CN115737461A - Ion-rich cream and preparation method thereof - Google Patents
Ion-rich cream and preparation method thereof Download PDFInfo
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- CN115737461A CN115737461A CN202211616545.6A CN202211616545A CN115737461A CN 115737461 A CN115737461 A CN 115737461A CN 202211616545 A CN202211616545 A CN 202211616545A CN 115737461 A CN115737461 A CN 115737461A
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Abstract
The invention discloses an ion-rich cream and a preparation method thereof, and the ion-rich cream comprises the following components: 2.5-8% of polyglycerol emulsifier, 2-7% of polypropylene glycol emulsifier, 4-12% of emollient oil, 8-20% of polyalcohol, 0.1-2% of higher fatty alcohol/acid ester, 0.1-3.0% of salt ion and the balance of deionized water. The ion-rich cream disclosed by the invention is characterized in that on the basis of not adding a high-molecular thickening agent, the bonding of an emulsifier and a water phase is influenced through ionic bonds, so that the performance of the emulsifier is changed, and a material body is changed from an emulsion state with good fluidity into a cream state with certain consistency. The cream has good long-term stability, can be added with more ionic active substances with efficacy, and has wide market prospect.
Description
Technical Field
The present invention relates to a cosmetic and a preparation method thereof, and more particularly, to an ion-rich cream and a preparation method thereof.
Background
Water-in-oil systems and oil-in-water systems are two common systems. Wherein the water-in-oil (W/O) emulsion is formed by mixing oil, water and an emulsifier, the system is in a form that the water is dispersed in the oil in a droplet form, the water phase is an internal phase or a dispersed phase, and the oil is an external phase or a dispersed medium; the oil-in-water system is one of the most commonly used emulsification systems for topical cream emulsions, and is represented by O/W, the oilingwater, which is an emulsification system in which an oil is dispersed in water, the oil being the internal phase and the water being the continuous external phase.
Compared with the prior art, the oil-in-water system has the advantages of simple operation, fresh skin feel, better spreadability and the like, but the moisturizing effect is not as good as that of a water-in-oil system (W/O); the water-in-oil type emulsion has smooth appearance, moist and mellow texture, high-efficiency cleaning effect and excellent lubricating effect, but has strong greasy feeling, and is the most common preparation formulation in the aspects of cosmetic production and ointment preparation.
With the vigorous development of the cosmetic consumer market and the rise of the ingredients party and the grass planting economy, more and more consumers are getting to know and pay attention to the efficacy of the cosmetics. The efficacy, safety and other problems of cosmetics are also attracting more and more attention. Corresponding laws and regulations for the declaration and evaluation of the efficacy of cosmetics are issued by the national drug administration in recent two years, wherein corresponding efficacy test reports are required for the declaration of the efficacy, and the declared efficacy of the product can be proved to achieve the expectation. This requires that the amount of efficacy active added in the formulation be added to an effective amount, rather than the earlier concept of adding a declared amount, which is a significant challenge for most cosmetic systems. Since most efficacy actives are highly ionic and highly ionic actives can affect the emulsifying system of the formulation, particularly the thickening system, the highly ionic actives can react with the thickeners in the formulation to form flocs, which can destabilize the system.
At present, the known ion-resistant emulsifying system is only a water-in-oil emulsifying system, naCl is added into the water-in-oil system, the emulsification stability of the system is facilitated, but the skin feeling of water-in-oil smearing is generally more sticky and heavier than that of oil-in-water, and the difficulty of formula design and process regulation is greater than that of the oil-in-water system. In the market, a certain ion-resistant effect is achieved mostly by compounding a thickening agent, but the dosage of the thickening agent is not small, so that a layer of obvious thickening agent membrane feeling is generated after the product is used, the transdermal absorption of an effective active substance is influenced, and the emulsion cream is not favorable for better exerting the effect of the emulsion cream.
For example, chinese patent 201611000114.1 discloses a positively charged oil-in-water nano cream with whitening and spot-removing effects and a preparation method thereof, the positively charged oil-in-water nano cream is a nano cream obtained by adding a high molecular thickener carbomer for thickening, and the positively charged oil-in-water nano cream is a self-charged positive charge of phytosphingosine added in a system, and is not an ionic system.
