CN111135115A - Composition containing calamine - Google Patents

Composition containing calamine Download PDF

Info

Publication number
CN111135115A
CN111135115A CN201811313109.5A CN201811313109A CN111135115A CN 111135115 A CN111135115 A CN 111135115A CN 201811313109 A CN201811313109 A CN 201811313109A CN 111135115 A CN111135115 A CN 111135115A
Authority
CN
China
Prior art keywords
calamine
composition
weight
thickener
present
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201811313109.5A
Other languages
Chinese (zh)
Other versions
CN111135115B (en
Inventor
朱沁
丛远华
郑中博
冯春波
倪向梅
乔小玲
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shanghai Jahwa United Co Ltd
Original Assignee
Shanghai Jahwa United Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shanghai Jahwa United Co Ltd filed Critical Shanghai Jahwa United Co Ltd
Priority to CN201811313109.5A priority Critical patent/CN111135115B/en
Publication of CN111135115A publication Critical patent/CN111135115A/en
Application granted granted Critical
Publication of CN111135115B publication Critical patent/CN111135115B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/27Zinc; Compounds thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/26Aluminium; Compounds thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73Polysaccharides
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/10General cosmetic use

Abstract

The invention discloses a composition containing calamine, which comprises a combination of an inorganic salt thickening agent and a polysaccharide thickening agent, wherein the weight percentage of the inorganic salt thickening agent is equal to or more than 2%, and the weight percentage of the polysaccharide thickening agent is equal to or more than 1%. The invention also discloses the use of the composition in personal care products.

Description

Composition containing calamine
Technical Field
The present invention relates to calamine-containing compositions, and in particular to aqueous dosage forms of compositions that can carry high levels of calamine.
Background
Calamina is a mineral common medicine, has a long history of medicine taking in China, and can be traced back to Shaoxing school Jing Shuxiong Stan-type emergent materia Medica in the period of south and Song. It is sweet and warm in nature and flavor, enters liver, spleen and lung meridians, and has the effects of removing toxic substance, improving eyesight, removing nebula, astringing dampness, relieving itching and healing sore. All the classic records of Chinese and Western medicine are recorded. Clinically, Galamina is one of the commonly used medicines in dermatology and mainly treats unhealing ulcer, dribbling pus, eczema, skin pruritus and various rashes (such as urticaria, miliaria, eczema and the like). Because the calamine gives consideration to excellent efficacy and safety, the calamine is also widely applied to various diseases which are easy to occur in pediatrics, such as: umbilical cord infection, infantile red buttock, infantile eczema and dermatitis caused by improper nursing of the umbilical cord of the newborn.
Because of the excellent therapeutic effect of calamine on the treatment of skin diseases, it has been in the medical industry. In recent years, along with the pursuit of natural skin care ingredients by consumers, calamine is gradually recognized and accepted by consumers. But worth the attention of the researchers, because the calamine is the natural ore powder, the required onset of action is relatively high, for example, in the 2 nd edition of the Chinese hospital preparation standard, western medicine preparation, the addition of the calamine is 15%. The series of characteristics and requirements determine that the calamine is stably added into a preparation or a finished skin care product, and has very convenient use and use experience, so that the series of characteristics and requirements have great challenges.
Currently, in the fields of medicine and cosmetics, the formulations related to calamine are roughly divided into three types: powders, oils and aqueous formulations.
1) Powder preparation: the powder is a pure traditional Chinese medicine powder, has the functions of diminishing inflammation, relieving pain, astringing, removing the necrotic tissue, promoting granulation and promoting wound healing, but has the disadvantages of easy flying dust dispersion, easy inhalation into respiratory tract and lung, difficult attachment to the coating position and inconvenient use.
2) Oil formulation: by proper combination of fats and oils, high levels of calamine can be uniformly dispersed therein and stabilized, which is an advantage. But also the skin feel of the spread on the skin is not so good because of the large amount of oil. CN 108024946 a disperses up to 30% of the glycerin in the emu and jojoba oil combination, but the patent also clearly indicates that the skin feel is too sticky.
3) The water preparation formulation: this dosage form is the most widely used. Referring to the 2 nd edition of the Chinese Hospital preparation Standard, Western medicine preparation, the prescription of calamine: 150g of calamine, 50g of zinc oxide, 10ml of liquefied phenol, 50ml of glycerol and distilled water added to 1000 ml. Wherein the content of the calamine is up to 15 percent, but the prescription of the suspension has the defects of quick particle sedimentation, easy bottle bottom adhesion and difficult dispersion in the preparation and storage processes. This results in non-uniform drug concentration and is inconvenient for use. In addition, the improvement of the preparation process of calamine lotion and the comparison of clinical effects in the 14 th phase of 2017 of the Chinese Mongolian medicine indicate that the non-uniform dispersion liquid with inconsistent particle sizes is easy to settle and delaminate due to the particle size of the suspension agent being between 0.5 and 10 mu m. It is extremely difficult to control the stability of the suspension to keep the fine and uniform size of the drug particles and to achieve a high quality aqueous suspension. A similar preparation was used in CN 102935054A and CN 107019653A. CN 107496178A stably disperses calamine in cream and has a skin feel, but also because calamine is difficult to be added, the final addition amount of the cream does not reach the level of hospital preparations, and calamine is used only for the effect of correcting skin complexion. In addition, CN 107802511 a dispersed calamine in polyol as an intermediate added to the final product. Therefore, the content of calamine in the final product is 0.42-1.95%. There is also an order of magnitude difference from the prescribed dose.
In conclusion, there is still a need to find a calamine-containing product which can achieve the hospital preparation level and similar medicinal efficacy, and has good skin feel and good stability, and the calamine-containing product has very important application value.
Disclosure of Invention
The invention aims to provide a stable calamine composition. The composition can carry high-content calamine by adopting a composition of an inorganic salt thickening agent and a polysaccharide thickening agent. In addition, the composition has good stability, and also has good skin-smearing and washing-off properties.
In one aspect, the present invention provides a composition comprising calamine, said composition comprising a combination of an inorganic salt-based thickener and a polysaccharide-based thickener, said inorganic salt-based thickener being present in an amount of 2% by weight or more and said polysaccharide-based thickener being present in an amount of 1% by weight or more, based on the weight of the composition.
In a preferred embodiment, the weight percentage of the inorganic salt-based thickener is equal to or greater than 2.5%, and the weight percentage of the polysaccharide-based thickener is equal to or greater than 1.5%.
In a preferred embodiment, the weight ratio of the inorganic salt-based thickener to the polysaccharide-based thickener is 5: 3.
In a preferred embodiment, the inorganic salt-based thickener is aluminum magnesium silicate, and the polysaccharide-based thickener is xanthan gum.
In a preferred embodiment, the calamine composition of the present invention further comprises an additional thickener selected from the group consisting of: polyacrylic acids, acryloyl dimethyltaurate copolymers, cellulosics, carbomers.
In a preferred embodiment, the composition further comprises glycerin.
In a preferred embodiment, the composition further comprises phenoxyethanol.
In a preferred embodiment, the weight percentage of calamine in the composition is equal to or greater than 15% by weight of the composition.
In another aspect, the present invention is also directed to a mask product comprising the calamine composition of the present invention.
In another aspect, the present invention also relates to the use of the calamine compositions of the present invention in personal care products.
Detailed Description
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention, the preferred methods and materials are described herein. For the purposes of the present invention, the following terms are defined below.
The term "about" as used herein refers to an amount, level, value, dimension, size, or amount that differs by up to 30%, 20%, or 10% as compared to the amount, level, value, dimension, size, or amount of a reference. The percentages used herein are by weight unless otherwise indicated.
Throughout the specification and claims, unless the context requires otherwise, the word "comprise", and variations such as "comprises" and "comprising", will be understood to imply the inclusion of a stated integer or step or group of integers or steps but not the exclusion of any other integer or step or group of integers or steps.
In the present description and claims, unless otherwise specified, the contents of the components in the mixture refer to their weight percentages.
The present invention is based on the following unexpected findings: the combination of inorganic salt-based thickeners and polysaccharide-based thickeners in certain proportions not only provides for high loading of calamine (e.g., at least 15 wt.%), but also provides for stable and easy-to-apply and rinse-off calamine compositions (e.g., personal care products).
Therefore, the inorganic salt thickening agent and the polysaccharide thickening agent are compounded for the first time to bear high-content calamine, so that the stable high-content calamine composition is formed. In addition, when the composition of the present invention is applied to a personal care product, a stable personal care product carrying high levels of calamine can be formed that is easy to apply and wash off.
The invention provides an aqueous calamine composition. That is, a significant amount of water is included in the calamine compositions of the present invention. For example, in some embodiments, the water content of the calamine compositions of the present invention is greater than 50% by weight. In some more preferred embodiments, the water content in the calamine composition of the present invention is greater than 60% by weight. In some more preferred embodiments, the water content in the calamine composition of the present invention is greater than 68% by weight.
The biggest technical problem for aqueous compositions is their stability. The present inventors have investigated the effect of various thickeners on the stability of calamine compositions and have found that the desired stabilizing effect cannot be achieved with thickeners alone. However, the present inventors have surprisingly found that a stable aqueous calamine composition is achieved by using a combination of an inorganic salt-type thickener and a polysaccharide-type thickener. In some embodiments, the inorganic salt-based thickening agent is present in the calamine compositions of the present invention in an amount equal to or greater than 2% by weight. In some preferred embodiments, the inorganic salt-based thickening agent is present in the calamine compositions of the present invention in an amount equal to or greater than 2.5% by weight. In some embodiments, the polysaccharide thickener is present in the calamine compositions of the present invention in an amount equal to or greater than 1% by weight. In some preferred embodiments, the polysaccharide thickener is present in the calamine compositions of the present invention in an amount equal to or greater than 1.5% by weight.
In some embodiments, the weight ratio of inorganic salt-based thickener to polysaccharide-based thickener in the calamine compositions of the present invention is from 5:1 to 1: 1. The weight ratio of the inorganic salt thickening agent to the polysaccharide thickening agent in the calamine composition is 4:1 to 1: 1. In some preferred calamine compositions of the present invention the weight ratio of inorganic salt-based thickening agent to polysaccharide-based thickening agent is from 2:1 to 1: 1. In a most preferred embodiment, the weight ratio of inorganic salt-based thickener to polysaccharide-based thickener in the calamine composition of the present invention is 5: 3.
The inorganic salt as main thickener includes natural or synthetic composite silicate, including magnesium aluminum silicate, sodium magnesium silicate, lithium magnesium silicate, sodium lithium magnesium silicate, bentonite, modified bentonite, montmorillonite, modified montmorillonite, diatomite, etc.
Any conventional inorganic salt-type thickener can be used in the aqueous calamine composition of the present invention, and for example, magnesium aluminum silicate can be used. An example of magnesium aluminum silicate is that sold under the trade name sumeccton-SA by Kunimine Industries, ltd.
The polysaccharide thickener mainly comprises polygalactose, polymannan, polyglucose, mucopolysaccharide and other thickeners, such as: acacia, sodium alginate, deacetylated polysaccharide, hyaluronic acid, xanthan gum, etc.
Any conventional polysaccharide thickener may be used in the aqueous calamine composition of the present invention, and for example, xanthan gum may be used. Xanthan gum is also known as xanthan gum. An example of xanthan gum is that sold under the trade name GRINDSTED Xanthan 200 by DANISCO.
Any other conventional thickening agent may also be employed in the aqueous calamine composition of the present invention.
For example, the calamine composition further comprises an acryloyl dimethyl taurate copolymer-based thickener. In particular embodiments, the acryloyl dimethyl taurate copolymer-based thickener used includes EMT10 sold under the trade name SEPINOVEMT10 by SEPPIC corporation; simugel EG sold by SEPPIC under the name Simulgel EG; AVC sold under the trade name Aristoflex AVC by CLARIANT, Inc., and the like.
For example, the calamine compositions of the present invention also comprise a carbomer-based thickener. In particular embodiments, carbomer-based thickeners used include carbomer 980, sold by ROBOLUN corporation under the trade name Carbopol 980 Polymer; carbomer U-21 sold under the trade name Carbopol ultrez 21polymer by Lumbo, Inc., and the like.
For example, the calamine compositions of the present invention also comprise a polyacrylic thickener. In particular embodiments, polyacrylic thickeners used include Sepiplus400 sold under the trade name Sepiplus400 by SEPPIC corporation; polyacrylic acid POLYMER TR-1 sold under the trade name PemulentTR-1 POLYMER by Lumbo; acrylic copolymer AQF sold under the trade name DERMACRYL AQF by akzo nobel corporation; sodium polyacrylate Polymer Dispersion SPL sold by BASF corporation under the trade name Cosmedia SPL, and the like.
For example, the calamine compositions of the present invention also comprise a cellulosic thickener. In a particular embodiment, cellulosic thickeners used include those available under the trade name ASHLAND
Figure BDA0001855539980000051
Hydroxyethyl cellulose sold by 250HR Hydroxytylcellulose.
In some embodiments, glycerol is also included in the calamine compositions of the present invention. In a preferred embodiment, the calamine composition of the present invention comprises 10-15% by weight glycerol.
In some embodiments, the calamine compositions of the present invention further comprise a preservative. In a preferred embodiment, the calamine composition of the present invention comprises 0.1 to 1% by weight of a preservative. In a particular embodiment, the preservative used in the calamine composition of the present invention is phenoxyethanol.
In a preferred embodiment, calamine having a particle size of 3 μm or less is used to prepare the calamine composition of the present invention. In a specific embodiment, the present invention employs calamine sold by Union micropowder corporation.
The compositions of the present invention can carry high levels of calamine. For example, the composition of the invention may carry up to 15% by weight calamine. In a preferred embodiment, the composition of the invention may carry up to 20% by weight calamine. In a more preferred embodiment, the composition of the invention may carry up to 25% by weight calamine. In a more preferred embodiment, the composition of the invention may carry up to 30% by weight calamine. In a more preferred embodiment, the composition of the invention may carry up to 35% by weight calamine. In a more preferred embodiment, the composition of the invention may carry up to 40% by weight calamine.
