CN115737453A - Nano-efficacy substance inclusion soluble in transparent aqueous solution and preparation method thereof - Google Patents

Nano-efficacy substance inclusion soluble in transparent aqueous solution and preparation method thereof Download PDF

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CN115737453A
CN115737453A CN202211637611.8A CN202211637611A CN115737453A CN 115737453 A CN115737453 A CN 115737453A CN 202211637611 A CN202211637611 A CN 202211637611A CN 115737453 A CN115737453 A CN 115737453A
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nano
chitosan
efficacy
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CN115737453B (en
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彭雅娟
林彦炼
李旺凤
李国锋
莫婵娟
黄思莹
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Guangzhou Xufan Biotechnology Co ltd
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Abstract

The application relates to the field of cosmetics, and particularly discloses a nano efficacy substance inclusion soluble in a transparent water agent, which comprises the following components in percentage by mass: 1-4% of an efficacy substance; 5 to 15 percent of liposome; 10-30% of polyol; the balance of water; the total mass percentage is 100%; the effective substance is one or more of ceramide series and its analogues, salicyloyl phytosphingosine, hydroxypropyl dipalmitoamide MEA, glabridin, phloretin, and hydroxydecyl ubiquinone; the liposome is hydrogenated lecithin. The transparent water aqua has the advantages of high transparency, high stability and high transdermal permeability, has good compatibility with water, and can effectively solve the problem of the addition requirement of the transparent water aqua.

Description

Nano effect object inclusion soluble in transparent water agent and preparation method thereof
Technical Field
The application relates to the field of skin care products, in particular to a nano effect object inclusion body capable of being dissolved in a transparent water agent and a preparation method thereof.
Background
With the increasing market demand for functional skin care products, the technical requirements of cosmetic skin care product formulas on functional active substances are higher and higher, and the efficacy and safety of the active substances are taken into consideration in the development process of the cosmetic formulas. However, although the active substance has high activity in the practical application process, the phenomenon of reduced stability or difficult dissolution is easy to occur when the active substance is added into a formula, so that the active substance cannot exert the self-efficacy well.
In order to solve the problems of stability and insolubility of active substances, a nano-coating technology is adopted in the market, and most of the active substances are coated by using an emulsifier, wax and grease. However, the nano-efficacy substance prepared by the method can only be made into a product with an opaque dosage form, and cannot meet the requirement for a water aqua with high transparency requirement. Thus, there is still room for improvement.
Disclosure of Invention
The application provides a nano-efficacy substance inclusion soluble in a transparent aqueous solution and a preparation method thereof, and the nano-efficacy substance inclusion has the advantages of high transparency, high stability and high transdermal permeability, has good compatibility with water, and can effectively solve the problem of the addition requirement of the transparent aqueous solution.
In a first aspect, the present application provides a nano-functional material inclusion soluble in a transparent aqueous solution, which adopts the following technical scheme:
a nano effect object inclusion soluble in a transparent water agent comprises the following components in percentage by mass: 1-4% of an efficacy substance; 5 to 15 percent of liposome; 10-30% of polyol; the balance of water; the total mass percentage is 100 percent;
the functional substance is one or more of ceramide series and its analogues, salicyloyl phytosphingosine, hydroxypropyl dipalmitoamide MEA, glabridin, phloretin, and hydroxydecyl ubiquinone;
the liposome is hydrogenated lecithin.
By adopting the technical scheme, the ceramide series and analogues thereof and other insoluble substances are directly applied to a cosmetic formula, so that the problems of low water solubility, poor transdermal absorbability and low stability exist, the insoluble effect substance is coated by the hydrogenated lecithin to obtain the nano effect inclusion body, so that the insoluble effect substance can be stably and uniformly dissolved in a transparent water agent, the application of the traditional grease and emulsifier is abandoned, a brand new dispersing agent is adopted for achieving nanoscale coating, the dispersing agent has good compatibility with water, the water agent has high transparency, and the problem of the addition requirement of the transparent water agent is effectively solved. In addition, the hydrogenated lecithin has better skin-friendly and stratum corneum softening capacity, is beneficial to improving the transdermal permeability of the efficacy substance and is beneficial to the efficacy substance to better play a role.
