CN111166682A

CN111166682A - Micro-emulsified skin care emulsion and preparation method thereof

Info

Publication number: CN111166682A
Application number: CN202010050019.2A
Authority: CN
Inventors: 蔡汝青; 李松涛; 段朝辉
Original assignee: Guangzhou Gialen Cosmetics Co ltd
Current assignee: Guangzhou Gialen Cosmetics Co ltd
Priority date: 2020-01-17
Filing date: 2020-01-17
Publication date: 2020-05-19

Abstract

The invention relates to the technical field of skin care products, in particular to a micro-emulsified skin care emulsion and a preparation method thereof, wherein the formula of the micro-emulsified skin care emulsion comprises a phase A: 60-80% of deionized water, 0.05-0.5% of water-based thickening agent and 2-10% of polyalcohol; phase B: 5-30% of a microemulsion composition; and phase C: 1 to 10 percent of skin conditioner, 0.5 to 1 percent of preservative and 0.5 to 2 percent of auxiliary agent. Compared with the prior art, the skin care emulsion prepared by the invention has the advantages that the particle size can reach 80-300nm, the particle size distribution is more uniform, the skin care emulsion can be better absorbed by the skin, the moisturizing effect is obvious, the preparation process is more flexible, the production control is easy, and the industrial application is favorably realized.

Description

Micro-emulsified skin care emulsion and preparation method thereof

Technical Field

The invention relates to the technical field of skin care products, and particularly relates to a micro-emulsified skin care emulsion and a preparation method thereof.

Background

The skin care emulsion is a cosmetic preparation containing water and an oily emollient, can supplement moisture to skin, brings water-moist feeling, and simultaneously has the functions of softening skin and forming a protective layer on the surface of the skin to prevent moisture from evaporating, so the skin care emulsion is an extremely important preparation form in skin care products and has a large market scale.

The cosmetic active ingredients must be absorbed through the skin of the horny layer to achieve the effect of the active parts. The absorption pathway of the skin mainly includes the following three aspects: transmembrane absorption of stratum corneum cells, interstitial spaces between keratinocytes, sweat pores, etc. Generally, the macromolecules and water-soluble components are mainly absorbed through hair follicles, sweat glands and sebaceous glands, and the absorption amount is small; small molecules and fat-soluble components are absorbed mainly through the transmembrane and interstitial spaces of the stratum corneum cells. In order to improve the transdermal absorption rate, the improvement of the product formulation is mainly relied on, for example, by chemical penetration enhancer, by the destruction of physical barrier or by using external energy as driving force, such as by using micro-needle, ultrasonic penetration enhancer, ion introduction, etc. However, these methods described above are likely to increase the skin irritation response. In addition, the transdermal absorption rate can be effectively and safely improved by means of embedding target compounds (such as liposome, nanoparticles and the like), and for the emulsion, the method of reducing the particle size of the emulsion through a micro-emulsification technology is also a safe and effective mode.

The traditional skin care lotion is generally prepared by chemically synthesizing a surfactant and emulsifying skin care grease and water, wherein the particle size of the lotion is generally 0.1-10 mu m, the appearance of the lotion is milky white, the emulsified particle size is large, and the particle size distribution is uneven, so that the functional components are difficult to absorb by the skin. In order to reduce the emulsified particle size, a method of the prior art for achieving a smaller emulsified particle size by solubilizing emollient oils and fats, but this method must add a large amount of surfactants, including nonionic surfactants and anionic surfactants, which in turn cause skin irritation; the other method is to adopt an interfacial chemical method (such as a phase inversion emulsification method, a PIT method and the like), and although emulsion with smaller particle size can be obtained and a large amount of chemically synthesized surfactant is not needed, the defects are that the formula design and the process implementation are too harsh, the production is inconvenient and the industrial application is difficult to realize.

Disclosure of Invention

Aiming at the defects in the prior art, the invention provides the microemulsion skin care emulsion and the preparation method thereof, the particle size of the microemulsion skin care emulsion is reduced to 80-300nm, the particle size distribution is more uniform, the microemulsion skin care emulsion can be better absorbed by the skin, the preparation process is flexible, and the production control is easy.

