CN113712864A - Soap-based facial cleanser - Google Patents

Soap-based facial cleanser Download PDF

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Publication number
CN113712864A
CN113712864A CN202111033803.3A CN202111033803A CN113712864A CN 113712864 A CN113712864 A CN 113712864A CN 202111033803 A CN202111033803 A CN 202111033803A CN 113712864 A CN113712864 A CN 113712864A
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phase
facial cleanser
peach gum
cyclodextrin
polysaccharide
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孟宏
刘有停
曲召辉
刘宇红
刘月恒
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Taihe Kangmei Beijing Research Institute of Traditional Chinese Medicine Co Ltd
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Taihe Kangmei Beijing Research Institute of Traditional Chinese Medicine Co Ltd
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    • 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
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9783Angiosperms [Magnoliophyta]
    • A61K8/9789Magnoliopsida [dicotyledons]
    • 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
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/60Sugars; Derivatives 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
    • 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
    • A61K8/731Cellulose; Quaternized cellulose derivatives
    • 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
    • A61K8/732Starch; Amylose; Amylopectin; Derivatives 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
    • A61K8/738Cyclodextrins
    • 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
    • A61K8/81Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
    • A61K8/817Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen; Compositions or derivatives of such polymers, e.g. vinylimidazol, vinylcaprolactame, allylamines (Polyquaternium 6)
    • A61K8/8176Homopolymers of N-vinyl-pyrrolidones. Compositions of derivatives of such polymers
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P29/00Non-central analgesic, antipyretic or antiinflammatory agents, e.g. antirheumatic agents; Non-steroidal antiinflammatory drugs [NSAID]
    • 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
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/10Washing or bathing preparations
    • 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
    • A61K2800/80Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/84Products or compounds obtained by lyophilisation, freeze-drying

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Abstract

The invention relates to a soap-based facial cleanser, and belongs to the field of daily chemicals. The soap-based facial cleanser of the invention is added with an anti-irritation composition, which comprises peach gum extract and optionally radix clematidis extract. The cleansing cream has strong stability, and the addition of the composition can reduce the irritation of the cleansing cream to the skin, achieve the effect of inhibiting inflammatory reaction, relieve the tight feeling after washing, and have good cleaning power and foamability.

Description

Soap-based facial cleanser
Technical Field
The invention relates to a soap-based facial cleanser with strong stability and low irritation, belonging to the field of daily chemicals.
Background
The facial cleanser is a cleansing product for facial skin, and can remove dirt on the skin, make the skin fresh and cool, and help to maintain the normal physiological state of the skin. Of all skin care products, the most marketable is facial cleanser, and soap-based facial cleansers are one of the mainstream products. The soap-based facial cleanser is a fatty acid soap type facial cleanser obtained by saponification reaction of fatty acid and alkali, and has the characteristics of rich and fine foam, strong cleaning force, easiness in washing, capability of endowing skin with clean and refreshing feeling after use and the like. However, the soap base system is unstable at high temperature, the paste is easy to be discharged after being used for a long time, the pH value is high, the degreasing force is strong, and the washed skin is easy to dry and stretch and has strong irritation.
Aiming at the problems, the existing soap-based facial cleanser on the market mostly adopts the effect raw materials which are compounded with milder surfactant or added with fat-endowing agent, humectant and antagonistic stimulus to achieve the effects of reducing the stimulus and relieving the tight feeling, but even if the soap-based content is reduced or the milder surfactant or added with fat-endowing agent, humectant and the effective raw materials with antagonistic stimulus are compounded, the adverse symptoms of the soap-based facial cleanser on the skin can not be completely avoided. On the other hand, the stability of the soap-based facial cleanser cream body is improved by adjusting the process such as improving the cream forming point or adding a thickening agent, a suspending agent and the like in the existing method, but the problems of complex process operation, insignificant effect and the like exist. Therefore, the development of a soap-based facial cleanser with stable paste and low irritation has been the focus of attention of technicians.
Disclosure of Invention
Based on the defects of the prior art, the invention provides the soap-based facial cleanser with stable cream body and low irritation, the soap-based facial cleanser is strong in high-temperature stability, the irritation of the soap-based facial cleanser to the skin can be effectively reduced when the soap-based facial cleanser is used, the tight feeling after washing is improved, and the problem of water outflow of the cream body after long-time use is solved.
To achieve the object of the present invention, in a first aspect, the present invention provides a soap-based facial cleanser comprising phases a, B, C, D and E;
wherein, the phase A comprises fatty acid, emulsifier and ethylene glycol distearate;
wherein, the phase B comprises polyalcohol, chelating agent, pH regulator, water and surfactant;
wherein, the phase C comprises a thickening agent;
wherein phase D comprises an anti-irritant composition comprising peach gum extract and optionally, the extract of the plant's palm, a cationic conditioning agent;
according to the present invention, the above "optionally" means that the anti-irritant composition of the present invention comprises peach gum extract, with or without cactus extract.
Wherein phase E comprises a preservative.
According to some embodiments of the invention, phase E further comprises a perfume.
According to some embodiments of the invention, the peach gum extract comprises more than 30% by mass of peach gum polysaccharides.
According to a preferred embodiment of the present invention, the peach gum extract contains more than 50% by mass of peach gum polysaccharide.
According to a preferred embodiment of the present invention, the peach gum extract contains more than 70% by mass of peach gum polysaccharide.
According to some embodiments of the invention, the polysaccharide average molecular weight of the peach gum polysaccharide in the anti-irritation composition is 100-500 wDa.
According to some embodiments of the invention, the polysaccharide average molecular weight of the peach gum polysaccharide in the anti-irritation composition is 200-300 wDa.
According to some preferred embodiments of the present invention, the polysaccharide average molecular weight of the anti-irritation composition peach gum polysaccharide is 240-280 wDa.
According to some embodiments of the invention, when the anti-irritant composition comprises an extract of peach gum and an extract of cactus, the polysaccharides of peach gum and cactus have an average molecular weight of 100-500 wDa.
According to some embodiments of the invention, when the anti-irritant composition comprises an extract of peach gum and an extract of cactus, the polysaccharides of peach gum and cactus have an average molecular weight of 200-300 wDa.
According to some preferred embodiments of the present invention, when the anti-irritant composition comprises an extract of peach gum and an extract of cactus, the polysaccharides of peach gum and cactus have an average molecular weight of 240-280 wDa.
According to some embodiments of the invention, the anti-irritant composition further comprises as component 3) one or more of dextrin, cyclodextrin, methyl cyclodextrin, hydroxypropyl cyclodextrin, trehalose, polyvinylpyrrolidone, methyl cellulose, methylhydroxyethyl cellulose, hydroxypropylmethyl cellulose, hydroxyethyl cellulose and hydroxypropyl cellulose.
According to some embodiments of the invention, the phase D anti-irritant composition is prepared by a process comprising the steps of:
(1) extracting peach gum and optional radix Clematidis with water to obtain primary extractive solution;
(2) and centrifuging the primary extract to obtain a supernatant.
According to some embodiments of the invention, the weight ratio of peach gum to cactus in the anti-irritant composition is 1:5 to 15: 1.
According to some preferred embodiments of the invention, the weight ratio of peach gum to cactus in the anti-irritant composition is between 1:10 and 10: 1.
According to some embodiments of the present invention, the extraction temperature in step (1) is 50-90 ℃, for example, 50 ℃, 51 ℃, 52 ℃, 53 ℃, 54 ℃, 55 ℃, 56 ℃, 57 ℃, 58 ℃, 59 ℃, 60 ℃, 61 ℃, 62 ℃, 65 ℃, 68 ℃, 69 ℃, 70 ℃, 75 ℃, 78 ℃, 80 ℃, 82 ℃, 84 ℃, 88 ℃, 90 ℃, and the values between these values.
According to a preferred embodiment of the present invention, in the step (1), the extraction temperature is 60 to 75 ℃, and may be, for example, 60 ℃, 61 ℃, 62 ℃, 65 ℃, 68 ℃, 69 ℃, 70 ℃, 75 ℃.
According to some embodiments of the present invention, the extraction time in step (1) is 0.5-5h, and may be, for example, 30min, 40min, 50min, 1h, 1.5 h, 2h, 2.5 h, 3h, 3.5h, 4h, 5h, and points between these values.
According to some embodiments of the invention, the weight ratio of the total weight of peach gum and cactus to water in step (1) is 1: 10-1: 50, for example, may be 1:10 (m/m), 1: 11 (m/m), 1: 12 (m/m), 1: 13 (m/m), 1: 14 (m/m), 1: 15 (m/m), 1: 16 (m/m), 1: 17 (m/m), 1: 18 (m/m), 1:20 (m/m), 1:25 (m/m), 1:27 (m/m), 1:30 (m/m), 1:32 (m/m), 1:35 (m/m), 1: 36 (m/m), 1: 39 (m/m), 1:40 (m/m), 1: 41 (m/m), 1: 42 (m/m), 1: 45 (m/m), 1: 48 (m/m), 1: 50 (m/m).
According to a preferred embodiment of the present invention, in step (1), the weight ratio of the total weight of the peach gum and cactus to the water is 1:20 to 1:40, and may be 1:20 (m/m), 1:25 (m/m), 1:27 (m/m), 1:30 (m/m), 1:32 (m/m), 1:35 (m/m), 1: 36 (m/m), 1: 39 (m/m), 1:40 (m/m).
According to some embodiments of the present invention, the centrifugation in the step (2) is 4000-8000rpm for 5-30 min.
According to some embodiments of the invention, the method of preparing the anti-irritant composition further comprises step (3): and (3) carrying out microfiltration on the supernatant obtained in the step (2) by adopting a microfiltration membrane component to obtain a micro-filtrate.
According to some embodiments of the invention, the microfiltration membrane module of step (3) is selected from a ceramic microfiltration membrane module or a roll-type microfiltration membrane module.
According to some embodiments of the invention, the pore size of the microfiltration membrane module is between 50 and 200 nm.
According to some embodiments of the invention, the pore size of the microfiltration membrane module is 100 nm.
According to some embodiments of the invention, the method of preparing the anti-irritant composition further comprises step (4): and (4) compounding the micro-filtrate obtained in the step (3) with one or more of dextrin, cyclodextrin, methyl cyclodextrin, hydroxypropyl cyclodextrin, trehalose, polyvinylpyrrolidone, methyl cellulose, methyl hydroxyethyl cellulose, hydroxypropyl methyl cellulose, hydroxyethyl cellulose or hydroxypropyl cellulose to obtain a compound.
According to some embodiments of the invention, the weight ratio of the micro filtrate to one or more of dextrin, cyclodextrin, methyl cyclodextrin, hydroxypropyl cyclodextrin, trehalose, polyvinylpyrrolidone, methyl cellulose, methyl hydroxyethyl cellulose, hydroxypropyl methyl cellulose, hydroxyethyl cellulose or hydroxypropyl cellulose is 1: 1-1: 20.
according to some embodiments of the present invention, the compound obtained in step (4) may be dried and sterilized before use.
According to some embodiments of the invention, the drying is freeze-drying at-80 ℃ to-50 ℃ for 8 to 32 h.
According to some embodiments of the invention, the drying is spray drying, the inlet air temperature is 100 ℃ and 170 ℃, and the material flow rate is controlled to be 5-50 mL/min.
According to some embodiments of the invention, the drying is oven drying at 90-150 ℃ for 12-50h, pulverizing and sieving with a 80 mesh sieve, and taking the undersize fraction.
According to some embodiments of the invention, the sterilization process is cobalt 60 sterilization for 1-8 h.
According to some embodiments of the present invention, the sterilization is performed by using 100-700W microwave for 0.5-30 min.
According to some embodiments of the invention, the sterilization is dry heat sterilization at 90-150 ℃ for 0.5-5 h.
According to some embodiments of the invention, the components and the amounts of the facial cleanser are as follows:
Figure 331902DEST_PATH_IMAGE002
according to some embodiments of the invention, the phase a fatty acid is one or more of lauric acid, myristic acid, palmitic acid, stearic acid.
According to some embodiments of the invention, the phase a emulsifier is one or more of glyceryl stearate, glyceryl stearate SE, or PEG-100 stearate.
According to some embodiments of the invention, the phase B polyol is one or more of glycerol, butylene glycol, propylene glycol or dipropylene glycol.
According to some embodiments of the invention, the phase B chelator is disodium EDTA, trisodium EDTA, or tetrasodium EDTA.
According to some embodiments of the invention, the phase B pH adjusting agent is a pH adjusting agent, as is conventional in the art, to adjust the pH to 6.0-11.0.
According to some preferred embodiments of the invention, the pH adjusting agent is sodium hydroxide, potassium hydroxide or triethanolamine.
According to some embodiments of the invention, the phase B anionic surfactant is one or more of sodium laureth sulfate, ammonium laureth sulfate, TEA laureth sulfate.
According to some embodiments of the invention, the phase B amphoteric surfactant is cocamidopropyl betaine.
According to some embodiments of the invention, the phase C thickener is carbomer, an acrylic copolymer, xanthan gum or cellulose.
According to some embodiments of the invention, the phase D cationic conditioning agent is polyquaternium-7, polyquaternium-10, or the like, or a cationic polymer.
According to some embodiments of the invention, the phase D may further comprise sodium chloride for thickening sodium laureth sulfate (AES).
According to some embodiments of the invention, the sodium chloride is added in an amount of 0.00-2.00wt% based on the amount of sodium laureth sulfate (AES) added.
According to some embodiments of the invention, the phase E preservative is a preservative conventional in the art, and may be, for example, phenoxyethanol/ethylhexylglycerin or methylisothiazolinone/methylchloroisothiazolinone.
According to some embodiments of the invention, the phase E fragrance is a fragrance conventional in the art.
According to some embodiments of the invention, the facial cleanser is prepared by a method comprising the following steps:
(1) heating phase A to 80-85 deg.C, stirring;
(2) heating phase B to 80-85 deg.C;
(3) slowly adding the phase B into the phase A, and stirring for more than 1h under heat preservation;
(4) cooling to 50-60 deg.C, adding the prepared phase C, and stirring;
(5) cooling to 45 deg.C, adding D, E phases respectively, and stirring;
(6) cooling to room temperature and discharging.
The invention has the advantages of
The anti-irritation composition is added into the soap-based facial cleanser, so that the obtained facial cleanser cream has strong stability, the cleansing power, the foamability and the skin feel of the facial cleanser are kept, the irritation of the facial cleanser to the skin can be effectively reduced, the effect of inhibiting inflammatory reaction is achieved, and the tight feeling after washing can be relieved.
Drawings
FIG. 1 shows initial sample states of a comparative example 1 sample (left), a commercial auction sample (middle), and an example 1 sample (right);
FIG. 2 shows the state pictures of the samples of comparative example 1 (left), commercial auction (middle) and example 1 (right) after a constant temperature of 45 ℃ for 1 month;
FIG. 3 shows the water-out problem of the paste of comparative example 1 after 1 month of use;
fig. 4 shows a comparison of the state of the pastes of comparative example 1 (left) and example 1 (right) after 1 month of use.
The specific implementation mode is as follows:
the invention will be further described with reference to specific embodiments, and the advantages and features of the invention will become apparent as the description proceeds. The examples are illustrative only and do not limit the scope of the present invention in any way. It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention, and that such changes and modifications may be made without departing from the spirit and scope of the invention.
The sources of the raw materials used in the present invention are shown in Table 1, and the names and manufacturers of the instruments used in the present invention are shown in Table 2. The raw materials and instruments used in the invention are all conventional raw materials or instruments unless otherwise specified.
TABLE 1 raw materials and sources
Name of raw materials Standard Chinese name Purchasing manufacturer
Water (W) Water (W) Self-made
AES Sodium laureth sulfate Shanghai Kao Chemical Co.,Ltd.
CAB Cocoamidopropyl betaine Shanghai Kao Chemical Co.,Ltd.
Polyquaternium-7 Polyquaternium-7 Shanghai Lisheng Chemicals Co., Ltd
Lauric acid Lauric acid EMERY
Myristic acid Myristic acid EMERY
Palmitic acid Palmitic acid EMERY
Stearic acid Stearic acid EMERY
Glycerol stearate Glycerol stearate BASF
Pearling agent Ethylene glycol distearate Shanghai Kao Chemical Co.,Ltd.
HE PEG-7 Glycerol cocoate BASF CHINA Co.,Ltd.
Potassium hydroxide Potassium hydroxide SINOPHARM CHEMICAL REAGENT Co.,Ltd.
EDTA disodium salt EDTA disodium salt Beijing Jie Huatai and science and technology Limited liability company
Sodium chloride Sodium chloride SINOPHARM CHEMICAL REAGENT Co.,Ltd.
Peach gum —— Sui county Hengyuan XiangCommercial Co Ltd
Radix et caulis Opuntiae Dillenii —— Nippon Shangyu constant exposure edible agricultural products Co Ltd
Hydroxypropyl cyclodextrins Hydroxypropyl cyclodextrins SHANDONG BINZHOU ZHIYUAN BIOTECHNOLOGY Co.,Ltd.
TABLE 2 Instrument names and manufacturers
Name (R) Model number Manufacturer of the product
Electronic balance ML204/02 Mettlerlatio instruments (Shanghai) Co Ltd
Digital display constant temperature water bath HH-2 Yanghua Jintan City, Jiangsu province, manufacturing Limited company of instruments
IKA RW16 stirrer RW 16 B S25 IKA (Ika) instruments and Equipment, Guangzhou, Inc
Precise timing electric stirrer JJ-1 Yanghua Jintan City, Jiangsu province, manufacturing Limited company of instruments
High-speed centrifugal machine eppendorf centrifuge 5430 eppendorf AG
Microfiltration membrane module equipment CeraMem-0025 XIAMEN FILTER AND MEMBRANE TECHNOLOGY Co.,Ltd.
Freeze dryer FD-1A-50 Shanghai Yuming Instrument Co., Ltd
Spray drier QIMO-8000T Qimo (Shanghai) electronic technology Co., Ltd
Multifunctional pulverizer BJ-800A DEQING BAIJIE ELECTRIC APPLIANCE Co.,Ltd.
Electric heating constant temperature blast air drying box DHG-9070A Shanghai Jinghong experiment equipment Co Ltd
Electric ceramic stove LC-E190S Country electric appliances Co Ltd
Example 1 facial cleanser preparation
The raw materials and the proportion are as follows:
Figure 289493DEST_PATH_IMAGE004
example 2 facial cleanser preparation
The raw materials and the proportion are as follows:
Figure 931565DEST_PATH_IMAGE006
example 3 facial cleanser preparation
The raw materials and the proportion are as follows:
Figure 454950DEST_PATH_IMAGE008
example 4 facial cleanser preparation
The raw materials and the proportion are as follows:
Figure 150374DEST_PATH_IMAGE010
example 5 facial cleanser preparation
The raw materials and the proportion are as follows:
Figure 798524DEST_PATH_IMAGE012
example 6 facial cleanser preparation
The raw materials and the proportion are as follows:
Figure 276910DEST_PATH_IMAGE014
example 7 facial cleanser preparation
The raw materials and the proportion are as follows:
Figure 451539DEST_PATH_IMAGE016
example 8 facial cleanser preparation
The raw materials and the proportion are as follows:
Figure 927651DEST_PATH_IMAGE018
the formulation tables for the comparative examples of the invention and examples 9 to 12 are as follows:
Figure 187731DEST_PATH_IMAGE020
the facial cleanser is prepared by the following processes:
(1) heating the phase A raw material to 80-85 ℃, uniformly stirring, and keeping the temperature for later use;
(2) heating the phase B raw material to 80-85 ℃;
(3) slowly adding the phase B into the phase A under stirring, and stirring for more than 1h under heat preservation;
(4) cooling to 50-60 deg.C, adding the prepared phase C, and stirring;
(5) cooling to 45 deg.C, adding D, E phases respectively, and stirring;
(6) stirring and cooling to room temperature, and discharging.
The anti-irritation composition is prepared by the following steps:
anti-irritant composition a: adding 50 parts of pure water into 1 part of peach gum and 1 part of cactus, extracting with pure water, and extracting for 2 hours at 80 ℃; centrifuging at 5000rpm/min for 20min, and collecting supernatant; performing microfiltration and concentration by using a 100nm microfiltration membrane component, removing substances with the molecular weight below 100wDa in the supernatant, and retaining the effluent liquid to obtain a microfiltration solution; according to the micro-filtrate: hydroxypropyl cyclodextrin = 1:5 (m/m) compounding; freeze-drying the compounded substance at-80 deg.C for 12 h; pulverizing, sieving with 80 mesh sieve, and collecting the sieved part; sterilizing with cobalt 60 for 3 hr to obtain anti-irritation composition A.
In the anti-irritation composition A, the average molecular weight of the peach gum polysaccharide is 100-500 wDa.
Anti-irritant composition B: adding 50 parts of pure water into 1 part of peach gum and 1 part of cactus, extracting with pure water, and extracting for 2 hours at 80 ℃; centrifuging at 5000rpm/min for 20min, and collecting supernatant; performing microfiltration and concentration by using a 100nm microfiltration membrane component, removing substances with the molecular weight below 100wDa in the supernatant, and retaining the effluent liquid to obtain a microfiltration solution; according to the micro-filtrate: hydroxypropyl cyclodextrin = 1:10 (m/m) compounding; freeze-drying the compounded substance at-80 deg.C for 12 h; pulverizing, sieving with 80 mesh sieve, and collecting the sieved part; sterilizing with cobalt 60 for 3 hr to obtain anti-irritation composition B.
In the anti-irritation composition B, the average molecular weight of the peach gum polysaccharide is 100-500 wDa.
Off-line state observation and skin feel stability test
Comparative example 1 Example 1 Example 9 Example 10 Example 11 Example 12
Status of state The state is acceptable The state is acceptable With precipitation The state is too hard Excessive thickening and precipitation The state is acceptable
Skin feel After washing, has tight feeling Rich foam and no tension after washing Soap base has granular feeling The system has over-high pH and strong irritation Much foam and too strong degreasing power Poor foamability
First, reduce the irritation experiment
And (3) testing a sample: example 1, comparative example 1, and some commercially available facial cleanser (water, stearic acid, polyethylene glycol-8, myristic acid, potassium hydroxide, glycerin, lauric acid, ethanol, butylene glycol, glyceryl stearate SE, polyquaternium-7, disodium EDTA, methylparaben, propylparaben, etc. as main ingredients).
(1) Red blood cell assay
The experimental method comprises the following steps:
the density of erythrocytes in the erythrocyte suspension is adjusted at room temperature, and the OD value of erythrocytes is 1.3000-1.7000 when the erythrocytes are fully hemolyzed at 530 nm. 0.05% is selected as the detection concentration, and the hemolysis rate of the corresponding red blood cells is between 60% and 90% when 0.05% of the solution of the product in the comparative example 1 is used.
Taking a centrifugal tube, sequentially adding a test object, PBS and RBC suspension according to the table 3, and uniformly mixing, wherein the final concentration of a sample system is the test concentration; placing in a shaking table, incubating for 10min, and centrifuging; observing the phenomenon, taking supernatant, and determining OD 530; the hemolysis rate was calculated.
TABLE 3 reaction system (μ L)
Addition of reagents Test sample PBS RBC suspensions
Sample set 20 280 100
Model control group 300 0 100
Solvent control group 0 300 100
The hemolysis rate is calculated as:
erythrocyte hemolysis rate (%) = (OD _ sample group-OD _ solvent control)/(OD _ model control-OD _ solvent control) × 100.
TABLE 4 influence of the samples on the haemolysis Rate of erythrocytes
Sample name Comparative example 1 Market contest Example 1 PBS
Hemolytic rate of erythrocyte% 75 49 19 0
As can be seen from Table 4, the hemolysis rate of erythrocytes was significantly reduced when the 0.05% solution of example 1 was used for the hemolysis test. Experiments prove that the soap-based facial cleanser can effectively reduce irritation.
(2) Chick embryo test
The experimental method comprises the following steps:
the eggs of the SPF-grade white Lai Hangzhou chicken are fertilized and are fresh, clean and intact, and the mass of the eggs is 50g-60 g. Setting the incubation temperature to be 37.5 +/-0.5 ℃, the relative humidity to be 55-70%, the turntable frequency to be 3-6 times/h, turning over the eggs and incubating for 3 days, and stopping turning over the eggs after windowing on the 4 th day. When the eggs are incubated for 4 days, the eggs should be checked, unfertilized chick embryos are discarded, and broken or thin-shelled chick embryos cannot be used.
After the chick embryos are incubated for 4 days, the small end of the egg is punched with an electric grinder, 2-3mL of egg white is extracted with a 10mL syringe, a small window of 1cm by 1cm is made in the middle of the egg slightly near the large end using the electric grinder to expose the chorioallantoic membrane (CAM) of the chick embryos, and the eggshell and eggshell membrane are carefully removed with forceps. The structure of the vascular system and the growth of the chick embryos should be observed at this time. Sealing the hole at the small end and the small window at the middle part with transparent adhesive tape, and placing the sealed small window into an incubator for continuous culture. The growth condition of the chick embryos needs to be checked every day, and dead embryos are discarded in time. 10 day old chick embryos were used for the experiment. The transparent adhesive tape for sealing the small window is torn off, the area of the small window is enlarged by using tweezers, the observation visual field is enlarged, and the operation is careful without damaging the integrity of the egg membrane. The structure of the vascular system should be observed again at this point and a decision made as to its integrity and suitability for testing. The teflon ring was placed on the CAM to prepare for sample addition.
Each test subject was used as a group, and 6 chick embryos were tested in each group, and 40. mu.l of the test subject was applied directly to the surface of the CAM in the Teflon ring. After 30min at 37 ℃, the change of chorioallantoic membrane toxicity effect indexes (such as bleeding, angiolysis, coagulation and the like) is observed, and the Endpoint Score (ES) is calculated in a combined manner. And comparing the endpoint scores of the test object treatment groups with the endpoint scores of the negative control, wherein the lower the endpoint score of the sample is, the stronger the anti-stimulation effect of the test object is prompted.
TABLE 5 Effect of samples on chick embryo chorioallantoic Membrane stimulation fraction
Sample name 3% comparative example 1 3% of the commercial competitive products 3% example 1 Physiological saline
Chick embryo stimulation fraction (ES) 23.0 19.0 14.0 0
As can be seen from Table 5, the use of the facial cleanser of example 1 significantly reduced the irritation to the allantoic membrane of chicken embryo chorioallantoic membrane. Experiments prove that the soap-based facial cleanser can effectively reduce irritation.
Second, paste stability test
(1) High temperature stability
60g of comparative example 1, example 1 and a commercially available competitive product are respectively put in a 80mL sample bottle, placed in a constant temperature box, kept at the constant temperature of 45 ℃ for 1 month, and then returned to the room temperature to observe whether the phenomena of layering, precipitation and the like exist, and the results are shown in a figure 1 and a figure 2. FIG. 1 is an initial picture of 3 samples, comparative example 1 (left), a commercial auction (center), and example 1 (right); FIG. 2 is a photograph showing the samples of comparative example 1 (left), commercial auction (middle) and example 1 (right) after keeping the temperature at 45 ℃ for 1 month.
As can be seen from FIGS. 1 and 2, after the constant temperature of 45 ℃ is kept for 1 month, obvious layering phenomenon appears in comparative example 1 and the market competitive products; example 1 had no delamination and good stability. Experiments prove that the soap-based facial cleanser disclosed by the invention has good high-temperature stability.
(2) Long time water discharge experiment of paste
20g of the samples of the comparative example 1 and the example 1 are respectively taken and placed in a 30mL white soft rubber tube, the samples are respectively used for 1 time in the morning and at the evening, the samples are continuously used for one month, and whether the water is generated in the paste after long-time use is observed, and the result is shown in a figure 3 and a figure 4. Fig. 3 shows the water-out problem of the paste of comparative example 1 after 1 month of use, and fig. 4 shows the comparison of the state of the paste of comparative example 1 (left) and example 1 (right) after 1 month of use.
As can be seen from fig. 3 and 4, the paste of comparative example 1 showed no water-out after 2 consecutive uses for 1 month, while the paste of example 1 showed no water-out problem. Experiments prove that the soap-based facial cleanser disclosed by the invention can solve the problem that the cream body of the facial cleanser can be drained after the facial cleanser is used for a long time.
Third, tight feeling relieving experiment
60 volunteers were selected and divided into 3 groups of 20 persons each and tested using comparative example 1, example 1 and a commercial auction, respectively. After the skin is moistened by a tester by using clear water, a proper amount of test product is taken from the palm of the hand, and after foams are slightly kneaded out, the test product is applied to the face and the skin of the face is slightly kneaded for 30 s; then rinsed clean with clear water and used for 2 weeks for each sample. The testers scored according to their own feelings. The scoring criteria were in 10 points, the scoring criteria are shown in table 6, and the average results are shown in table 7.
TABLE 6 evaluation criteria
Weak (weak) Is weaker Medium and high grade Is stronger High strength
Cleaning power 0.00-2.00 2.00-4.00 4.00-6.00 6.00-8.00 8.00-10.00
Tightness after washing 0.00-2.00 2.00-4.00 4.00-6.00 6.00-8.00 8.00-10.00
Degree of moistening after drying 0.00-2.00 2.00-4.00 4.00-6.00 6.00-8.00 8.00-10.00
Amount of foam 0.00-2.00 2.00-4.00 4.00-6.00 6.00-8.00 8.00-10.00
TABLE 7 evaluation of post-wash tightness of test products
Comparative example 1 Example 1 Market contest
Cleaning power 9.30 9.20 9.15
Tightness after washing 9.05 5.85 7.20
Degree of moistening after drying 5.30 7.35 6.25
Amount of foam 9.10 9.05 9.00
As can be seen from Table 7, the cleansing milk of example 1 was used to reduce the feeling of tightness after washing while maintaining a good cleansing power. Experiments prove that the soap-based facial cleanser disclosed by the invention can relieve the tight feeling after washing.
The experiments prove that the anti-irritation composition has a certain soap base thickening effect, and the stability of the paste is improved; the addition of the composition can reduce the irritation to skin, achieve the effect of inhibiting inflammatory reaction, relieve the tight feeling after washing, and maintain good cleaning power and foamability.

Claims (10)

1. A soap-based facial cleanser comprises phase A, phase B, phase C, phase D and phase E,
wherein, the phase A comprises fatty acid, emulsifier and ethylene glycol distearate;
wherein, the phase B comprises polyalcohol, chelating agent, pH regulator, water and surfactant;
wherein, the phase C comprises a thickening agent;
wherein phase D comprises an anti-irritant composition comprising peach gum extract and optionally cactus extract, a cationic conditioning agent;
wherein phase E comprises antiseptic and optional essence.
2. The facial cleanser according to claim 1, wherein the peach gum extract comprises more than 30% of peach gum polysaccharide, preferably more than 50% of peach gum polysaccharide, and more preferably more than 70% of peach gum polysaccharide.
3. The facial cleanser according to claim 1 or 2, wherein the anti-irritation composition comprises peach gum polysaccharide and cactus polysaccharide, wherein the average polysaccharide molecular weight of the peach gum polysaccharide and the cactus polysaccharide is 100-500wDa, preferably 200-300wDa, more preferably 240-280 wDa.
4. A facial cleanser according to any one of claims 1 to 3, wherein said anti-irritant composition further comprises component 3) one or more of dextrin, cyclodextrin, methylcyclodextrin, hydroxypropyl cyclodextrin, trehalose, polyvinylpyrrolidone, methylcellulose, methylhydroxyethylcellulose, hydroxypropylmethylcellulose, hydroxyethylcellulose and hydroxypropylcellulose.
5. The facial cleanser according to any one of claims 1 to 4, wherein the anti-irritant composition is prepared by a preparation method comprising the following steps:
(1) extracting peach gum and optional radix Clematidis with water to obtain primary extractive solution, preferably at 50-90 deg.C for 0.5-5 hr;
(2) and centrifuging the primary extract to obtain a supernatant.
6. The facial cleanser according to claim 5, wherein the weight ratio of peach gum to cactus in step (1) is 1:5-15:1, preferably 1:10-10: 1.
7. The facial cleanser according to claim 5 or 6, wherein the weight ratio of the total weight of the peach gum and the cactus to the water in the step (1) is 1: 10-1: 50.
8. the facial cleanser according to any one of claims 5 to 7, wherein the preparation method of the anti-irritant composition further comprises the step (3): and (3) carrying out microfiltration on the supernatant obtained in the step (2) by adopting a microfiltration membrane module to obtain a micro-filtrate, preferably, the microfiltration membrane module is selected from a ceramic microfiltration membrane module or a roll-type microfiltration membrane module, more preferably, the pore diameter of the microfiltration membrane module is 50-200nm, and more preferably 100 nm.
9. The facial cleanser according to claim 8, wherein the method for preparing said anti-irritant composition further comprises the step (4): and (3) compounding the micro-filtrate obtained in the step (3) with one or more of dextrin, cyclodextrin, methyl cyclodextrin, hydroxypropyl cyclodextrin, trehalose, polyvinylpyrrolidone, methyl cellulose, methyl hydroxyethyl cellulose, hydroxypropyl methyl cellulose, hydroxyethyl cellulose or hydroxypropyl cellulose to obtain a compound, preferably, the weight ratio of the micro-filtrate to one or more of dextrin, cyclodextrin, methyl cyclodextrin, hydroxypropyl cyclodextrin, trehalose, polyvinylpyrrolidone, methyl cellulose, methyl hydroxyethyl cellulose, hydroxypropyl methyl cellulose, hydroxyethyl cellulose or hydroxypropyl cellulose is 1: 1-1: 20.
10. the facial cleanser according to any one of claims 1 to 9, wherein the phase B surfactant comprises an anionic surfactant and an optional amphoteric surfactant, and preferably, the components of the facial cleanser are used in the following amounts: phase A: 10.00-35.00wt% of fatty acid, 0.50-5.00 wt% of emulsifier and 0.00-3.00 wt% of ethylene glycol distearate; phase B: 5.00-30.00 wt% of polyhydric alcohol, 0.10-1.00 wt% of chelating agent, 0.50-14.00 wt% of pH regulator, 0.00-10.00 wt% of water TO100, 0.00-10.00 wt% of anionic surfactant and 0.00-10.00 wt% of amphoteric surfactant; and C phase: 0.01 to 10.00 weight percent of thickening agent and 0.10 to 20.00 weight percent of water; phase D: 0.01-5.00 wt% of anti-irritation composition and 0.00-1.00 wt% of cationic conditioner; phase E: 0.05 to 1.00 weight percent of preservative and 0.00 to 1.00 weight percent of essence.
CN202111033803.3A 2021-09-03 2021-09-03 Soap-based facial cleanser Pending CN113712864A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112891266A (en) * 2019-12-25 2021-06-04 太和康美(北京)中医研究院有限公司 Peach gum extract and preparation method and application thereof
CN113018224A (en) * 2019-12-25 2021-06-25 太和康美(北京)中医研究院有限公司 Anti-irritation composition and application thereof
CN113018225A (en) * 2019-12-25 2021-06-25 太和康美(北京)中医研究院有限公司 Low-irritation facial cleanser
CN113041193A (en) * 2021-03-26 2021-06-29 北京东方淼森生物科技有限公司 Anti-irritation composition and preparation method and application thereof
IN201921034001A (en) * 2020-05-23 2021-08-27

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112891266A (en) * 2019-12-25 2021-06-04 太和康美(北京)中医研究院有限公司 Peach gum extract and preparation method and application thereof
CN113018224A (en) * 2019-12-25 2021-06-25 太和康美(北京)中医研究院有限公司 Anti-irritation composition and application thereof
CN113018225A (en) * 2019-12-25 2021-06-25 太和康美(北京)中医研究院有限公司 Low-irritation facial cleanser
IN201921034001A (en) * 2020-05-23 2021-08-27
CN113041193A (en) * 2021-03-26 2021-06-29 北京东方淼森生物科技有限公司 Anti-irritation composition and preparation method and application thereof

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