Meanwhile, the suspension effect is generated by utilizing the mutual hydrogen bond binding action of the polyhydric alcohols, so that nano efficacy substance particles can stably exist in liquid and are not easy to aggregate, so that methods such as a solubilizer, grease or wax are not needed to be used for extra assistance, and the polyhydric alcohols generate a synergistic effect with the efficacy substance, thereby being beneficial to improving the moisturizing effect of the inclusion.
Preferably, the particle size of the efficacy substance is 100-300nm.
By adopting the technical scheme, the functional substance can be uniformly and stably coated by the hydrogenated lecithin, and the stability and the transdermal permeability of the nano functional inclusion body are further improved.
Preferably, the polyhydric alcohol is one or more of 1, 3-butanediol, 1, 2-pentanediol, 1, 2-hexanediol, glycerol, dipropylene glycol, sorbitol, methyl propylene glycol, iso-1, 3-propanediol.
Preferably, the nano efficacy substance inclusion also comprises chitosan and carboxymethyl chitosan, wherein the chitosan and carboxymethyl chitosan respectively account for 1-2% and 1-4% of the nano efficacy substance inclusion by mass percent.
By adopting the technical scheme, in order to further improve the transparency of the nano efficacy object inclusion, chitosan and carboxymethyl chitosan are added, the surface of the chitosan can be connected with functional groups, and the nano efficacy object inclusion is flexibly loaded in a wrapping mode; carboxymethyl chitosan is a chitin derivative of chitosan subjected to carboxymethylation reaction, and carboxyl and amino on the carboxymethyl chitosan are hydrophilic groups and have strong hydrophilicity. Therefore, the synergistic cooperation of the chitosan and the carboxymethyl chitosan is beneficial to further improving the hydrophilicity of the nano efficacy substance inclusion, so that the nano efficacy substance inclusion is better compatible with water, and the transparency of the nano efficacy substance inclusion is improved.
Preferably, the mass ratio of the chitosan to the carboxymethyl chitosan is 1: (1.5-1.8).
By adopting the technical scheme, the chitosan and the carboxymethyl chitosan are matched with each other in a specific proportion, so that the nano effect object inclusion is better wrapped, the compatibility between the nano effect object inclusion and water is improved, and the nano effect object inclusion can be more quickly dissolved in the transparent water aqua.
Preferably, the preparation method of the carboxymethyl chitosan comprises the following steps:
s1: swelling: adding 10-20 parts by mass of chitosan into a reaction kettle, adding 100-120 parts by mass of isopropanol, and uniformly stirring for 1-2 hours to obtain a solution A;
s2: alkalization: adding 50-60 parts by mass of sodium hydroxide solution into the solution A for 5-6 times, heating to 40-50 ℃, and uniformly stirring for 30-40min to obtain solution B;
s3: carboxymethylation: dissolving 10-20 parts by mass of chloroacetic acid in 50-60 parts by mass of isopropanol solution, adding into the solution B for 4-5 times within 30-40min, and heating in water bath at 50-60 ℃ for 3-5h;
s4: and (3) terminating the reaction: adjusting pH to 6-7, removing isopropanol, adding water for full dissolution, centrifuging, removing supernatant, precipitating with anhydrous ethanol, filtering, and washing with ethanol to obtain carboxymethyl chitosan.
By adopting the technical scheme, the carboxymethyl chitosan prepared by the method has higher purity, so that the carboxymethyl chitosan is better matched with chitosan, and the hydrophilicity of the nano effect object inclusion is improved, so that the nano effect object inclusion has higher transparency.
Preferably, the degree of substitution of the carboxymethyl chitosan is 80 to 90%.
By adopting the technical scheme, the carboxymethyl chitosan with a specific degree of substitution is cooperatively matched with the chitosan, so that the carboxymethyl chitosan is better compatible with the chitosan, and the transparency of the nano functional object inclusion body is optimal.