The present invention also relates to a mask product comprising the calamine composition of the present invention. The high calamine-bearing composition of the present invention can be used in a variety of personal care products, such as facial masks. In some embodiments, the personal care product may be a skin care product. For example, the personal care product may be a rinse-off skin care product of the spread type. In a particular embodiment, the personal care product is a mask.
Detailed Description
The technical aspects of the present invention will be described in detail below with reference to preferred embodiments, but the scope of the present invention is not limited to these embodiments, and the technical aspects of the present invention are intended to be described and not limited. Test methods in which specific conditions are not specified in the following examples are generally carried out under conventional conditions or under conditions recommended by the manufacturer. All percentages and parts are by weight unless otherwise indicated.
The raw materials used in the examples of the present invention and their manufacturers are shown in table 1.
TABLE 1
Figure BDA0001855539980000061
Figure BDA0001855539980000071
The experimental apparatus used in the embodiment of the present invention includes:
1. fixed agitator IKA RW20
2. Weighing balance METTLER TOLEDO PL602-S
3. HWS 28 model of constant temperature water bath Shanghai-Hengchun scientific instruments Co., Ltd
Examples 1 to 48: preparation of calamine-containing composition
An aqueous composition containing calamine was prepared with the components shown in table 2. The method comprises the following specific steps: weighing deionized water, starting a fixed stirrer at a rotating speed of 1000-2000 r/min, adding the thickening agent, and stirring for 20-30 min until the thickening agent is completely dissolved and no particles exist; keeping stirring state, respectively adding glycerol and phenoxyethanol, stirring for 5 minutes at the rotation speed of 1000 r/min-2000 r/min until the glycerol and the phenoxyethanol are completely dissolved in the material body. Keeping the stirrer in an opening state, slowly adding 15 parts by mass of calamine at the rotating speed of 1000 r/min-2000 r/min, and stirring for 5 minutes after the calamine is completely added until the calamine is completely dispersed in the material body. And finally, complementing the rest deionized water to 100%, and stirring for 1-2 minutes until the material body is uniform.
Figure BDA0001855539980000091
Figure BDA0001855539980000101
Figure BDA0001855539980000111
Figure BDA0001855539980000121
Test example 1: stability Studies for the compositions of examples 1-48
The stability evaluation method is that the sample is placed in three stable constant temperature boxes of-10 ℃, normal temperature (25 ℃) and 40 ℃, and the condition that whether the material body has the state change (whether the material body is layered or not, whether the material body has water or not, unevenness and the like) is examined for one month, if the material body is not normally changed before and after a certain temperature condition for one month, ○ is shown, and the change shows delta, and the result is shown in Table 3.
TABLE 3
Figure BDA0001855539980000131
Figure BDA0001855539980000141
As shown in Table 3, different types of single thickeners were selected to stabilize the calamine powder, among which the acrylic dimethyltaurate copolymer thickeners such as EMT10, Simugel EG, AVC, in the range that the formulation could be added, in an attempt to add various proportions of the thickeners, but at each temperature did not stabilize the calamine in the formulation well.
The carbomer thickening agent commonly used by people selects 2 commonly used raw materials of carbomer 980 and carbomer U-21, and the conventional amount proportion or the proportion higher than the conventional amount is tried to be added into the formula, but the calamine cannot be well supported at each temperature.
In addition, xanthan gum, sodium alginate and guar gum, which are the most commonly used polysaccharide thickeners, were chosen, with the result that also the loading of calamine was not very stable.
Attempts have also been made to use polyacrylic thickeners, such as: sepiplus400, polyacrylic acid polymer TR-1, acrylic acid (ester) copolymer AQF and sodium polyacrylate polymer dispersion SPL, most of which can not stabilize calamine. Only Sepiplus400 after addition to 1.5 parts by mass and 2 parts by mass passed the stability test at normal temperature, and the stability at the remaining temperatures was still failed.
After the cellulose thickener hydroxyethyl cellulose is added into 1 part by mass, the formula can be stable at normal temperature, but cannot be stable at high temperature of 40 ℃.
Inorganic salt thickening agents of magnesium aluminum silicate, bentonite and diatomite are selected, and after 2 parts by mass of magnesium aluminum silicate is added into a formula, the magnesium aluminum silicate can be stable at minus 10 ℃ and 25 ℃, but the stability at the high temperature of 40 ℃ cannot pass. The load bearing capacity of both bentonite and diatomaceous earth is not ideal.
It follows that the use of a single thickener in the formulation to stabilise a large amount of calamine does not give the desired effect.
Test example 2: smear and rinse-off evaluation for the compositions of examples 1-48
The smearing evaluation method was as follows: taking a test area with the area of 4cm x 4cm at the inner side of the front arm, smearing 1 g of sample, and smearing clockwise for 10 circles, wherein the sample is not easy to smear and the background color of the exposed skin in the test area is 0 min; the skin is easy to apply, but the bottom color of the exposed skin in the test area is 1 minute; the skin is not easily smeared but the bottom color of the skin is not exposed in the test area for 1 minute; the sample can be easily spread and the test area does not reveal a base color of 2 points (best for 2 points). The results are shown in Table 4.
The washout evaluation method was as follows: a4 cm by 4cm area of the inner side of the forearm was applied with 1 g of the sample, and after 5 minutes of application, the area was rinsed with flowing water at the same flow rate for 60 seconds, with 0 minutes for no wash, 1 minute for partial wash, and 2 minutes for complete wash (2 minutes is the best). The results are shown in Table 4.
TABLE 4
Figure BDA0001855539980000161
Figure BDA0001855539980000171
As shown in Table 4, the smearing feeling by using Sepiplus400 was uniform in the case of using a thickener based on an acryloyl dimethyltaurate copolymer, and the washability was general in the case of using more than 1 part by mass. When the polyacrylic acid polymer TR-1 was used, the coating feeling was satisfactory only when the amount of addition was 2 parts by mass, but the washability was not satisfactory. When the acrylic acid (ester) copolymer AQF is used, the coating feeling is more desirable when the amount is 1 part by mass, but the washability is also not desirable.
The use of formulations of the acryloyl dimethyl taurate copolymers can achieve ideal smear feel, but none are well washable.
All formulations using cellulose as thickener have good spreadability, but the same washability is not ideal.
Formulations using carbomers as thickeners provide good rinse-off feel at low levels of addition, but are not ideal for application.
The formula using inorganic salts of magnesium aluminum silicate, bentonite and diatomite as the thickening agent can meet the ideal smearing property and the ideal washing feeling.
Polysaccharide xanthan gum is used as a thickening agent, when the addition amount is 1 part by mass and the addition amount of sodium alginate is 0.5 part by mass, ideal smearing feeling and washing-off effect can be achieved at the same time, and the two can not be met at the same time by other use amounts.
Examples 49 to 77: preparation of calamine-containing composition
An aqueous composition containing calamine was prepared with the components shown in table 5. The method comprises the following specific steps: weighing deionized water, starting a fixed stirrer at a rotating speed of 1000-2000 r/min, adding the thickening agent, and stirring for 20-30 min until the thickening agent is completely dissolved and no particles exist; keeping stirring state, respectively adding glycerol and phenoxyethanol, stirring for 5 minutes at the rotation speed of 1000 r/min-2000 r/min until the glycerol and the phenoxyethanol are completely dissolved in the material body. Keeping the stirrer in an opening state, slowly adding the calamine at the rotating speed of 1000 r/min-2000 r/min, and stirring for 5 minutes after the calamine is completely added until the calamine is completely dispersed in the material body. And finally, complementing the rest deionized water to 100%, and stirring for 1-2 minutes until the material body is uniform.
Figure BDA0001855539980000191
Figure BDA0001855539980000201
Figure BDA0001855539980000211
Test example 3: stability Studies for the compositions of examples 49-77
The stability evaluation method was carried out by placing the sample in three stable thermostats at-10 deg.C, room temperature (25 deg.C) and 40 deg.C, examining for one month to see if the material had morphological changes (such as delamination, bleeding, unevenness, etc.), if the material had not changed before and after a certain temperature condition for one month, ○ was indicated, and Δ was indicated by the change, as shown in Table 6.
TABLE 6
Figure BDA0001855539980000221
Figure BDA0001855539980000231
As shown in table 6, attempts to stabilize calamine in the formulation with xanthan gum in combination with polyacrylic thickeners did not have the desired stability at each temperature.
The xanthan gum and the acryloyl dimethyl taurate copolymer are matched and combined, and the stability is not good at various temperatures.
The xanthan gum is matched with a cellulose thickener, and the formula can have an ideal stable state.
Xanthan gum in combination with carbomer thickeners does not stabilize calamine well in the formulation.
The xanthan gum is matched with an inorganic salt thickener, namely magnesium aluminum silicate, so that an ideal stable state can be achieved.
The use of xanthan gum in combination with 3 thickeners, cellulose and polyacrylic acid, was attempted to achieve a stable formulation when xanthan gum was 2 parts by mass, hydroxyethyl cellulose was 1 part by mass, and sodium polyacrylate polymer dispersion SPL was 1 part by mass.
When 3 kinds of thickeners including xanthan gum, cellulose and inorganic salt are combined, a large amount of calamine in the formula can be stabilized when 1 part by mass of xanthan gum, 0.3 part by mass of hydroxyethyl cellulose and 2 parts by mass of magnesium aluminum silicate are used. The stability of other dosage is not ideal.
Test example 4: smear and washout evaluations for the compositions of examples 49-77
The smearing evaluation method was as follows: taking a test area with the area of 4cm x 4cm at the inner side of the front arm, smearing 1 g of sample, and smearing clockwise for 10 circles, wherein the sample is not easy to smear and the background color of the exposed skin in the test area is 0 min; the skin is easy to apply, but the bottom color of the exposed skin in the test area is 1 minute; the skin is not easily smeared but the bottom color of the skin is not exposed in the test area for 1 minute; the sample can be easily spread and the test area does not reveal a base color of 2 points (best for 2 points).
The washout evaluation method was as follows: a4 cm by 4cm area of the inner side of the forearm was applied with 1 g of the sample, and after 5 minutes of application, the area was rinsed with flowing water at the same flow rate for 60 seconds, with 0 minutes for no wash, 1 minute for partial wash, and 2 minutes for complete wash (2 minutes is the best). The results are shown in Table 7.
TABLE 7
Figure BDA0001855539980000241
Figure BDA0001855539980000251
As shown in Table 7, most of the formulations using xanthan gum in combination with polyacrylic thickener gave good spreadability, but at the same time the washout was not very good.
Most of the Chinese xanthan gum and the acryloyl dimethyl taurate copolymer have good spreadability, but the washability is not satisfactory.
The formula of the xanthan gum matched with the cellulose thickening agent has good spreadability, but is difficult to wash.
The formula of the xanthan gum matched with the carbomer thickening agent has common smearing property and common washing property in most formulas.
The formula of the xanthan gum matched with the inorganic salt thickener magnesium aluminum silicate can simultaneously meet the requirements of good smearing property and good washing property.
The formula of using xanthan gum in combination with 3 thickeners, cellulose and polyacrylic acid, is good in smearing property, but poor in washing property.
When the xanthan gum is combined with 3 thickening agents of cellulose and inorganic salt, the smearing property of the same formula is good, but the xanthan gum is difficult to wash off.
Comparative examples 1 to 12: preparation of calamine-containing composition
An aqueous composition containing calamine was prepared with the components shown in table 8. The method comprises the following specific steps: weighing deionized water, starting a fixed stirrer at a rotating speed of 1000-2000 r/min, adding aluminum magnesium silicate, and stirring for 30-40 min until the aluminum magnesium silicate is completely dissolved and no particles exist; uniformly dispersing xanthan gum and glycerin, adding the mixture into the material body, keeping a stirrer on, stirring for 15-20 minutes at the rotation speed of 1000-2000 r/min until the mixture is uniformly dispersed and has no particles; adding phenoxyethanol, and stirring for 5 minutes at the rotating speed of the stirrer of 1000-2000 r/min; keeping the stirrer in an open state, slowly adding the calamine at the rotating speed of 1000 r/min-2000 r/min, and stirring for 5-10 min after the calamine is completely added until the calamine is completely dispersed in the material body. And finally, complementing the rest deionized water to 100%, and stirring for 1-2 minutes until the material body is uniform.
TABLE 8
Calamine (Calamina) Glycerol Phenoxyethanol Deionized water Magnesium aluminum silicate Chinese gum
Comparative example 1 15 12 0.5 To 100 0.5 0.5
Comparative example 2 15 12 0.5 To 100 0.5 1
Comparative example 3 15 12 0.5 To 100 0.5 1.5
Comparative example 4 15 12 0.5 To 100 1 0.5
Comparative example 5 15 12 0.5 To 100 1 1
Comparative example 6 15 12 0.5 To 100 1 1.5
Comparative example 7 15 12 0.5 To 100 1.5 0.5
Comparative example 8 15 12 0.5 To 100 1.5 1
Comparative example 9 15 12 0.5 To 100 1.5 1.5
Comparative example 10 15 12 0.5 To 100 2 0.5
Comparative example 11 15 12 0.5 To 100 2 1
Comparative example 12 15 12 0.5 To 100 2.5 1
Example 66 15 12 0.5 To 100 2.5 1.5
Test example 5: stability Studies on the compositions of comparative examples 1-12
The stability evaluation method was carried out by placing the sample in three stable thermostats at-10 deg.C, room temperature (25 deg.C) and 40 deg.C, examining for one month to see if the material had morphological changes (such as delamination, bleeding, unevenness, etc.), if the material had not normally changed before and after a certain temperature condition for one month, ○ was indicated, and Δ was indicated by the change, as shown in Table 9.
TABLE 9
Figure BDA0001855539980000261
Figure BDA0001855539980000271
As shown in table 9, by adjusting the combination of magnesium aluminum silicate and xanthan gum in different proportions, when the amount of magnesium aluminum silicate is less than 2 parts by mass, none of the formulations can well carry 15 parts by mass of calamine. When the aluminum magnesium silicate is used in 2 parts by mass and is matched with xanthan gum, the formula can be stabilized at the normal temperature of 25 ℃, but the stability problem still exists at the low temperature of minus 10 ℃ and the high temperature of 40 ℃. When the amount of the aluminum magnesium silicate is increased to 2.5 parts by mass and the xanthan gum is used to 1 part by mass, the stability problem exists at the high temperature of 40 ℃. When the amount of the aluminum magnesium silicate is 2.5 parts by mass and the xanthan gum is 1.5 parts by mass, the problem of high-temperature stability can be solved, and the stability at minus 10 ℃ and normal temperature of 25 ℃ can be ensured.
Test example 6: evaluation of spreadability and washability against the compositions of comparative examples 1-12
The smearing evaluation method was as follows: taking a test area with the area of 4cm x 4cm at the inner side of the front arm, smearing 1 g of sample, and smearing clockwise for 10 circles, wherein the sample is not easy to smear and the background color of the exposed skin in the test area is 0 min; the skin is easy to apply, but the bottom color of the exposed skin in the test area is 1 minute; the skin is not easily smeared but the bottom color of the skin is not exposed in the test area for 1 minute; the sample can be easily spread and the test area does not reveal a base color of 2 points (best for 2 points). The results are shown in the following table.
The washout evaluation method was as follows: a4 cm by 4cm area of the inner side of the forearm was applied with 1 g of the sample, and after 5 minutes of application, the area was rinsed with flowing water at the same flow rate for 60 seconds, with 0 minutes for no wash, 1 minute for partial wash, and 2 minutes for complete wash (2 minutes is the best). The results are shown in the following table.
Watch 10
Feeling of smearing Property of washing off
Comparative example 1 2 1
Comparative example 2 2 1
Comparative example 3 2 1
Comparative example 4 2 2
Comparative example 5 2 1
Comparative example 6 2 1
Comparative example 7 2 2
Comparative example 8 2 2
Comparative example 9 2 2
Comparative example 10 2 2
Comparative example 11 2 2
Comparative example 12 2 2
Example 66 2 2
By adjusting the combination of the aluminum magnesium silicate and the xanthan gum in different proportions, when the aluminum magnesium silicate is up to 1 part by mass and the xanthan gum is up to 0.5 part by mass, the coating and washing performances are good. The using amount of the aluminum magnesium silicate reaches more than 1.5 parts by mass, and the highest using amount of the xanthan gum reaches 1.5 parts by mass, so that the xanthan gum has good smearing feeling and good washing performance. In other combinations, the coating feel was good, but the washability was slightly weaker.
Examples 78 to 85: preparation of different content calamine composition
An aqueous composition containing calamine was prepared with the components shown in table 11. The method comprises the following specific steps: weighing deionized water, starting a fixed stirrer at a rotating speed of 1000-2000 r/min, adding aluminum magnesium silicate, and stirring for 30-40 min until the aluminum magnesium silicate is completely dissolved and no particles exist; uniformly dispersing xanthan gum and glycerin, adding the mixture into the material body, keeping a stirrer on, stirring for 15-20 minutes at the rotation speed of 1000-2000 r/min until the mixture is uniformly dispersed and has no particles; adding phenoxyethanol, and stirring for 5 minutes at the rotating speed of the stirrer of 1000-2000 r/min; keeping the stirrer in an open state, slowly adding the calamine at the rotating speed of 1000 r/min-2000 r/min, and stirring for 5-10 min after the calamine is completely added until the calamine is completely dispersed in the material body. And finally, complementing the rest deionized water to 100%, and stirring for 1-2 minutes until the material body is uniform.
TABLE 11
Examples Calamine (Calamina) Glycerol Phenoxyethanol Deionized water Magnesium aluminum silicate Chinese gum
78 0.01 12 0.5 To 100 2.5 1.5
79 1 12 0.5 To 100 2.5 1.5
80 5 12 0.5 To 100 2.5 1.5
81 10 12 0.5 To 100 2.5 1.5
82 15 12 0.5 To 100 2.5 1.5
83 20 12 0.5 To 100 2.5 1.5
84 30 12 0.5 To 100 2.5 1.5
85 35 12 0.5 To 100 2.5 1.5
Test example 7: stability Studies on the compositions of examples 78-85
The stability evaluation method is that the sample is placed in three stable constant temperature boxes of-10 ℃, normal temperature (25 ℃) and 40 ℃, and the observation is carried out for one month to see whether the material body has the phenomenon of morphological change (whether the material body is layered or not, whether the material body is out of water or not, uneven and the like), if the material body is not changed normally before and after a certain temperature condition for one month, ○ is shown, and the change shows delta, and the results are shown in the following table.
TABLE 12
Figure BDA0001855539980000291
Figure BDA0001855539980000301
The amount of magnesium aluminum silicate and xanthan gum used in the formulation was 2.5 parts by mass and 1.5 parts by mass, and it was tried to add calamine in an amount of 0.01 to 35 parts by mass to the formulation, and the formulation had an ideal stabilizing effect at each temperature.
Test example 8: smear and washout evaluations for the compositions of examples 78-85
The smearing evaluation method was as follows: taking a test area with the area of 4cm x 4cm at the inner side of the front arm, smearing 1 g of sample, and smearing clockwise for 10 circles, wherein the sample is not easy to smear and the background color of the exposed skin in the test area is 0 min; the skin is easy to apply, but the bottom color of the exposed skin in the test area is 1 minute; the skin is not easily smeared but the bottom color of the skin is not exposed in the test area for 1 minute; the sample can be easily spread and the test area does not reveal a base color of 2 points (best for 2 points). The results are shown in the following table.
The washout evaluation method was as follows: a4 cm by 4cm area of the inner side of the forearm was applied with 1 g of the sample, and after 5 minutes of application, the area was rinsed with flowing water at the same flow rate for 60 seconds, with 0 minutes for no wash, 1 minute for partial wash, and 2 minutes for complete wash (2 minutes is the best). The results are shown in the following table.
Watch 13
Figure BDA0001855539980000302
Figure BDA0001855539980000311
The dosage of the magnesium aluminum silicate and the xanthan gum in the formula is 2.5 parts by mass and 1.5 parts by mass, and the attempt to add 0.01 part by mass to 35 parts by mass of calamine in the formula ensures that each formula has good spreadability and washability.
Example 86: preparation of facial mask
Figure BDA0001855539980000312

Claims (10)

1. A calamine-containing composition comprising a combination of an inorganic salt-based thickening agent in an amount of 2% by weight or more and a polysaccharide-based thickening agent in an amount of 1% by weight or more, based on the weight of the composition.
2. The composition according to claim 1, wherein the inorganic salt-based thickener is present in an amount of 2.5% by weight or more and the polysaccharide-based thickener is present in an amount of 1.5% by weight or more.
3. The composition according to claim 1, wherein the weight ratio of the inorganic salt-based thickener to the polysaccharide-based thickener is 5: 3.
4. The composition according to claim 1, wherein said inorganic salt-based thickener is magnesium aluminum silicate and said polysaccharide-based thickener is xanthan gum.
5. The composition of claim 1, further comprising an additional thickener selected from the group consisting of: polyacrylic acids, acryloyl dimethyltaurate copolymers, cellulosics, carbomers.
6. The composition of claim 1, wherein the composition further comprises glycerin.
7. The composition of claim 1, wherein the composition further comprises phenoxyethanol.
8. The composition of claim 1, wherein the weight percentage of calamine in the composition is equal to or greater than 15% by weight of the composition.
9. A mask product comprising the composition of claim 1.
10. Use of the composition of claim 1 in a personal care product.
CN201811313109.5A 2018-11-06 2018-11-06 Calamine-containing composition Active CN111135115B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201811313109.5A CN111135115B (en) 2018-11-06 2018-11-06 Calamine-containing composition