Therefore, there is a need to provide a high ionic resistance oil-in-water emulsion system to add more ionic efficacy actives and to provide a wider market for the resulting cosmetic product.
Disclosure of Invention
The invention aims to provide an ion-rich cream and a preparation method thereof, the ion-rich cream is prepared from an oil-in-water system by adopting a self-thickening method by adding a salt ion auxiliary emulsifier, the obtained cream has good long-term stability, and more ion type functional active substances can be added, so that the ion-rich cream has better market expectation.
In order to achieve the object of the present invention, in one aspect, the present invention provides an ion-rich cream, which comprises the following components in percentage by weight:
the ion-rich cream has a forming mechanism different from that of the cream in the prior art, and the ion bond formed by the added ions and water influences the bonding between the water phase and the emulsifier on the basis of not adding a high-molecular thickening agent, so that the performance of the emulsifier is changed to achieve the thickening effect, and the cream has good long-term stability.
Because the ion-rich cream of the invention forms ionic bonds through the hydration of the added salt ions and the water in the system, the system of the invention has ionic property, and even more ionic functional active substances are added, the stability of the system is not influenced.
That is, the ion-rich cream of the present invention is prepared by a method of adding salt ions, reducing the action force of the emulsifier and water, and converting the material body from a cream-like state with good fluidity to a cream-like state with a certain consistency.
Because the ion-rich cream is an oil-in-water system and does not adopt a macromolecular thickening agent, the skin feel is more fresh and cool, the spreadability is better, and the efficacy active substance is easier to be absorbed through the skin.
In the invention, in order to overcome the problems in the prior art, the inventor selects to use a polyglycerol emulsifier and a polypropylene glycol emulsifier to be compounded, and the preferable proportion of the compounding is between 1:2 and 4:1. The inventors have found that within the above mentioned ratio ranges, the built emulsifier system can be made into oil-in-water emulsions without thickeners and with small amounts of higher fatty alcohols/acids/acid esters, which tend to aggregate and thicken on contact with ions. In addition, the inventor also discovers that the salt ions are added into the microemulsion prepared by the compound emulsifier system after high pressure, so that the microemulsion has a thickening effect, and the salt ions are added into the microemulsion after high pressure, so that the thickening effect is better.
In the ion-rich cream, the polyglycerol emulsifier is compounded with the polypropylene glycol emulsifier, and the principle is as follows: the HLB value of the selected polyglycerol emulsifier is moderate and is about 8-12, the HLB value of the selected polypropylene glycol emulsifier is low and is about 2-6, and an emulsifying system prepared by compounding the polyglycerol emulsifier and the polypropylene glycol emulsifier is in a more critical but stable state, so that the performance of the emulsifier is easily changed when salt ions are added. The principle of thickening the emulsifying system by the salt ions is as follows: the salt ions can generate stronger hydration with water to form ionic bonds, and the ionic bonds are stronger than the hydrogen bonds generated by the hydration of the compound emulsifier and the water, so that the action of the emulsifier and the water is reduced, the emulsifier is more soluble in an oil phase, and liquid drops are more prone to be gathered together.
In the ion-rich cream of the present invention, the polyglycerol emulsifier is a hydrophilic emulsifier having an HLB value of about 8 to about 12 (e.g., polyglycerol-3-methylglucdistearate HLB value of about 9), which is compatible with electrolytes or active ingredients, and which is non-irritating to the eyes and skin.
In the ion-rich cream, the selected polypropylene glycol emulsifier is an oleophilic emulsifier, has an HLB value of about 2-6 (such as an HLB value of PPG-3 myristyl alcohol ether of about 5), has good stable emulsifying capacity and thickening capacity, and has no irritation to eyes and skin.
The HLB value, called the hydrophilic-hydrophobic balance, also called the water-oil degree, indicates the balance of hydrophilic groups and lipophilic groups in the surfactant molecule. Usually, the HLB value of a nonionic surfactant is in the range of 0 to 20, the HLB value of paraffin wax having the highest hydrophobicity and composed entirely of saturated alkyl groups is 0, the HLB value of polyoxyethylene having the highest hydrophilicity and composed entirely of hydrophilic oxyethylene groups is 20, and the HLB values of other surfactants are in the range of 0 to 20. The greater the HLB value, the more hydrophilic it is, the smaller the HLB value, the more lipophilic it is. However, with the advent of new surfactants, more hydrophilic species have been put into practical use, such as sodium lauryl sulfate having an HLB value of 40.
It is noted that the HLB value, although measurable by some method, is generally about one; in addition, the HLB value can also be calculated by some empirical formula, for example:
HLB＝7+11.7lgM W /M 0
in the formula, M W And M 0 The molecular weights of the hydrophilic group and the lipophilic group in the surfactant molecule, respectively.
Therefore, the HLB value in the present invention cannot be considered mechanically and absolutely. It should also be noted that many surfactants have had HLB values that have not been determined or measured, but this does not mean that the HLB values of many surfactants cannot be determined or calculated.
Preferably, in the ion-rich cream of the present invention, the polyglycerol based emulsifier used may be, but is not limited to, at least one of the following group: polyglyceryl-3 methyl glucose distearate, polyglyceryl-6 distearate, polyglyceryl-3 methyl glucose diisostearate, polyglyceryl-3 beeswax.
Preferably, in the ion-rich cream of the present invention, the polypropylene glycol emulsifier used may be, but is not limited to, at least one of the following group: PPG-2 stearate, PPG-2 oleyl ether, PPG-3 myristyl alcohol ether and PPG-4-cetyl polyether-1.
In the ion-rich cream of the present invention, the salt ions used may be at least one of organic salt ions, inorganic salt ions and ionic efficacy actives; wherein, the preferred organic salt ion includes but is not limited to sodium citrate, and dipotassium glycyrrhizinate, etc., the preferred inorganic salt ion includes but is not limited to magnesium sulfate, sodium chloride, and potassium chloride, etc., the preferred ionic efficacy active substance can be but is not limited to at least one of the following group: calcium PCA, zinc PCA, magnesium PCA, and tripeptide-1 copper, among others. It is noted that certain ionic efficacy actives may also be referred to as organic salt ions, which are not strictly conceptually distinct, but may be substituted for one another in certain instances.
In the ion-rich cream, if PCA zinc is selected as the salt ions, the zinc-rich cream has the effects of resisting bacteria, inhibiting excessive sebum secretion, resisting inflammation, resisting oxidation and the like of a zinc element; if tripeptide-1 copper is selected as the salt ion, the copper can play a role in resisting oxidation, promoting collagen proliferation and assisting wound healing in the action of skin tissues. Various ions are not involved in the human skin metabolic process and the human life activity, so that the ions play a vital role in the processes. For example, epidermal calcium ions can regulate the secretory function of lamellar bodies in cells, and when the concentration of calcium ions in the epidermis is suddenly changed (e.g., the concentration is sharply decreased), a large number of lamellar bodies are secreted, thereby rapidly repairing the skin barrier.
In the ion-rich cream of the present invention, the emollient oil used may be, but is not limited to, at least one of the following group: synthetic ester oil, nonpolar hydrocarbon oil, methyl silicone oil and vegetable oil. Among these, preferred synthetic ester oils include, but are not limited to, dioctyl carbonate, coco-caprylate/caprate, hydrogenated ethylhexyl olivate, caprylic/capric triglyceride, pentaerythritol tetra (ethylhexanoate), cetyl ethylhexanoate, and isopropyl palmitate; preferred non-polar hydrocarbon oils include, but are not limited to, liquid paraffin, hydrogenated polyisobutene, hydrogenated polydecene, and squalane; preferred methyl silicone oils include, but are not limited to, polydimethylsiloxane, methylpolysiloxane, octylmethicone, and phenyl trimethicone; preferred vegetable fats include, but are not limited to, coconut oil, rapeseed oil, olive fruit oil, tocopherols, shea butter, cocoa butter, and meadowfoam seed oil.
In the ion-rich cream of the present invention, the higher fatty alcohol/acid ester used may be, but is not limited to, at least one of the following group: higher fatty alcohols, higher fatty acids, and higher fatty acid esters. Among them, preferred higher fatty alcohols include, but are not limited to, behenyl alcohol, cetyl alcohol, stearyl alcohol, and cetearyl alcohol; preferred higher fatty acids include, but are not limited to, palmitic acid, myristic acid, and behenic acid; preferred higher fatty acid esters include, but are not limited to, stearyl heptanoate and cetyl palmitate.
Further, the ion-rich cream of the present invention may further comprise a skin conditioner in an amount of 0.01% to 5.0% by weight based on the total weight of the cream. Preferred skin conditioning agents may be, but are not limited to, at least one of the following groups: palmitoyl tripeptide-5, acetyl hexapeptide-8, nicotinamide, glycyrrhiza glabra extract, ceramide NS/ceramide NG, ceramide NP, ceramide AP, retinol palmitate, and ascorbyl palmitate.
In the ion-rich cream of the present invention, the polyhydric alcohol used may be, but is not limited to, at least one of glycerin, propylene glycol, 1,2-hexanediol, 1,3-propanediol, butanediol.
Furthermore, the ion-rich cream of the invention can also comprise 0.1-1.0% of preservative based on the total weight of the cream. The preservative can be at least one of, but not limited to, glyceryl caprylate, phenoxyethanol, p-hydroxyacetophenone, caprylyl glycol, and ethylhexyl glycerin.
In another aspect, to achieve the object of the present invention, the present invention also provides a method for preparing the above ion-rich cream, comprising the steps of:
(1) Slowly adding polyglycerol emulsifier, polypropylene glycol emulsifier, higher fatty alcohol/acid ester and skin caring oil ester into an emulsifying cylinder, stirring and melting to uniform state without particles; sequentially adding the polyhydric alcohols while stirring, and stirring to a uniform state;
(2) Adding part of materials to be dissolved and the balance of water into a water phase cylinder, and dissolving until the materials are transparent and have no particles;
(3) After the step (1) and the step (2) are finished, slowly pumping the raw materials in the water phase cylinder into the emulsifying cylinder under the stirring state, and stirring and homogenizing;
(4) After the step (3) is finished, slowly adding the salt ion mixed phase which is uniformly mixed with water in advance and the skin conditioner (if any) into the emulsifying cylinder in sequence under the stirring state, and continuously stirring until the material body is uniform after the completion.
In order to accelerate the dissolution, the emulsification cylinder of step (1) and the aqueous phase cylinder of step (2) may be heated, for example to 75-85 ℃; accordingly, the temperature reduction is carried out in step (3) and step (4), for example, to 25 to 35 ℃ or less.
The ion-rich cream disclosed by the invention is characterized in that on the basis of not adding a high-molecular thickener, the bonding between an emulsifier and a water phase is influenced through ionic bonds, the performance of the emulsifier is changed, and a cream with a certain consistency is changed from an emulsion with good fluidity. The cream has good long-term stability, can be added with more ionic active substances with efficacy, and has wide market prospect.
The present invention will be further described with reference to specific embodiments, but these embodiments are only illustrative of certain specific embodiments of the present invention and are not intended to limit the present invention. It will be apparent to those skilled in the art that various modifications and variations can be made without departing from the principles of the invention, and it is also considered to be within the scope of the invention.
Detailed Description
Preparation experiment of cream
Example 1
The ion-rich cream of example 1 was prepared according to the following process steps:
(1) Setting the temperature of an emulsification cylinder to be 75-85 ℃, sequentially and slowly adding the phase A raw materials into the emulsification cylinder, and stirring and dissolving the phase A raw materials until the phase A raw materials are uniform and free of particles; adding the phase B in sequence while stirring, and stirring to a uniform state;
(2) Setting the temperature of a water phase cylinder to be 75-85 ℃, sequentially adding the C-phase raw material into the water phase cylinder, and heating and dissolving until the C-phase raw material is transparent and granular-free;
(3) After the above process is completed, slowly pumping the raw materials in the water phase cylinder into the emulsifying cylinder under the stirring state, stirring and homogenizing for 3-5 minutes, and then opening and cooling to 25-35 ℃;
(4) After the above process is completed, under the stirring state, slowly adding the uniformly pre-mixed D phase into the emulsifying cylinder, cooling the emulsifying cylinder after the completion, continuously stirring until the material body is uniform, and discharging.
The raw material formula of the ion-rich cream in example 1 is as follows:
example 2
The preparation method of the ion-rich cream of example 2 is substantially the same as that of example 1. The raw material formulation used in example 2 was as follows:
example 3
The preparation method of the ion-rich cream of example 3 is substantially the same as that of example 1. The raw material formulation used in example 3 was as follows:
comparative example
The cosmetic products of comparative examples 1-5 were prepared according to the preparation method of example 1, but using the raw material formulations as shown in table 1:
table 1 comparative (example) formulations 1-5 and resulting product evaluations:
from the products prepared in comparative examples 1 to 5, it was found that the ion-rich cream of the present invention could not be successfully prepared by using only the polyglycerol based emulsifier (hydrophilic emulsifier) in combination with other non-polypropylene glycol type oleophilic emulsifiers, or only the polypropylene glycol type emulsifier in combination with other non-polyglycerol based hydrophilic emulsifiers, or by using other hydrophilic and lipophilic emulsifiers other than the polyglycerol based emulsifier and the polypropylene glycol type emulsifier; in comparative example 2, both a polyglycerol emulsifier and a polypropylene glycol emulsifier were used, but the product performance was not satisfactory because the content of the polypropylene glycol emulsifier was only about 1%.
Test experiments on creams
1. And (3) stability testing:
the stability of the ion-rich creams prepared in example 1, example 2 and example 3 was evaluated and the results are summarized in table 2.
Table 2 stability test report:
note: in the table, A indicates no change in appearance and properties; b shows that the appearance and the properties are slightly changed and the viscosity is reduced; c represents a large change in appearance and properties, demixing or demulsification
2. And (3) viscosity testing:
the ion-rich creams prepared in example 1, example 2 and example 3 were subjected to viscosity testing, and the results are summarized in table 3.
Table 3 viscosity test results:
from the experimental results of table 3, it can be seen that the viscosity of the body increases greatly upon addition of the salt ion.
3. And (3) particle size testing:
the ion-rich creams prepared in example 1, example 2 and example 3 were subjected to particle size testing, and the experimental results are summarized in table 4.
Table 4 particle size test results
From the experimental results of table 4, it was found that the particle size hardly changed significantly after the addition of the salt ion, although the viscosity of the material body was greatly increased. This indicates that the change in appearance of the product from emulsion to cream is not due to a change in the size of its particles, but rather to an increase in viscosity due to aggregation between the particles.
Claims (10)
1. An ion-rich cream, which comprises the following components in percentage by weight:
2. the cream of claim 1, wherein the polyglycerol-based emulsifier is a hydrophilic emulsifier having an HLB value of about 8 to 12, and the polypropylene glycol-based emulsifier is an oleophilic emulsifier having an HLB value of about 2 to 6.
3. The cream of claim 1, wherein the polyglycerol-based emulsifier is at least one selected from the group consisting of: polyglyceryl-3-methylglucose distearate, polyglyceryl-6-distearate, polyglyceryl-3-methylglucose diisostearate, polyglyceryl-3-beeswax.
4. The cream according to claim 1, wherein the polypropylene glycol-based emulsifier is at least one selected from the group consisting of: PPG-2 stearate, PPG-2 oleyl ether, PPG-3 myristyl alcohol ether and PPG-4-cetyl polyether-1.
5. The cream of claim 1, wherein the salt ion is selected from at least one of the group consisting of: organic salt ions, inorganic salt ions and ionic efficacy actives; wherein the organic salt ions comprise sodium citrate and dipotassium glycyrrhizinate, and the inorganic salt ions comprise magnesium sulfate, sodium chloride and potassium chloride; the ionic efficacy actives include calcium PCA, zinc PCA, magnesium PCA, and the tripeptide-1 copper.
6. The cream of claim 1, wherein the emollient oil is at least one selected from the group consisting of: synthetic ester oil, nonpolar hydrocarbon oil, methyl silicone oil, and vegetable oil; wherein the synthetic ester oil comprises dioctyl carbonate, coco-caprylate/caprate, hydrogenated ethylhexyl olivate, caprylic/capric triglyceride, pentaerythritol tetra (ethyl hexanoate), cetyl ethyl hexanoate, and isopropyl palmitate; the nonpolar hydrocarbon oil comprises liquid paraffin, hydrogenated polyisobutene, hydrogenated polydecene and squalane; the methyl silicone oil comprises polydimethylsiloxane, methyl polysiloxane, octyl polymethylsiloxane and phenyl polytrimethylsiloxane; the vegetable oil comprises coconut oil, rapeseed oil, olive fruit oil, tocopherol, shea butter, cocoa seed fat and meadowfoam seed oil.
7. The cream of claim 1, wherein the higher fatty alcohol/acid ester is at least one selected from the group consisting of: higher fatty alcohols, higher fatty acids, and higher fatty acid esters; wherein the higher fatty alcohol comprises behenyl alcohol, cetyl alcohol, stearyl alcohol and cetearyl alcohol; the higher fatty acid comprises palmitic acid, myristic acid and behenic acid; the higher fatty acid ester comprises stearyl heptanoate and cetyl palmitate.
8. The cream of claim 1, wherein the cream further comprises 0.01% to 5.0% of a skin conditioning agent.
9. The cream of claim 8, wherein the skin conditioning agent is at least one selected from the group consisting of: palmitoyl tripeptide-5, acetyl hexapeptide-8, nicotinamide, glycyrrhiza glabra extract, ceramide NS/ceramide NG, ceramide NP, ceramide AP, retinol palmitate, and ascorbyl palmitate.
10. A process for preparing a cream according to any one of claims 1 to 9, comprising the steps of:
(1) Slowly adding polyglycerol emulsifier, polypropylene glycol emulsifier, higher fatty alcohol/acid ester and emollient oil ester into an emulsifying cylinder, stirring and melting to be uniform and particle-free; sequentially adding the polyhydric alcohols while stirring, and stirring to a uniform state;
(2) Adding part of materials to be dissolved and the balance of water into a water phase cylinder, and dissolving the materials to be dissolved and the balance of water until the materials are transparent and have no particles;
(3) After the step (1) and the step (2) are finished, slowly pumping the raw materials in the water phase cylinder into the emulsifying cylinder under the stirring state, and stirring and homogenizing;
(4) After the step (3) is finished, slowly adding the salt ion mixed phase which is uniformly mixed with water in advance and the skin conditioner (if any) into the emulsifying cylinder in sequence under the stirring state, and continuously stirring until the material body is uniform after the completion.
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Citations (4)
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|---|---|---|---|---|
| CN101584647A (en) * | 2008-05-20 | 2009-11-25 | 赢创德固赛(中国)投资有限公司 | Polylol-in-oil composition with high vitamin C content and preparation method thereof |
| CN106999414A (en) * | 2014-12-03 | 2017-08-01 | 欧莱雅 | Include the composition of self-association type polyurethane, fatty alcohol or acid, nonionic surfactant and pigment |
| CN107007481A (en) * | 2017-04-18 | 2017-08-04 | 上海相宜本草化妆品股份有限公司 | A kind of multiple emulsion compositons and preparation method thereof |
| CN114099357A (en) * | 2021-11-30 | 2022-03-01 | 江苏瑞霆生物科技有限公司 | Hydroxytyrosol-containing polyol-in-oil nano emulsion, and preparation method and application thereof |
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2022
- 2022-12-15 CN CN202211616545.6A patent/CN115737461A/en active Pending
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| CN101584647A (en) * | 2008-05-20 | 2009-11-25 | 赢创德固赛(中国)投资有限公司 | Polylol-in-oil composition with high vitamin C content and preparation method thereof |
| CN106999414A (en) * | 2014-12-03 | 2017-08-01 | 欧莱雅 | Include the composition of self-association type polyurethane, fatty alcohol or acid, nonionic surfactant and pigment |
| CN107007481A (en) * | 2017-04-18 | 2017-08-04 | 上海相宜本草化妆品股份有限公司 | A kind of multiple emulsion compositons and preparation method thereof |
| CN114099357A (en) * | 2021-11-30 | 2022-03-01 | 江苏瑞霆生物科技有限公司 | Hydroxytyrosol-containing polyol-in-oil nano emulsion, and preparation method and application thereof |
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