In a second aspect, the present application provides a method for preparing a nano functional substance inclusion soluble in a transparent aqueous solution, which adopts the following technical scheme:
a preparation method of a nano functional substance inclusion soluble in a transparent aqueous solution comprises the following steps:
s1: weighing the effective substances and the liposome according to the formula, heating to 80-100 ℃, and dissolving to be uniform and transparent;
s2: adding polyalcohol and water, homogenizing in an ultrasonic homogenizer with ultrasonic frequency of 19-29kHz, power of 1300-1500W, and ultrasonic time of 10-30min to obtain nanometer functional substance inclusion.
By adopting the technical scheme, the effect substance and the liposome are dissolved at the temperature of 80-100 ℃, so that the effect substance is better wrapped by the hydrogenated lecithin, and the movement between molecules is accelerated at the temperature, thereby being beneficial to improving the speed of wrapping the effect substance by the hydrogenated lecithin and accelerating the reaction process; then an ultrasonic homogenization treatment mode is used to enable the particle size of the effect substance to reach 100nm to 300nm, hydrogenated lecithin is adopted to wrap the effect substance, and polyalcohol is added in an auxiliary mode to generate suspension to enable the structure of the effect substance to be stable. The method for preparing the nano effect object inclusion has the advantages of simple production process, high production efficiency and low production cost, and is beneficial to industrial production.
In summary, the present application includes at least one of the following beneficial technical effects:
1. the nanometer effect inclusion is obtained by coating the insoluble effect substance with the hydrogenated lecithin, so that the insoluble effect substance can be stably and uniformly dissolved in the transparent water agent, the application of the traditional grease and emulsifier is abandoned, a brand new dispersing agent is adopted for achieving nanoscale encapsulation, the dispersing agent has good compatibility with water, the water agent has high transparency, and the problem of the addition requirement of the transparent water agent is effectively solved. Meanwhile, the suspension effect is generated by utilizing the hydrogen bond combination effect of the polyols, so that nano efficacy substance particles can stably exist in liquid and are not easy to aggregate, so that the method of using solubilizer, grease or wax and the like is not needed to be particularly assisted, and the synergistic effect is generated by adding the polyols and the efficacy substances, thereby being beneficial to improving the moisturizing effect of the inclusion.
2. Chitosan and carboxymethyl chitosan are added, the surface of the chitosan can be connected with functional groups, and a nano functional object inclusion is flexibly loaded in a wrapping manner; carboxymethyl chitosan is a chitin derivative of chitosan subjected to carboxymethylation reaction, and carboxyl and amino on the carboxymethyl chitosan are hydrophilic groups and have strong hydrophilicity. Therefore, the synergistic cooperation of the chitosan and the carboxymethyl chitosan is beneficial to further improving the hydrophilicity of the nano effect object inclusion, so that the nano effect object inclusion is better compatible with water, and the transparency of the nano effect object inclusion is improved.
3. The method is adopted to prepare the nano effect substance inclusion, the effect substance and the liposome are dissolved at the temperature of 80-100 ℃, so that the effect substance is better wrapped by the hydrogenated lecithin, and the movement between molecules is accelerated at the temperature, thereby being beneficial to improving the speed of wrapping the effect substance by the hydrogenated lecithin and accelerating the reaction process; then an ultrasonic homogenization treatment mode is used to enable the particle size of the effect substance to reach 100nm to 300nm, hydrogenated lecithin is adopted to wrap the effect substance, and polyalcohol is added in an auxiliary mode to generate suspension to enable the structure of the effect substance to be stable. Simple production process, high production efficiency and low production cost, and is favorable for industrial production.
Detailed Description
The present application will be described in further detail with reference to examples.