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201811313109.5A CN111135115B (en) 2018-11-06 2018-11-06 Calamine-containing composition

Publications (2)

Publication Number Publication Date
CN111135115A true CN111135115A (en) 2020-05-12
CN111135115B CN111135115B (en) 2023-10-17

Family

ID=70516494

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201811313109.5A Active CN111135115B (en) 2018-11-06 2018-11-06 Calamine-containing composition

Country Status (1)

Country Link
CN (1) CN111135115B (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112569132A (en) * 2020-11-30 2021-03-30 彭氏(惠州)实业发展有限公司 Bath cream and preparation method thereof
CN115778885A (en) * 2022-12-05 2023-03-14 波顿香料股份有限公司 Preparation method of dendrobium officinale extract with antioxidant and moisturizing effects and skin cream

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1337226A (en) * 2001-09-24 2002-02-27 中国人民解放军军事医学科学院放射医学研究所林仲武 Calamine lotion
US20020120241A1 (en) * 2000-12-22 2002-08-29 Tyrrell David John Absorbent articles with hydrophilic compositions containing anionic polymers
CN1635996A (en) * 2000-06-02 2005-07-06 彭特法姆股份公司 Topical agent for dermatological use containing 4-hydroxyphenyl-alpha-D-glucopyranoside
CN101485623A (en) * 2009-01-08 2009-07-22 王秀玲 Anti-acne cosmetic composition and facial mask containing the composition
CN105560165A (en) * 2015-11-26 2016-05-11 陕西玉航电子有限公司 Calamina gel and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1635996A (en) * 2000-06-02 2005-07-06 彭特法姆股份公司 Topical agent for dermatological use containing 4-hydroxyphenyl-alpha-D-glucopyranoside
US20020120241A1 (en) * 2000-12-22 2002-08-29 Tyrrell David John Absorbent articles with hydrophilic compositions containing anionic polymers
CN1337226A (en) * 2001-09-24 2002-02-27 中国人民解放军军事医学科学院放射医学研究所林仲武 Calamine lotion
CN101485623A (en) * 2009-01-08 2009-07-22 王秀玲 Anti-acne cosmetic composition and facial mask containing the composition
CN105560165A (en) * 2015-11-26 2016-05-11 陕西玉航电子有限公司 Calamina gel and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112569132A (en) * 2020-11-30 2021-03-30 彭氏(惠州)实业发展有限公司 Bath cream and preparation method thereof
CN115778885A (en) * 2022-12-05 2023-03-14 波顿香料股份有限公司 Preparation method of dendrobium officinale extract with antioxidant and moisturizing effects and skin cream

Also Published As

Publication number Publication date
CN111135115B (en) 2023-10-17

Similar Documents

Publication Publication Date Title
KR101667937B1 (en) Cosmetics composition of peel-off type pack and method preparing the same
CN108498345A (en) A kind of gel adhesive and preparation method thereof
CN112515992B (en) Stable composition comprising triethyl citrate and glycine
KR101768710B1 (en) Manufacturing method of eyelash extension patch having wrinkle-improving function
CN105407870A (en) Organogel composition and organogel mask pack produced by using same
CN111135115B (en) Calamine-containing composition
CN104013574B (en) Suspension preparation of temperature change painless nano sulfadiazine metallic compound hyaluronic acid
CN105169408A (en) Sodium alginate antibiosis spray and preparation method thereof
CN108498450B (en) High-permeability moisture mask and preparation method thereof
JP2022501314A (en) Topical composition
CN103211753A (en) Gel matrix
CN109199984B (en) Whitening and skin-care composition capable of changing powder into cream and preparation method thereof
US20080085291A1 (en) Solid cosmetic and therapeutic compositions applicable to the human skin and gellable on contact with water
JPH032124A (en) Liquid agent for external application
CN113940897B (en) Preparation method of anti-aging composition, anti-aging composition and use method thereof
CN112957315B (en) Personal care gel, preparation method and application
CN112773816B (en) Wound repair spray and preparation method and application thereof
CN104800137B (en) The applications of golden flower Flos Camelliae Japonicae extracts, preserving moisture and protecting skin composition and preparation method thereof
KR101431456B1 (en) Oil-in-water type organogel composition
CN112138085B (en) Traditional Chinese medicine composition with function of regulating asthenopia and preparation method thereof
US8808759B1 (en) Stabilized colloidal preparations, pre-mix and process for preparing skin care compositions, improved skin care composition, method for treating the skin
CN110742820A (en) Dihydroartemisine D-salt cosmetic agents and uses thereof
CN111588663B (en) Fixing gel composition and preparation method thereof
CN104138352B (en) Calcipotriol non-aqueous gel
CN116327620B (en) Calendula skin care oil for infants and preparation method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant