1000bar for 3 to 9 times.
9. Use of the ascorbyl tetraisopalmitate lyotropic liquid crystal nanoparticle dispersion according to any one of claims 1 to 4 or the ascorbyl tetraisopalmitate lyotropic liquid crystal nanoparticle dispersion obtained by the preparation method according to any one of claims 5 to 8 in a cosmetic lotion.
10. The toning lotion is characterized by comprising the following components in percentage by mass: 1-3% of ascorbyl tetraisopalmitate lyotropic liquid crystal nanoparticle dispersion, 80-93.37% of water, 0.03-1% of chelating agent, 0.3-0.1% of anti-inflammatory agent, 5-15% of humectant and 0.3-1% of preservative, wherein the ascorbyl tetraisopalmitate lyotropic liquid crystal nanoparticle dispersion is the ascorbyl tetraisopalmitate lyotropic liquid crystal nanoparticle dispersion according to any one of claims 1-4 or the ascorbyl tetraisopalmitate lyotropic liquid crystal nanoparticle dispersion obtained by the preparation method according to any one of claims 5-8.
CN202310173488.7A 2023-02-28 2023-02-28 Ascorbyl tetraisopalmitate lyotropic liquid crystal nanoparticle dispersion, preparation method and application thereof, and toning lotion Pending CN116098832A (en)

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