Preparation example 1
The preparation method of the carboxymethyl chitosan comprises the following steps:
s1: swelling: adding 10kg of chitosan into a reaction kettle, adding 100kg of isopropanol, and uniformly stirring for 1 hour to obtain a solution A;
s2: alkalization: adding 50kg of sodium hydroxide solution into the solution A for 5 times, heating to 40 ℃, and uniformly stirring for 30min to obtain a solution B;
s3: carboxymethylation: dissolving 10kg of chloroacetic acid in 50kg of isopropanol solution, adding into the solution B for 4 times within 30min, and heating in a water bath at 50 ℃ for 3h;
s4: and (3) reaction termination: adjusting pH to 6, removing isopropanol, adding water for full dissolution, centrifuging, removing supernatant, precipitating with anhydrous ethanol, filtering, and washing with ethanol to obtain carboxymethyl chitosan; the degree of substitution of carboxymethyl chitosan was 80%.
Preparation example 2
The difference from preparation example 1 is that:
the preparation method of the carboxymethyl chitosan comprises the following steps:
s1: swelling: adding 20kg of chitosan into a reaction kettle, adding 120kg of isopropanol, and uniformly stirring for 2 hours to obtain a solution A;
s2: alkalization: adding 60kg of sodium hydroxide solution into the solution A for 6 times, heating to 50 ℃, and uniformly stirring for 40min to obtain a solution B;
s3: carboxymethylation: dissolving 20kg of chloroacetic acid in 60kg of isopropanol solution, adding into the solution B for 5 times within 40min, and heating in a water bath at 60 ℃ for 5h;
s4: and (3) reaction termination: adjusting pH to 7, removing isopropanol, adding water for full dissolution, centrifuging, removing supernatant, precipitating with anhydrous ethanol, filtering, and washing with ethanol to obtain carboxymethyl chitosan; the degree of substitution of carboxymethyl chitosan was 90%.
Preparation example 3
The difference from preparation example 1 is that: the preparation method of the carboxymethyl chitosan comprises the following steps:
s1: swelling: adding 5kg of chitosan into a reaction kettle, adding 80kg of isopropanol, and uniformly stirring for 1h to obtain a solution A;
s2: alkalization: adding 40kg of sodium hydroxide solution into the solution A for 5 times, heating to 40 ℃, and uniformly stirring for 30min to obtain a solution B;
s3: carboxymethylation: dissolving 7kg of chloroacetic acid in 40kg of isopropanol solution, adding into the solution B for 4 times within 30min, and heating in a water bath at 50 ℃ for 3h;
s4: and (3) reaction termination: adjusting pH to 6, removing isopropanol, adding water for full dissolution, centrifuging, removing supernatant, precipitating with anhydrous ethanol, filtering, and washing with ethanol to obtain carboxymethyl chitosan; the degree of substitution of carboxymethyl chitosan was 70%.
Preparation example 4
The difference from preparation example 1 is that:
s1: swelling: adding 25kg of chitosan into a reaction kettle, adding 130kg of isopropanol, and uniformly stirring for 1h to obtain a solution A;
s2: alkalization: adding 65kg of sodium hydroxide solution into the solution A for 5 times, heating to 40 ℃, and uniformly stirring for 30min to obtain a solution B;
s3: carboxymethylation: dissolving 30kg of chloroacetic acid in 70kg of isopropanol solution, adding into the solution B for 4 times within 30min, and heating in a water bath at 50 ℃ for 3h;
s4: and (3) reaction termination: adjusting pH to 6, removing isopropanol, adding water for full dissolution, centrifuging, removing supernatant, precipitating with anhydrous ethanol, filtering, and washing with ethanol to obtain carboxymethyl chitosan; the degree of substitution of carboxymethyl chitosan was 100%.
Example 1
A nano-efficacy substance inclusion soluble in a transparent aqueous solution comprises the following components by mass:
1kg of efficacy substance; 5kg of liposome; 10kg of polyhydric alcohol; 84kg of water;
wherein the efficacy substance is ceramide; the liposome is hydrogenated lecithin; the polyalcohol is glycerol; the particle size of the functional substance is 100nm.
A preparation method of a nano effect object inclusion soluble in a transparent water agent comprises the following steps:
s1: respectively weighing 1kg of ceramide and 5kg of hydrogenated lecithin, heating to 85 ℃, and dissolving to be uniform and transparent;
s2: then adding 10kg of glycerin and 84kg of water, and homogenizing in an ultrasonic homogenizer with the ultrasonic frequency of 19kHz, the power of 1300W and the ultrasonic time of 10min to obtain the nano functional object inclusion.
Example 2
The difference from example 1 is that:
a nano-efficacy substance inclusion soluble in a transparent aqueous solution comprises the following components by mass:
4kg of functional materials; 15kg of liposome; 30kg of polyhydric alcohol; 51kg of water;
wherein the functional substance is hydroxypropyl dipalmitoyl amide MEA; the liposome is hydrogenated lecithin; the polyhydric alcohols are 1, 3-butanediol and 1, 2-hexanediol; the particle size of the functional substance is 300nm.
A preparation method of a nano functional substance inclusion soluble in a transparent aqueous solution comprises the following steps:
s1: respectively weighing 4kg of hydroxypropyl dipalmityl amide MEA and 15kg of hydrogenated lecithin, heating to 100 ℃, and dissolving to be uniform and transparent;
s2: then 15kg of 1, 3-butanediol, 15kg of 1, 2-hexanediol and 51kg of water are added, and the mixture is put into an ultrasonic homogenizer for homogenization, wherein the ultrasonic frequency is 29kHz, the power is 1500W, and the ultrasonic time is 30min, so that the nano functional object inclusion is obtained.
Comparative example 1
The difference from example 2 is that: the amount of each component is not within the scope of the present application, i.e.: the nano functional substance inclusion comprises the following components in parts by mass:
5kg of functional materials; 20kg of liposome; 8kg of polyol; 67kg of water.
Comparative example 2
The difference from example 2 is that: the temperature in S1 was 60 ℃.
Comparative example 3
The difference from example 2 is that: in S2, the ultrasonic frequency is 16kHz, the power is 1200W, and the ultrasonic time is 8min.
Comparative example 4
The difference from example 2 is that: in S2, the ultrasonic frequency is 32kHz, the power is 1600W, and the ultrasonic time is 35min.
Example 3
The difference from example 2 is that: the nano efficacy substance inclusion also comprises chitosan and carboxymethyl chitosan, wherein the chitosan and the carboxymethyl chitosan respectively account for 1 percent and 1 percent of the nano efficacy substance inclusion by mass, namely the chitosan accounts for 1kg by mass, the carboxymethyl chitosan accounts for 1kg by mass, and the water accounts for 82kg by mass; carboxymethyl chitosan the carboxymethyl chitosan prepared in preparation example 1 was used.
Example 4
The difference from example 2 is that: the nano efficacy substance inclusion also comprises chitosan and carboxymethyl chitosan, wherein the chitosan and the carboxymethyl chitosan respectively account for 2 percent and 4 percent of the nano efficacy substance inclusion by mass, namely the chitosan accounts for 2kg by mass, and the carboxymethyl chitosan accounts for 4kg by mass; 78kg of water; carboxymethyl chitosan the carboxymethyl chitosan prepared in preparation example 1 was used.
Example 5
The difference from example 2 is that: the nano effect object inclusion also comprises chitosan and carboxymethyl chitosan, wherein the chitosan and the carboxymethyl chitosan respectively account for 1.5 percent and 3 percent of the nano effect object inclusion by mass, namely the chitosan accounts for 1.5kg by mass, and the carboxymethyl chitosan accounts for 3kg by mass; 79.5kg of water; carboxymethyl chitosan the carboxymethyl chitosan prepared in preparation example 2 was used.
Example 6
The differences from example 5 are: carboxymethyl chitosan the carboxymethyl chitosan prepared in preparation example 3 was used.
Example 7
The differences from example 5 are: carboxymethyl chitosan the carboxymethyl chitosan prepared in preparation example 4 was used.
Example 8
The difference from example 5 is that: the mass ratio of chitosan to carboxymethyl chitosan is 1:1.5.
example 9
The differences from example 5 are: the mass ratio of chitosan to carboxymethyl chitosan is 1:1.8.
application example 1
An aqueous solution comprises the following components by mass:
phase A: 89.95kg of water; 5kg of glycerol; 0.05kg of EDTA disodium;
phase B: 3kg of butanediol; 0.5kg of p-hydroxyacetophenone;
and C phase: 1kg of the nano functional object inclusion prepared in the example 1 is adopted; 0.5kg of hexanediol.
The preparation method of the aqueous solution comprises the following steps:
s1: weighing the phase A raw material into a container A, weighing the phase B raw material into a container B, heating to 75 ℃, pouring the phase A raw material after complete dissolution, and uniformly stirring;
s2: cooling to 45 deg.C, adding C phase raw material, stirring, and discharging to obtain aqueous solution.
Application examples 2 to 13
The difference from application example 1 is that: the nano efficacy object inclusion prepared in examples 2-9 and comparative examples 1-4 was used.
Blank control group
The difference from application example 1 is that: no nano effect object inclusion is added in the C phase.
Experiment 1 stability test
And (3) heat resistance test: the water aqua prepared in the application examples 1-13 and the blank control group are respectively put into an electric heating constant temperature incubator at 40 ℃ for 24 hours, and after the room temperature is recovered, whether turbidity, precipitation and other phenomena appear or not is observed.
Cold resistance test: the water aqua prepared in the application examples 1-13 and the blank control group are respectively put in a refrigerator with the temperature of-5 ℃ for 24 hours, and the phenomena of turbidity, precipitation and the like are observed after the room temperature is recovered.
And (3) centrifugal test: and respectively placing the water aqua prepared in the application examples 1-13 and the blank control group in a centrifuge, and testing at the rotating speed of 3000r/min for 30min to observe whether the sample is turbid or precipitated.
Experiment 2 light transmittance test
The light transmittances of the application examples 1-13 and the blank control group in the visible light region (380-780 nm) were respectively detected by an ultraviolet-visible spectrophotometer (Shimadzu UV-2550).
Experiment 3 average particle size test
The particle size distributions of application examples 1-13 and the blank control group were measured using a laser particle size analyzer (MalvernZS-90), respectively.
Experiment 4 transdermal penetration Performance test
In the experiment, in-vitro pigskin is used as an experimental material, the back skin of a non-traumatic pig is selected, a subcutaneous fat layer is removed, hair on the surface of the pigskin is cut to be below 2mm by an electric hair clipper, then a circular sheet with the diameter of 4cm is drilled by a circular puncher, and the thickness of the sheet is trimmed to be not more than 1mm. The knocked-down pigskin sample was cleaned and mounted on a Franz diffusion transdermal cell with its dermal layer facing the receiving cell containing PBS and the stratum corneum exposed in the dosing chamber and mounted with iron clips. 100 mu L of the aqueous solution prepared in application examples 1-13 and the blank control group are respectively added into a dosing pool, and then the skin penetration is carried out for 4h by massaging for 2min with a mini massager. Accurately collecting 3mL of receiving solution at regular time (and supplementing 3mL of receiving solution), accurately adding 1mL of ethyl acetate, extracting on shaking table, adding quantitative anhydrous ethanol, measuring absorbance at 274nm, and calculating cumulative permeation amount (μ g/cm) 3 ). The larger the cumulative penetration, the better the transdermal permeability of the nano efficacy agent inclusion.
The results are shown in Table 1.
TABLE 1
Figure 153774DEST_PATH_IMAGE002
According to the comparison between the application example 10 and the application examples 1-2 in the table 1, the dosage of the functional substance, the hydrogenated lecithin and the glycerol in the application example 10 is not in the range protected by the application, and the water aqua in the application example 10 is a semitransparent liquid and generates a turbid phenomenon at 40 ℃, which indicates that the heat resistance of the nano functional substance inclusion is not better than that of the application examples 1-2; the precipitation phenomenon appears at the temperature of minus 5 ℃, which shows that the cold resistance of the nano functional object inclusion is not as good as that of the application example 1-2; the light transmittance is lower than that of application examples 1-2, the average particle size is larger than that of application examples 1-2, and the proportion of the functional substance, the hydrogenated lecithin and the glycerol influences the transparency of the nano functional substance inclusion. Therefore, the dosage of the functional substance, the hydrogenated lecithin and the glycerol is only within the protection range of the application, so that the nano functional substance inclusion has higher transparency, and the effect of the application can not be achieved by any proportion.
According to the comparison between the application example 11 and the application examples 1-2 in the table 1, the dissolution temperature of the efficacy material and the hydrogenated lecithin in the application example 11 is 60 ℃, while the temperature in the application example 1 is 80 ℃, the temperature in the application example 2 is 100 ℃, and the light transmittance of the water aqua in the application example 11 is smaller than that in the application example 1-2, because the encapsulation effect of the efficacy material and the hydrogenated lecithin is not well generated when the temperature is 60 ℃, and the transparency of the nano efficacy material inclusion is affected. Therefore, only when the temperature is 80-100 ℃, the functional substance and the hydrogenated lecithin can better generate the wrapping effect, and meanwhile, due to the high temperature, the movement among molecules is accelerated, so that the wrapping speed is favorably improved, the reaction process is accelerated, and the transparency of the nano functional substance inclusion is improved.
According to the comparison of application examples 12-13 in table 1 with application example 1, respectively, the ultrasonic frequency, power and ultrasonic time in application examples 12-13 are not in the range protected by the application example 1, and the light transmittance of the aqueous solution in application example 12 is less than that of application example 1, because the ultrasonic frequency, power and ultrasonic time in application example 12 are lower than the parameters in application example 1, particles cannot reach the nano range at this time, and the efficacy substance and the hydrogenated lecithin cannot reach the complete encapsulation state; the light transmittance of the aqueous solution in application example 13 is lower than that of application example 1, because the ultrasonic frequency, power and ultrasonic time in application example 13 are higher than those in application example 1, the structures of particles such as ceramide and the like are damaged, and the effect substance and the hydrogenated lecithin cannot be well coated. Therefore, the ultrasonic frequency, power and ultrasonic time only have the effect of improving the transparency of the nano efficacy object inclusion within the protection range of the application.
In summary, the ratio of the functional substance to the hydrogenated lecithin and the glycerol in the application is cooperatively matched with the dissolution temperature, the ultrasonic frequency, the power and the ultrasonic time of the functional substance and the hydrogenated lecithin, so that the transparency of the nano functional substance inclusion is greatly improved.
According to the comparison between the application examples 3-5 in the table 1 and the application example 2, the nano effect object inclusion further comprises chitosan and carboxymethyl chitosan, and the light transmittance of the aqueous solution in the application examples 3-5 is greater than that of the application example 2, which shows that the carboxymethyl chitosan prepared by the method is cooperated with chitosan, so that the hydrophilicity of the nano effect object inclusion is improved, the nano effect object inclusion is better compatible with water, and the transparency of the nano effect object inclusion is improved. The surface of the chitosan can be connected with functional groups, and a nano functional object inclusion is flexibly loaded in a wrapping mode; carboxymethyl chitosan is a chitin derivative obtained by performing carboxymethylation reaction on chitosan, and carboxyl and amino groups on the carboxymethyl chitosan are hydrophilic groups and have strong hydrophilicity.
According to comparison between application examples 6-7 and application example 5 in table 1, the degree of substitution of carboxymethyl chitosan in application example 6 is 70%, the degree of substitution of carboxymethyl chitosan in application example 7 is 100%, and the light transmittance of the aqueous solution in application examples 6-7 is smaller than that of application example 5, because the degree of substitution of carboxymethyl chitosan is 70% and 100%, the coating effect with chitosan cannot be well generated, and the transparency of the nano efficacy substance coating is affected.
According to the comparison between the application examples 8-9 and the application example 5 in the table 1, the mass ratio of the chitosan to the carboxymethyl chitosan in the application example 8 is 1:1.5, the mass ratio of the chitosan to the carboxymethyl chitosan in the application example 9 is 1:1.8, the light transmittance of the aqueous solution in application examples 8-9 is greater than that in application example 5, and the cumulative transmittance is also higher than that in application example 5, which indicates that the synergistic cooperation of chitosan and carboxymethyl chitosan in a specific ratio is beneficial to improving the transparency and transdermal permeability of the nano effect object inclusion.
In conclusion, the carboxymethyl chitosan prepared by the method disclosed by the application and the chitosan are cooperatively matched in a specific ratio, so that the compatibility between the nano effect object inclusion and water is improved, the nano effect object inclusion can be dissolved in a transparent aqueous solution more quickly, the transdermal permeability of the nano effect object inclusion is improved, and the effect objects can better play a role.
The above embodiments are preferred embodiments of the present application, and the protection scope of the present application is not limited by the above embodiments, so: equivalent changes in structure, shape and principle of the present application shall be covered by the protection scope of the present application.

Claims (8)

1. A nanometer efficacy object inclusion body which can be dissolved in transparent water agent is characterized in that: the composite material comprises the following components in percentage by mass: 1-4% of an efficacy substance; 5 to 15 percent of liposome; 10-30% of polyol; the balance of water; the total mass percentage is 100%;
the functional substance is one or more of ceramide series and its analogues, salicyloyl phytosphingosine, hydroxypropyl dipalmitoamide MEA, glabridin, phloretin, and hydroxydecyl ubiquinone;
the liposome is hydrogenated lecithin.
2. The nano efficacy object inclusion body soluble in transparent water agent according to claim 1, wherein: the particle size of the efficacy substance is 100-300nm.
3. The nano efficacy object inclusion body soluble in transparent water agent according to claim 1, wherein: the polyalcohol is one or more of 1, 3-butanediol, 1, 2-pentanediol, 1, 2-hexanediol, glycerol, dipropylene glycol, sorbitol, methyl propylene glycol and iso-1, 3-propanediol.
4. The nano efficacy object inclusion body soluble in transparent water agent according to claim 1, wherein: the nano effect object inclusion also comprises chitosan and carboxymethyl chitosan, wherein the chitosan and the carboxymethyl chitosan respectively account for 1-2% and 1-4% of the nano effect object inclusion by mass percent.
5. The nano efficacy object inclusion body soluble in transparent water agent according to claim 4, wherein: the mass ratio of the chitosan to the carboxymethyl chitosan is 1: (1.5-1.8).
6. The nano efficacy object inclusion body soluble in transparent water agent according to claim 5, wherein: the preparation method of the carboxymethyl chitosan comprises the following steps:
s1: swelling: adding 10-20 parts by mass of chitosan into a reaction kettle, adding 100-120 parts by mass of isopropanol, and uniformly stirring for 1-2 hours to obtain a solution A;
s2: alkalization: adding 50-60 parts by mass of sodium hydroxide solution into the solution A for 5-6 times, heating to 40-50 ℃, and uniformly stirring for 30-40min to obtain solution B;
s3: carboxymethylation: dissolving 10-20 parts by mass of chloroacetic acid in 50-60 parts by mass of isopropanol solution, adding into the solution B for 4-5 times within 30-40min, and heating in water bath at 50-60 ℃ for 3-5h;
s4: and (3) reaction termination: adjusting pH to 6-7, removing isopropanol, adding water for dissolving, centrifuging, removing supernatant, precipitating with anhydrous ethanol, filtering, and washing with ethanol to obtain carboxymethyl chitosan.
7. The nano efficacy object inclusion body soluble in transparent water agent according to claim 6, wherein: the substitution degree of the carboxymethyl chitosan is 80-90%.
8. A method for preparing nano efficacy material inclusion soluble in transparent water agent according to any one of claims 1 to 7, which is characterized in that: the method comprises the following steps:
s1: weighing the effective substances and the liposome according to the formula, heating to 80-100 ℃, and dissolving to be uniform and transparent;
s2: adding polyalcohol and water, homogenizing in an ultrasonic homogenizer with ultrasonic frequency of 19-29kHz and power of 1300-1500W for 10-30min to obtain nanometer functional substance inclusion.
CN202211637611.8A 2022-12-20 2022-12-20 Nanometer functional object inclusion soluble in transparent water agent and preparation method thereof Active CN115737453B (en)

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