The purpose of the invention is realized by the following technical scheme:

provides a micro-emulsified skin care emulsion which is prepared from the following raw materials in percentage by mass:

phase A: 60-80% of deionized water, 0.05-0.5% of water-based thickening agent and 2-10% of polyalcohol;

phase B: 5-30% of a microemulsion composition;

and C phase: 1-10% of skin conditioner, 0.5-1% of preservative and 0.5-2% of auxiliary agent;

wherein, the microemulsion composition consists of 2 to 10 percent of hydrogenated lecithin, 5 to 30 percent of emollient oil, 0.1 to 0.5 percent of ceramide, 0.5 to 2 percent of phytosterol, 30 to 85 percent of polyalcohol and 5 to 30 percent of deionized water according to the mass percentage; the emulsion particle size of the microemulsion composition is 80-300 nm.

In the technical scheme, the aqueous thickening agent is one or a mixture of more than two of xanthan gum, hydroxyethyl cellulose, carbomer, propionate/C10-30 alkanol acrylate cross-linked polymer, carrageenan, crinkle carrageenan, sodium magnesium silicate, hydroxypropyl methyl cellulose and carboxymethyl cellulose.

In the above technical scheme, the polyhydric alcohol is one or a mixture of more than two of glycerol, propylene glycol, 1, 3-propanediol, 1, 2-pentanediol, dipropylene glycol, butanediol and diglycerol.

In the technical scheme, the skin-moistening oil is one or a mixture of more than two of hydrocarbon oil such as squalane, hydrogenated polyisobutene, synthetic ester oil and vegetable oil.

In the technical scheme, the synthetic ester grease is any one of caprylic/capric triglyceride, triglyceride (ethyl hexanoate) and cetyl ethyl hexanoate; the vegetable oil is any one of olive oil, chinaroot greenbrier seed oil and shea butter.

In the above technical scheme, the ceramide is one or a mixture of more than two of ceramide 1, ceramide 2, ceramide 3 and ceramide 6.

In the technical scheme, the content of PC in the hydrogenated lecithin is more than or equal to 25 percent.

In the technical scheme, the skin conditioner is one or a mixture of more than two of sodium hyaluronate, hydrolyzed hyaluronic acid, acetylated sodium hyaluronate, dipotassium glycyrrhizinate, allantoin, panthenol, polyquaternium-61, betaine and trehalose.

In the technical scheme, the preservative is one or a mixture of more than two of phenoxyethanol, chlorphenesin, ethylhexyl glycerol, 1, 2-pentanediol, 1, 2-hexanediol, p-hydroxyacetophenone and caprylyl hydroximic acid; the auxiliary agent is one or a mixture of more than two of EDTA disodium, pentetate, sodium phytate, citric acid, sodium citrate, triethanolamine, arginine, sodium hydroxide and potassium hydroxide.

The invention also provides a preparation method of the micro-emulsified skin care emulsion, which comprises the following steps:

step a, preparing a B-phase microemulsion composition:

uniformly mixing hydrogenated lecithin, polyhydric alcohol and deionized water according to the formula amount, heating to 75-85 ℃, slowly adding skin-moistening oil with ceramide and phytosterol dissolved therein at 75-85 ℃, homogenizing the mixed solution for 5-8min at the homogenizing speed of 3000-6000rpm, performing high-pressure homogenization treatment at the homogenizing pressure of 200-800bar for 2-5 times, and determining the qualified particle size of the emulsion to obtain a mixture B phase;

b, setting the temperature of an emulsifying pot to be 84-86 ℃, adding deionized water according to the formula amount, keeping the temperature and sterilizing for 25-35min, cooling to 43-46 ℃, starting stirring, controlling the stirring speed to be 35-45r/min, adding an aqueous thickening agent until the mixture is completely and uniformly dispersed, then adding polyol, and continuously stirring uniformly to obtain a mixture phase A;

c, slowly adding the phase B into an emulsifying pot, stirring for 25-35min at the speed of 35-45r/min, starting homogenizing at the speed of 500-1000r/min for 3-5 min;

and d, adding the phase C into the emulsifying pot, continuously stirring for 5-15min, then performing defoaming treatment, discharging after the detection is qualified, and filling to obtain the micro-emulsified skin care emulsion.

The invention has the beneficial effects that:

the microemulsified skin care emulsion disclosed by the invention is composed of a phase A (52-80% of deionized water, 0.05-0.5% of an aqueous thickening agent and 2-10% of polyhydric alcohol), a phase B (5-25% of a microemulsified composition) and a phase C (1-10% of a skin conditioner, 0.5-1% of a preservative and 0.5-2% of an auxiliary agent), and is prepared into a microemulsified composition with a smaller particle size under a specific process condition in the preparation process, and then is mixed with other components to prepare the skin care emulsion. Compared with the prior art, the invention has the following advantages:

(1) the particle size of the skin care emulsion prepared by the invention is 80-300nm which is far smaller than that of the traditional emulsion, the particle size distribution is more uniform, the appearance of the skin care emulsion presents blue opalescence, and the skin care emulsion can be better absorbed by the skin;

(2) according to the formula, the traditional chemically synthesized surfactant is not adopted, and the lecithin emulsifier is selected, so that the skin-friendly oil emulsion has high affinity with the skin, has no potential irritation to the skin, and is better in safety;

(3) compared with the interfacial chemical method emulsification methods (such as a phase inversion emulsification method, a PIT method and the like) in the prior art, the preparation method disclosed by the invention has the advantages that the hydrogenated lecithin is used as the emulsifier, the high-pressure homogenization method is adopted, the selection range of the skin-moistening oil is wide, the formula design and the process conditions are flexible, the production and the process control are easy, and the industrial application can be realized;

(4) after the micro-emulsified skin care emulsion disclosed by the invention is used, the skin feel is clear, the skin care emulsion is water-moist and not sticky, and the micro-emulsified skin care emulsion has a remarkable moisturizing effect.

Drawings

FIG. 1 is a graph showing the particle size and particle size distribution of the microemulsion composition of example 1.

FIG. 2 is a graph showing the particle size and particle size distribution of the microemulsion composition of example 2.

FIG. 3 is a graph showing the particle size and particle size distribution of the microemulsion composition of example 3.

FIG. 4 is a graph showing the particle size and particle size distribution of the microemulsion composition of example 4.

Fig. 5 is a graph of the evaluation result of moisturizing efficacy of the microemulsion skin care emulsion of example 4.

Detailed Description

The present invention will be described in further detail with reference to specific examples, but the present invention is not limited thereto.

Example 1:

the preparation method of the microemulsified skin care emulsion of the embodiment comprises the following steps (the following dosage is calculated by mass percent):

step a, preparing a micro-emulsified composition:

a1) adding 3% hydrogenated lecithin (PC content is more than or equal to 25%), 45.5% glycerin, 20% butanediol and 10% deionized water into an emulsifying pot, uniformly mixing at normal temperature, heating the emulsifying pot to 85 ℃, starting stirring for 45r/min, stirring for 30min, and homogenizing at 3000rpm for 5 min;

a2) adding 10% squalane, 3% caprylic/capric triglyceride, 7% shea butter, 0.5% ceramide and 2% phytosterol into an oil pan, and heating to 85 deg.C;

a3) slowly pumping the oil phase into an emulsifying pot, starting homogenizing at 3000rpm for 8min after the oil phase is pumped;

a4) homogenizing the obtained emulsion under high pressure at 500bar for 3 times, and measuring the particle diameter to 80-300nm to obtain microemulsion composition with particle diameter and particle diameter distribution shown in figure 1.

B, setting the temperature of an emulsifying pot to be 85 ℃, adding 60% deionized water, preserving heat, sterilizing for 30min, cooling to 45 ℃, starting stirring for 40r/min, and adding 0.15% carbomer and 0.05% xanthan gum until the materials are completely and uniformly dispersed; pre-dispersing 0.2% of sodium hyaluronate, 0.05% of acetylated sodium hyaluronate and 0.05% of hydrolyzed hyaluronic acid by using 2% of glycerol, 3.8% of butanediol and 2% of 1, 2-pentanediol, then adding the mixture into an emulsifying pot, and continuously stirring; after the polymer is completely dispersed uniformly, 0.1% dipotassium glycyrrhizinate, 0.1% allantoin and 0.5% betaine are added, and the mixture is continuously stirred uniformly.

And c, slowly adding 30% of the microemulsion composition into the emulsifying pot, keeping the stirring speed at 40r/min for continuously stirring for 30min, and after the stirring is uniform, starting the homogenization, wherein the homogenization speed is 500rpm, and the homogenization is 5 min.

And d, adding 0.3% of EDTA disodium, 0.2% of arginine, 0.4% of phenoxyethanol and 0.1% of ethylhexyl glycerol, continuing stirring for 10min, discharging after defoaming treatment, and filling to obtain the micro-emulsified skin care emulsion sample.

Example 2:

step a, preparing a micro-emulsified composition:

a1) adding 5% hydrogenated lecithin (PC content is more than or equal to 25%), 84.4% propylene glycol and 5% deionized water into an emulsifying pot, uniformly mixing at normal temperature, heating the emulsifying pot to 80 ℃, starting stirring for 40r/min, stirring for 30min, and homogenizing at 4000rpm for 4 min;

a2) adding 5% hydrogenated polyisobutene, 0.1% ceramide and 0.5% phytosterol into an oil pan, and heating to 80 ℃;

a3) slowly pumping the oil phase into an emulsifying pot, starting homogenizing at 6000rpm for 5min after the oil phase is pumped;

a4) homogenizing the obtained emulsion under high pressure at 800bar for 5 times, and measuring the particle diameter to 80-300nm to obtain microemulsion composition with particle diameter and particle diameter distribution shown in figure 2.

B, setting the temperature of an emulsifying pot to be 84 ℃, adding 72% of deionized water, preserving heat, sterilizing for 25min, cooling to 46 ℃, starting stirring for 35r/min, and adding 0.05% of propionic acid (ester)/C10-30 alkanol acrylate cross-linked polymer until the mixture is completely and uniformly dispersed; pre-dispersing 1% of sodium hyaluronate and 1% of hydrolyzed hyaluronic acid with 4.5% of dipropylene glycol, 1.2% of butanediol and 4.3% of diglycerol, adding into an emulsifying pot, and continuously stirring; after the polymer is completely and uniformly dispersed, adding 2% of panthenol and 6% of polyquaternium-61, and continuously stirring uniformly.

And c, slowly adding 5 percent of the microemulsion composition into the emulsifying pot, keeping the stirring speed at 40r/min for continuously stirring for 30min, and after the stirring is uniform, starting the homogenization, wherein the homogenization speed is 700rpm, and the homogenization is 5 min.

And d, adding 0.8% of sodium phytate, 0.3% of citric acid, 0.9% of sodium citrate, 0.45% of chlorphenesin and 0.5% of 1, 2-hexanediol, continuously stirring for 5min, discharging after defoaming treatment, and filling to obtain the micro-emulsified skin care emulsion sample.

Example 3:

step a, preparing a micro-emulsified composition:

a1) adding 10% hydrogenated lecithin (the content of PC is more than or equal to 25%), 25% 1, 3-propylene glycol, 6% dipropylene glycol, 24% glycerol and 18.7% deionized water into an emulsifying pot, uniformly mixing at normal temperature, heating the emulsifying pot to 75 ℃, starting stirring for 45r/min, stirring for 30min, and homogenizing at 5000rpm for 3 min;

a2) adding 5% squalane, 2% triglyceride (ethyl hexanoate), 8% olive oil, 0.3% ceramide and 1% phytosterol into an oil pan, and heating to 75 ℃;

a3) slowly pumping the oil phase into an emulsifying pot, starting homogenizing at 5000rpm for 7min after the oil phase is pumped;

a4) homogenizing the obtained emulsion under high pressure at 200bar for 4 times, and measuring the particle diameter to 80-300nm to obtain microemulsion composition with particle diameter and particle diameter distribution shown in figure 3.

B, setting the temperature of an emulsifying pot to be 86 ℃, adding 80% deionized water, preserving heat, sterilizing for 30min, cooling to 43 ℃, starting stirring for 45r/min, and adding 0.25% hydroxyethyl cellulose and 0.05% carrageenan until the materials are completely and uniformly dispersed; pre-dispersing 0.2% of acetylated sodium hyaluronate and 0.3% of hydrolyzed hyaluronic acid by using 1.5% of propylene glycol and 0.5% of 1, 3-propylene glycol, adding the mixture into an emulsifying pot, and continuously stirring; after the polymer is completely and uniformly dispersed, 1 percent of trehalose and 2 percent of betaine are added, and the mixture is continuously and uniformly stirred.

And c, slowly adding 12 percent of the microemulsion composition into the emulsifying pot, keeping the stirring speed at 40r/min for continuously stirring for 30min, and after the stirring is uniform, starting the homogenization, wherein the homogenizing speed is 800rpm, and the homogenizing time is 4 min.

And d, adding 0.8% of sodium hydroxide, 0.4% of pentasodium pentetate, 0.5% of p-hydroxyacetophenone and 0.5% of caprylyl hydroximic acid, continuing stirring for 15min, defoaming, discharging and filling to obtain the micro-emulsified skin care emulsion sample.

Example 4:

step a, preparing a micro-emulsified composition:

a1) adding 8% hydrogenated lecithin (PC content is more than or equal to 25%), 14% butanediol, 16% diglycerol and 30% deionized water into an emulsifying pot, uniformly mixing at normal temperature, heating the emulsifying pot to 82 ℃, starting stirring for 45r/min, stirring for 35min, and homogenizing at 6000rpm for 3 min;

a2) adding 20% cetyl ethylhexanoate, 10% meadowfoam seed oil, 0.5% ceramide and 1.5% phytosterol into an oil pan, and heating to 82 ℃;

a3) slowly pumping the oil phase into an emulsifying pot, starting homogenizing at 4000rpm for 6min after the oil phase is pumped;

a4) homogenizing the obtained emulsion under high pressure at 600bar for 2 times, and measuring the particle diameter to 80-300nm to obtain microemulsion composition with particle diameter and particle diameter distribution shown in figure 4.

B, setting the temperature of the emulsifying pot to be 85 ℃, adding 65% of deionized water, preserving heat, sterilizing for 30min, cooling to 44 ℃, starting stirring for 40r/min, adding 0.1% of carrageen crispus, 0.25% of sodium magnesium silicate and 0.15% of hydroxypropyl methyl cellulose until the mixture is completely and uniformly dispersed; pre-dispersing 0.7% of sodium hyaluronate, 0.55% of acetylated sodium hyaluronate and 0.35% of hydrolyzed hyaluronic acid by using 3% of glycerol, 2% of butanediol and 1% of propylene glycol, adding the mixture into an emulsifying pot, and continuously stirring; after the polymer is completely and uniformly dispersed, 1.4 percent of dipotassium glycyrrhizinate, 0.8 percent of allantoin and 2.2 percent of polyquaternium-61 are added and stirred continuously and uniformly.

And c, slowly adding 21% of the microemulsion composition into the emulsifying pot, keeping the stirring speed at 40r/min for continuously stirring for 30min, and after the stirring is uniform, starting the homogenization, wherein the homogenizing speed is 1000rpm, and the homogenizing is performed for 3 min.

And d, adding 0.1% of ethylhexyl glycerol, 0.7% of 1, 2-pentanediol, 0.5% of potassium hydroxide and 1% of triethanolamine, continuously stirring for 12min, defoaming, discharging and filling to obtain the micro-emulsified skin care emulsion sample.

And (3) evaluating the efficacy:

the micro-emulsified skin care emulsion of example 4 was used as a test sample for evaluation of moisturizing efficacy:

subject: selecting 24 subjects, age 20-50 years;

the test method comprises the following steps: cosmetic moisturizing efficacy evaluation guidelines QB/T4256-2011;

test area: the inner side of the forearm;

the using method comprises the following steps: the test sample is (2.0 +/-0.1) mg/cm²The amount of (A) is used for single coating;

the service cycle is as follows: 6 hours;

frequency of use: the disposable use;

and (3) testing period: 0h, 1h, 3h and 6 h; as a blank control before use;

testing parameters: moisture content of stratum corneum was measured using a skin moisture meter Corneometer CM 825 (a.u.)

And (3) testing results: as shown in table 1 and fig. 5.

TABLE 1 stratum corneum moisture content of control and test samples of example 4 (a.u.)

	Before using the product	After using the product for 1h	After using the product for 3 hours	After using the product for 6 hours
					Blank control	27.64	28.38	29.13	29.25
Test sample	25.73	40.30	37.85	35.89

Note: in FIG. 5, significant differences (p <0.05) compared to pre-application are shown

From FIG. 5, it can be seen that an increase in the water content of the stratum corneum means an increase in the water content of the stratum corneum by evaluating the change in the water content of the stratum corneum. Compared with a blank control before using the product, the water content of the stratum corneum of the skin at the using part of the measured sample is remarkably increased after 1h, 3h and 6h of using the product. Therefore, the microemulsified skin care emulsion sample disclosed by the invention has a remarkable moisturizing effect in a test.

The above-mentioned embodiments are only for convenience of description, and are not intended to limit the present invention in any way, and those skilled in the art will understand that the technical features of the present invention can be modified or changed by other equivalent embodiments without departing from the scope of the present invention.

Claims

1. A micro-emulsified skin care emulsion is characterized in that: the micro-emulsified skin care emulsion is prepared from the following raw materials in percentage by mass:

phase B: 5-30% of a microemulsion composition;

2. A microemulsified skin care emulsion according to claim 1 wherein: the water-based thickener is one or a mixture of more than two of xanthan gum, hydroxyethyl cellulose, carbomer, propionic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, carrageenan, crinkle carrageenan, sodium magnesium silicate, hydroxypropyl methyl cellulose and carboxymethyl cellulose.

3. A microemulsified skin care emulsion according to claim 1 wherein: the polyalcohol is one or more of glycerol, propylene glycol, 1, 3-propylene glycol, 1, 2-pentanediol, dipropylene glycol, butanediol and diglycerol.

4. A microemulsified skin care emulsion according to claim 1 wherein: the emollient oil is one or more of hydrocarbon oil such as squalane, hydrogenated polyisobutene, synthetic ester oil and vegetable oil.

5. A microemulsified skin care emulsion according to claim 4 wherein: the synthetic ester grease is any one of caprylic/capric triglyceride, triglyceride (ethyl hexanoate) and cetyl ethyl hexanoate; the vegetable oil is any one of olive oil, chinaroot greenbrier seed oil and shea butter.

6. A microemulsified skin care emulsion according to claim 1 wherein: the ceramide is one or a mixture of more than two of ceramide 1, ceramide 2, ceramide 3 and ceramide 6.

7. A microemulsified skin care emulsion according to claim 1 wherein: the content of PC in the hydrogenated lecithin is more than or equal to 25 percent.

8. A microemulsified skin care emulsion according to claim 1 wherein: the skin conditioner is one or more of sodium hyaluronate, hydrolyzed hyaluronic acid, acetylated sodium hyaluronate, dipotassium glycyrrhizinate, allantoin, panthenol, polyquaternium-61, betaine and trehalose.

9. A microemulsified skin care emulsion according to claim 1 wherein: the preservative is one or a mixture of more than two of phenoxyethanol, chlorphenesin, ethylhexyl glycerol, 1, 2-pentanediol, 1, 2-hexanediol, p-hydroxyacetophenone and caprylyl hydroximic acid; the auxiliary agent is one or a mixture of more than two of EDTA disodium, pentetate, sodium phytate, citric acid, sodium citrate, triethanolamine, arginine, sodium hydroxide and potassium hydroxide.

10. A method of preparing a microemulsified skin care emulsion as claimed in any one of claims 1 to 9, comprising the steps of:

step a, preparing a B-phase microemulsion composition: