CN111265415B - Modified attapulgite, preparation method thereof and application thereof in external medicines and skin care products - Google Patents

Modified attapulgite, preparation method thereof and application thereof in external medicines and skin care products Download PDF

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CN111265415B
CN111265415B CN202010200130.5A CN202010200130A CN111265415B CN 111265415 B CN111265415 B CN 111265415B CN 202010200130 A CN202010200130 A CN 202010200130A CN 111265415 B CN111265415 B CN 111265415B
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polysaccharide
skin
attapulgite
external
skin care
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CN111265415A (en
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张哲�
王丹阳
薛圣鸽
王玉兰
刘扬
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Yikang Technology Shenzhen Co ltd
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Baiyin Division Innovation Research Institute Of Northwest Normal University
Gansu Shengyuan Traditional Chinese Medicine Co ltd
Northwest Normal University
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    • A61K47/51—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates the non-active ingredient being a modifying agent
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    • A61K47/55—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates the non-active ingredient being a modifying agent the modifying agent being an organic compound the modifying agent being also a pharmacologically or therapeutically active agent, i.e. the entire conjugate being a codrug, i.e. a dimer, oligomer or polymer of pharmacologically or therapeutically active compounds
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    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
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    • A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
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    • A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97—Cosmetics 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
    • A61K8/9783—Angiosperms [Magnoliophyta]
    • A61K8/9789—Magnoliopsida [dicotyledons]
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    • A—HUMAN NECESSITIES
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • A61Q19/08—Anti-ageing preparations

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Abstract

The invention relates to a modified attapulgite, a preparation method thereof and application thereof in external medicines and skin care products, belonging to the field of new materials.

Description

Modified attapulgite, preparation method thereof and application thereof in external medicines and skin care products
Technical Field
The invention relates to the field of new materials, in particular to a modified attapulgite, a preparation method thereof and application thereof in external medicines and skin care products.
Background
Attapulgite belongs to natural clay mineral, and has wide application. It is suitable for makeup blusher, face powder, eyebrow powder, lipstick, etc. because of its excellent smoothness, adhesion and air permeability. Due to good compatibility with organisms, the compound has wide research reports on the aspect of being used as a medical carrier, particularly being used as a targeting drug carrier and a drug sustained-release agent. However, the attapulgite material is rarely reported as an auxiliary material for promoting the drug effect of external drugs or the skin care effect of skin care products.
Natural products such as astragalus, angelica, aloe vera gel and the like can be used as cosmetic raw materials and have the functions of resisting aging, whitening, moisturizing, repairing and the like, and products in some forms such as facial mask mud, facial mask sheets, essence and the like which take astragalus as a main raw material are reported in the prior art. However, in the aspect of fully exerting the skin care effects of natural products such as astragalus and the like, a space capable of being excavated and improved is provided, and a natural skin care product which is good in effect, safe, good in use experience acceptance and more promising in popularization potential needs to be further developed.
Disclosure of Invention
The invention aims to provide a new material which is suitable for skin external preparations and can play a role in synergism, a modified attapulgite, a preparation method thereof and application thereof in external medicines and skin care products.
In order to achieve the purpose, the invention adopts the technical scheme that:
the invention provides a modified attapulgite, which is obtained by modifying attapulgite powder with polysaccharide.
The polysaccharide is selected from one or more of zymosan, aloe barbadensis leaf polysaccharide, Aphanothece purpurea polysaccharide, tamarind seed polysaccharide, tuberose polysaccharide, euglena minutissima polysaccharide and Cassia angustifolia seed polysaccharide; preferably zymosan;
the attapulgite powder is more than 2000 meshes, or 2000-3000 meshes, or more than 3000 meshes.
Optionally, the polysaccharide is obtained by mixing any three of zymosan, aloe barbadensis leaf polysaccharide, Aphanothece crispa polysaccharide, tamarind seed polysaccharide, tuberose polysaccharide, euglena gracilis polysaccharide and Cassia angustifolia seed polysaccharide according to a mass ratio of 1:1: 1.
In another aspect of the invention, a preparation method of any one of the modified attapulgite is provided: preparing attapulgite powder into an organic solvent suspension, adding polysaccharide, stirring uniformly, dripping concentrated acid, stirring, removing generated water until no water is generated, and press-filtering, washing and drying the product to obtain the attapulgite polysaccharide-polysaccharide complex;
preferably, the organic solvent is anhydrous diethyl ether or petroleum ether or ethyl acetate; the concentrated acid is concentrated sulfuric acid or concentrated nitric acid.
In the preparation method, the attapulgite powder is preferably prepared into an anhydrous ether suspension with the mass concentration of 5%, the polysaccharide is added, after uniform stirring, concentrated sulfuric acid accounting for ten-thousandth of the mass of the attapulgite is dropped, the mixture is stirred for reaction at the temperature of 45 ℃, and generated water is removed while stirring until no water is generated.
The feeding amount of the polysaccharide and the attapulgite powder is 1-10% by mass, preferably 3-8% by mass, and more preferably 5% by mass.
In another aspect of the invention, the modified attapulgite is used for preparing external medicines or skin care products.
Regarding the application, preferably in the external medicine or the skin care product, the modified attapulgite comprises the following components in percentage by mass: 0.1-5%; preferably 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1.0%, 1.1%, 1.2%, 1.5%, 2.0%, 3.0%, 4.0%, 5.0%, or a value between any two values;
the external medicine is antibacterial and anti-inflammatory ointment;
the skin care product refers to a daily skin care product, an anti-aging external product, a whitening external product, an acne-removing external product or a moisturizing external product.
In another aspect, the invention provides a skin external preparation, wherein the modified attapulgite comprises the following components in percentage by mass: 0.1-5%; preferably 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1.0%, 1.1%, 1.2%, 1.5%, 2.0%, 3.0%, 4.0%, 5.0%, or a value between any two values;
the skin external product is an external medicine or a skin care product;
the external medicine is antibacterial and anti-inflammatory ointment;
the skin care product refers to a daily skin care product, an anti-aging external product, a whitening external product, an acne-removing external product or a moisturizing external product.
A preferred skin external preparation comprises the following components in parts by weight: 0.1-5 parts of modified attapulgite, 25-40 parts of astragalus extract, 10-25 parts of angelica extract, 1-10 parts of aloe vera gel, 0.1-1 part of pearl powder and 10-20 parts of hyaluronic acid;
wherein, the grain diameter of the astragalus extract powder and the angelica extract powder is preferably more than 250 meshes;
preferably, the astragalus extract or the angelica extract is prepared by the following method: cleaning radix astragali or radix Angelicae sinensis, slicing, drying, pulverizing, adding water, stirring, extracting water soluble components by low temperature and high pressure difference continuous cell wall breaking extraction technology, concentrating the water solution, freeze drying, and pulverizing.
Preferably, the disinfectant also comprises 20-35 parts of sterile water.
Experimental data show that the novel material is used in external pharmaceutical products or skin care products, and can safely, effectively and remarkably improve the efficacy of the product. The modified attapulgite material is used in skin care products which take natural extracts as main functional components, has obvious effect on enhancing the skin care effect, improves the use experience of the products and is beneficial to product popularization.
The modified attapulgite adopts polysaccharide molecules (such as zymosan) with a special proportion to graft the surface of the attapulgite, is favorable for being fused with natural extracts (Chinese medicinal material extracts) rich in polysaccharide, and improves the loading capacity of the attapulgite on effective components, thereby improving the uniformity of the effective components in the product and the slow release effect on the skin. The product has good uniformity and slow release effect, so that the antibacterial and anti-inflammatory components in the components such as the astragalus, the angelica and the like can exert the effects on the skin mildly and durably.
In a preferred embodiment of the invention, the polysaccharide is preferably zymosan, which is a high molecular polysaccharide substance that adsorbs pathogenic bacteria, resists tumor and virus, relieves radiation damage, and stimulates and enhances immune function; experiments in the embodiment of the invention prove that, compared with attapulgite modified by other polysaccharides, attapulgite modified by zymosan has the best antibacterial effect, and attapulgite modified by zymosan has the strongest adsorption capacity.
In a preferred embodiment of the invention, the skin care product taking the astragalus extract as the main component is a composite essence of the astragalus extract and the modified attapulgite. The anti-aging, whitening, acne removing, moisturizing, antibacterial and other effects of the product are obviously superior to those of similar products. The radix astragali is dried root of Astragalus membranaceus bge or Astragalus membranaceus bge of Leguminosae, and has sweet and slightly warm taste and enters lung and spleen channels. Has the effects of invigorating qi, invigorating yang, consolidating superficial resistance, arresting sweating, inducing diuresis, relieving edema, removing toxic substance, expelling pus, healing sore and promoting granulation, and can be used for treating lung and spleen qi deficiency, middle-qi sinking, exterior deficiency spontaneous sweating, qi deficiency edema, sore and carbuncle difficult ulcer or chronic ulcer difficult ulcer. Modern researches find that the main chemical components of astragalus root are polysaccharide, saponin and flavone, wherein the polysaccharide component mainly comprises heteropolysaccharide and glucan. The astragalus contains amino acids, vitamins, polysaccharides and other nutrient substances, has the effects of benefiting qi and nourishing blood, strengthening body resistance and consolidating superficial resistance, and eliminating swelling and promoting granulation, and has the effects of delaying senility, preventing pigmentation and whitening.
Angelica sinensis (Oliv.) Diels is dried root of Angelica sinensis (Oliv.) Diels, Umbelliferae. The water extract of radix Angelicae sinensis is rich in ferulic acid, nicotinic acid, sucrose and various amino acids, and has antioxidant and free radical scavenging effects. Chinese angelica is a good product for beauty for women besides having the efficacies of promoting blood circulation and enriching blood. The angelica can effectively enhance the metabolism and endocrine function of a human body, prevent and treat diseases such as facial dryness, desquamation, pruritus and the like, enables the skin to become smoother and tender, and has a certain effect on delaying senility of women. In addition, the angelica sinensis extract can inhibit the activity of tyrosinase and reduce the formation of melanin, thereby achieving the whitening effect.
The astragalus extract and the angelica extract adopted by the invention are as follows: preferably, water soluble extract is adopted, and the water soluble substance does not contain alcohol soluble ester, so that the air permeability to skin is better. In the aspect of preparation process, a low-temperature high-pressure-difference continuous cell wall breaking extraction technology is adopted to extract water-soluble components, alcohol-soluble esters are removed, and only essential components beneficial to skin are reserved.
Aloe vera gel: has effects in activating cell, delaying skin aging, astringing, regulating skin, nourishing skin, and protecting skin; the scavenger for contained free radicals such as superoxide dismutase, peroxidase, vitamin C, vitamin E, carotene, etc. can scavenge free radicals which can cause skin cell aging, and delay skin cell aging; the amino acids, vitamins, minerals, ferment, organic acids and water in the product are essential nutrients for skin, and have natural astringent effect, and can be used for consolidating skin, preventing skin relaxation, effectively retaining water, and inhibiting melanin generation.
Pearl powder: has good whitening effect.
Hyaluronic acid: mainly increases the viscosity of the essence and provides moisturizing effect for the skin.
The invention has the beneficial effects that: the modified attapulgite surface of the product can obviously increase the loading capacity of the effective components, has good slow release property, and can fully exert the effects of the components. The modified attapulgite is applied to skin external products to prepare external medicines or skin care products, and a large amount of functional components in the products are loaded on the surface of the attapulgite and slowly released, so that the functions of the products are exerted to the maximum extent. The skin external product containing the modified attapulgite prepared by the invention has obvious effects of resisting aging, whitening skin, removing acne, moisturizing, resisting bacteria and the like.
Detailed Description
The invention is further illustrated by the following examples, which are not intended to be limiting.
The experimental procedures in the following examples are conventional unless otherwise specified.
Sources of materials
Attapulgite powder: purity higher than 99.9%, fineness 3000 mesh, Jiangsu Jinhan New Material Co., Ltd, product number BAT-010;
polysaccharide: zymosan, Hubei Qifei pharmaceutical chemical Co., Ltd, cat # 9010-72-4; aloe barbadensis leaf polysaccharide, Fengxing grass Biotech Co., Ltd, Cat No. PH-010-; polysaccharide of Temple Porphyra, Shanghai Haotai Biotech, Inc., trade name Sacran; tamarind seedy polysaccharide, gansu yumeitang materials manufacturing limited, cat # B4963402; tuberose polysaccharide, gansu yumeitang materials manufacturing ltd, cat No. B4963417; euglena gracilis polysaccharide, gansu yumeitang materials manufacturing ltd, cat No. B4963436; cassia angustifolia Vahl seed polysaccharide, Guangzhou Renshe New Material science and technology Co., Ltd., Cat 03.
Organic solvent: anhydrous ether, petroleum ether, ethyl acetate, analytically pure, commercially available.
Concentrated sulfuric acid: chemically pure, commercially available.
Concentrated nitric acid: chemically pure, commercially available.
Hyaluronic acid: west ampere wanfang biotechnology limited, cat #: 2019-5-TMZS.
Example 1 preparation of modified Attapulgite
The modified attapulgite is prepared by the following steps:
1. the attapulgite powder with the purity higher than 99.9 percent is selected and added with an organic solvent (anhydrous ether or petroleum ether or ethyl acetate) to prepare a suspension with the mass concentration of 5 percent.
2. Adding 1-10 wt% of polysaccharide (one or more selected from zymosan, aloe barbadensis leaf polysaccharide, Aphanothece purpurea polysaccharide, tamarind seed polysaccharide, tuberose polysaccharide, euglena gracilis polysaccharide and Cassia angustifolia seed polysaccharide, or mixing any three of them at a weight ratio of 1:1: 1) into attapulgite powder, and stirring.
3. Dropping concentrated acid (concentrated sulfuric acid or concentrated nitric acid) one-ten-thousandth of the mass of attapulgite, stirring at 45 ℃ for reaction, and removing generated water while stirring until no water is generated.
4. And (3) carrying out filter pressing on the product, washing the product for 3-5 times by using ultrapure water, and carrying out spray drying to obtain the modified attapulgite with the particle size of not less than 3000 meshes, wherein an exemplary product is shown in a table 1-1.
TABLE 1-1 modified Attapulgite exemplary products
Figure BDA0002419080400000051
The bacteriostatic activity and surface loading capacity of 7 modified attapulgite in table 1-1 were compared, and unmodified attapulgite was used as a control.
5. Bacteriostasis experiment and surface load capacity detection
Propionibacterium acnes: the strain source is as follows: beijing Zhongke quality testing Biotech Co., Ltd, strain No.: CL 7052.
Preparation of experimental bacterial suspension: the propionibacterium acnes is cultured in a test tube culture medium for 48 hours at 37 ℃ in a thermostat, then sterile ultrapure water is added, and the mixture is shaken to obtain an experimental bacteria suspension.
15mL of the melted SOB medium was taken and placed in a sterile plate, and then 1mL of the experimental strain was added dropwise and allowed to spread flat on the bottom of the plate. After the culture medium is solidified, 4 Oxford cups are vertically placed on each flat plate, then 0.1mL of experimental sample is respectively added, after the culture is carried out for 24 hours at 37 ℃, the size (unit: mm) of the diameter of the inhibition zone is respectively measured, each experimental group is repeated for 3 times, the average value of the experimental results is obtained, and the results are shown in tables 1-2.
Completely drying various polysaccharide modified attapulgite and a control, accurately weighing 1.0000g of a solution of a astragalus extract (prepared by the method in the embodiment 2 of the invention) with the same concentration, performing saturated adsorption, drying to constant weight, and calculating the weight gain ratio. The results are shown in tables 1-2.
TABLE 1-2 results of antibacterial and surface loading capabilities of Attapulgite
Experimental products Propionibacterium acnes Weight ratio of
Yeast polysaccharide modified attapulgite 8.2 35.20％
Aloe barbadensis leaf polysaccharide modified attapulgite 8.1 19.80％
Polysaccharide modified attapulgite of laver in mosque in water 4.2 28.90％
Acid bean seed polysaccharide modified attapulgite 7.4 23.90％
Polianthes tuberosa polysaccharide modified attapulgite 7.8 14.40％
Euglena gracilis polysaccharide modified attapulgite 3.6 30.90％
Cassia angustifolia VahlSeed polysaccharide modified attapulgite 5.9 21.50％
Unmodified attapulgite 3.2 10.20％
The experimental results show that the antibacterial activity and the surface loading capacity of the modified attapulgite are both greatly improved compared with that of unmodified attapulgite, and the zymosan modification effect is the best in the modified attapulgite.
The invention also carries out a parallel experiment that the mass ratio of the polysaccharide type to the attapulgite is between 1 and 10 percent, and obtains the same rule as the data presented in the table 1-2. Among the polysaccharides or combinations that may be used, zymosan performs best.
The polysaccharide proportion is too small, the load capacity of the modified attapulgite is not obviously changed, and the attapulgite is easy to settle in the essence; the ratio of polysaccharide is too high, the reaction of polysaccharide and hydroxyl on the surface of attapulgite is basically saturated, and the redundant polysaccharide is washed away in the washing step in the preparation process, thereby causing the waste of raw materials and the increase of cost.
Example 2 skin care product using modified attapulgite for extracting essence from traditional Chinese medicinal materials
Preparing materials:
1. modified attapulgite, product 1 in example 1.
2. Astragalus membranaceus water-soluble extract powder: cleaning radix astragali, slicing, drying, micronizing to 800 mesh, adding ultrapure water 20 times the mass of radix astragali, ultrasonically stirring at low temperature for 30min, extracting water-soluble essence component by low-temperature high-pressure-difference continuous cell wall breaking extraction technology, concentrating the water solution, freeze drying, and pulverizing to 250 mesh to obtain radix astragali water-soluble extract powder.
3. Powder of water-soluble extract of Angelica sinensis: cleaning radix Angelicae sinensis, slicing, drying, micronizing to 800 mesh, adding ultrapure water 20 times the mass of radix Angelicae sinensis, ultrasonically stirring at low temperature for 30min, extracting water-soluble essence component by low-temperature high-pressure-difference continuous cell wall breaking extraction technology, concentrating the water solution, freeze drying, and pulverizing to 250 mesh to obtain radix Angelicae sinensis water-soluble extract powder.
The low-temperature high-pressure-difference continuous cell wall breaking extraction technology of the astragalus and the angelica is operated according to the application of the six-flavor acne removing prescription extracted under the low-temperature high-pressure difference in facial mask liquid (Wu Yuan, etc., China cosmetic medicine, 10 months in 2013, volume 22, 19 th).
The step utilizes the most advanced low-temperature high-pressure-difference continuous cell disruption extraction process at present, takes ultrapure water as an extractant, skillfully separates and removes ester substances contained in Chinese herbal medicines, and more thoroughly extracts the beneficial essence part of astragalus and compounds thereof to the skin.
4. Preparing aloe gel: the aloe gel is purchased directly or made by self. The self-making method comprises the following steps: peeling fresh aloe, adding 5 times of ultrapure water, mashing, stirring, and filtering to remove residue to obtain pure natural aloe gel.
5. The pearl powder is crushed into over 3000 mesh powder.
The method comprises the following steps:
weighing the components according to the weight parts, uniformly mixing, standing for 20-26 hours, then performing ultrasonic dispersion, homogenizing at low temperature and high pressure, and performing ultraviolet light sterilization to obtain the astragalus extract essence product.
6 exemplary astragalus extract essence products were prepared according to the above method, the formulation of which is shown in table 2 below:
TABLE 2 parts by weight of the components in the different experimental groups
Figure BDA0002419080400000071
Experimental example 3 product Performance test
The product is as follows: the 6 exemplary products listed in example 2 and the comparative products listed in Table 3-1 below.
TABLE 3-1 comparative test products and parts by weight of the respective Components
Figure BDA0002419080400000072
The experimental design is illustrated as follows:
comparative groups 1 and 2, in order to verify the effect of the modified attapulgite: except for the variation factor of the attapulgite components, the proportion of each component of the comparative groups 1-2 is consistent with that of the invention group 1.
The comparison group 3 is to verify the effect of the process for extracting astragalus and angelica of the invention: the ratio of comparative group 3 and comparative group 1 was the same, but the sources of the extracts of Astragalus membranaceus and Angelica sinensis were different.
Comparative groups 4 and 5 are intended to compare the product of the invention with existing products.
Anti-aging experiment
Testing an instrument: the skin elastometer manufactured by CK company, germany, model MPA580, the probe used was a revisometer RV600 elasto-fibrous tissue test probe.
Volunteers: a total of 330 normal women aged 30-60 years were divided into 11 groups of 30 persons each for the invention and control groups. Every person uses 1g of the product in the morning and evening every day, and the using time is 6 months.
The tester area: the forehead area 2cm above the middle of the eyebrow, the chin area 2cm below the middle of the lower lip, and the left and right cheek areas at the intersection of the nose tip and the pupil.
The test method comprises the following steps:
constant negative pressure mode (-), negative pressure set to 450 mbar.
Uf-maximum amount of skin stretching;
Ue-the amount of stretching of the skin at 0.1 seconds after a constant negative pressure has been applied to the skin, to locate the amount of stretching of the elastic portion;
Uv—Uf-Uethe amount of stretching of the viscoelastic part of the skin, or the plastic part.
As for skin, the younger the skin, the skin with good elasticity, UeThe higher the value of (A), and for aged skinSkin with poor elasticity, elastic part value UeRelatively low, and a viscoelastic part value UvThe value is relatively high.
The testing steps are as follows:
measuring blank value 30min after cleaning test area, and calculating skin elasticity increase rate (also U) according to the measured valuevReduced rate of skin elasticity) to determine the anti-aging effect, the higher the rate of increase of skin elasticity, i.e., UvThe more the reduction rate, the better the anti-aging effect.
The calculation method comprises the following steps: the viscoelastic part value of the skin without the use of the product according to the invention and the aforementioned comparative product is denoted Uv-0The value of the viscoelastic part of the skin when using the product of the invention and the aforementioned comparative product is once denoted as Uv-Hair 1～Uv-Hair 6，Uv-to-1～Uv-to-5，Uv-Hair 1～Uv-Hair 6And Uv-to-1～Uv-to-5Subtract U respectivelyv-0Is divided by Uv-0The percentage value of (A) is the skin elasticity increase rate.
All data are averaged after the test and the results of the rate of increase in skin elasticity are shown in Table 3-2.
TABLE 3-2 statistical data of anti-aging experiments
Figure BDA0002419080400000091
And (3) test data show that: the product of the invention has good anti-aging performance.
Second, test of whitening effect
(1) Experimental methods
Volunteers: a total of 330 normal women aged 30-60 years were divided into 11 groups of 30 persons each for the invention and control groups. Every person used 1g of the product of the invention every morning and evening for 8 weeks, while all other whitening skin care products were discontinued during the test period.
The volunteers were asked to follow up at the same time during the day at each visit 0 week before use and at 2, 4 and 8 weeks after use, for a total of 4 times. Before each test, the volunteers washed their faces with facial cleanser and gently dried their face water with a paper towel, and after sitting still for 30min in a constant temperature and humidity (room temperature (20 ± 2 ℃) and relative humidity 50% ± 5%), they were tested by technicians.
(2) Black redness of facial skin
The blackness values of the left and right cheek regions were measured using a skin blackness tester, and the average was taken 3 times. Facial skin L and b values: values of L and b were measured for the left and right cheek areas using a cantoda analyzer tester and averaged 2 times. L indicates brightness, and the higher the value of L, the more white the skin is; b indicates the range from yellow to blue, and the lower the value of b, the lower the yellowness of the skin.
The test results are shown in tables 3-3, 3-4, and 3-5.
(3) Subjective evaluation of volunteers: volunteers evaluated their skin condition at visits of weeks 4 and 8, respectively; at the visit of week 8, the product was completed using questionnaires, the product efficacy was evaluated according to the subjective experience of the individual, the average of the available questionnaires was taken, but the volunteers were no less than 90.
Subjective evaluations were made on the product at week 4 and 8 follow-up visits. The evaluation contents are:
1) subjective evaluation of skin condition: the skin moisture, the skin whiteness, the skin glossiness and the overall skin state are graded by 1-5 grades, 1 grade-obviously worsened, 2 grades-obviously worsened, 3 grades-unchanged, 4 grades-slightly better, and 5 grades-obviously better.
2) Subjective evaluation of skin problems: can improve the conditions of skin darkness, skin color spots, skin dryness, roughness, dullness and uneven skin color: the scoring standard of 1-5 points is adopted, 1 point is changed, 2 points are unchanged, 3 points are common/some, 4 points are better/more, and 5 points are better/more.
3) Stress response after use: for improving the conditions of erythema/rash (redness and swelling), pruritus, dryness, desquamation, tingling sensation, acne and the like, a rating standard of 1-5 points is adopted, 1 point is zero, 2 points are slight/few, 3 points are normal/some, 4 points are more/more, and 5 points are more.
The statistics of the evaluation results are shown in tables 3-6.
(4) Evaluation by professional personnel:
at the follow-up of weeks 4 and 8, respectively, the facial skin condition of the volunteers was evaluated, and the average of the effective evaluations was taken, but the number of evaluations was not less than 90.
Professional evaluation is carried out on the product at the follow-up visit of 4 and 8 weeks, and the evaluation contents are as follows:
1) for evaluation of the skin whiteness, a scoring standard of 1-5 points is adopted, 1 point is obviously deteriorated, 2 points are obviously deteriorated, 3 points are unchanged, 4 points are slightly improved, and 5 points are obviously improved;
2) evaluation of skin brightness: the grading standard of 1-5 grades is adopted, wherein 1 grade is zero, 2 grades is slightly bright, 3 grades is bright, 4 grades is obviously bright, and 5 grades is very bright;
3) evaluation of the depth of color unevenness: adopting a grading standard of 1-9 points, wherein 1 point is zero, 2-4 points are slightly lightened, 5-7 points are lightened, and 8-9 points are obviously lightened;
4) the overall skin state: by adopting a grading standard of 1-6 grades, 1 grade is obviously worsened, 2 grades is worsened, 3 grades is unchanged, 4 grades is slightly improved, 5 grades is obviously improved, and 6 grades is very good.
The statistics of the evaluation results are shown in tables 3-7.
(5) The result of the detection
The results of the blackness test are the blackness values shown in tables 3-3.
TABLE 3-3 results of the jetness test
Figure BDA0002419080400000101
Figure BDA0002419080400000111
According to the skin blackness value test result, the product has the effect of reducing the skin blackness, so that the skin color is brightened, and the effect of whitening the skin is achieved.
Tables 3-4 show the results of the skin L value test, and tables 3-5 show the results of the skin b value test.
Table 3-4 skin L value test results
Figure BDA0002419080400000112
According to the skin brightness L value test result, the product can directly improve the skin brightness, so that the effect of whitening the skin is achieved.
Tables 3-5 skin b values test results
Figure BDA0002419080400000121
According to the result of the skin yellowness b value test, the product has the effect of reducing the skin yellowness b value, and can improve the skin dullness and increase the whiteness.
Tables 3-6 show the results of subjective evaluations of volunteers.
Tables 3-6 subjective evaluation results of volunteers
Figure BDA0002419080400000122
Figure BDA0002419080400000131
According to the subjective evaluation results of volunteers, the skin moistening degree, the skin whitening degree, the skin glossiness and the overall skin state are greatly improved; the skin is dull, the skin color spot, the skin dryness, the roughness and the dull luster and the uneven skin color are greatly improved; the stress response appeared after the application is scored, and dryness, desquamation, pruritus, erythema/rash and pox hardly appear, which indicates that the product has good safety.
Tables 3 to 7 show the results of evaluation by the skilled worker.
TABLE 3-7 evaluation results of professionals
Figure BDA0002419080400000132
As can be seen from the evaluation of professional personnel, the product is very helpful for improving various indexes of the skin.
Third, testing anti-inflammatory and bacteriostatic effects
And (3) testing the antibacterial performance: the products of invention groups 1-6 were tested.
Bacillus subtilis, and the strain source is as follows: beijing Beinanna institute of Biotechnology, Strain No.: s-10069-250 MG;
coli: the strain source is as follows: beijing Beinanna institute of Biotechnology, Strain No.: s-48275-25 MG-F;
staphylococcus aureus: the strain source is as follows: beijing Beinanna institute of Biotechnology, Strain No.: s-77140-25 MG;
candida albicans: the strain source is as follows: beijing Zhongke quality testing Biotech Co., Ltd, strain No.: CL 1502;
pseudomonas aeruginosa: the strain source is as follows: beijing Zhongke quality testing Biotech Co., Ltd, strain No.: ZKCCT-132;
propionibacterium acnes: the strain source is as follows: beijing Zhongke quality testing Biotech Co., Ltd, strain No.: CL 7052.
Preparation of experimental bacterial suspension: bacillus subtilis, Escherichia coli, Staphylococcus aureus, Candida albicans, Pseudomonas aeruginosa and Propionibacterium acnes are cultured in a test tube culture medium at 37 ℃ for 48 hours in a thermostat, then aseptically treated ultrapure water is added, and the mixture is shaken to obtain an experimental bacteria suspension.
15mL of the melted SOB medium was taken and placed in a sterile plate, and then 1mL of the experimental strain was added dropwise and allowed to spread flat on the bottom of the plate. After the culture medium is solidified, 4 Oxford cups are vertically placed on each flat plate, then 0.1mL of experimental sample is respectively added, after the culture is carried out for 24 hours at 37 ℃, the size (unit: mm) of the diameter of the inhibition zone is respectively measured, each experimental group is repeated for 3 times, the average value of the experimental results is obtained, and the results are shown in Table 4, so that the product has good antibacterial effect.
TABLE 4
Figure BDA0002419080400000141
Fourth, moisture retention Performance test
Volunteers: a total of 330 normal women aged 30-60 years were divided into 11 groups of 30 persons each for the invention and control groups. After 2 hours of skin cleansing, the product of the invention and the comparative product (1 g each) were applied and skin moisture was measured at 1h, 4h, 8h, 12h, 16h and 24h, respectively. The measurements were carried out using a skin moisture tester of Delfin vapormer, finland at 25 ℃, 50% relative humidity, averaged and the results are given in table 5.
TABLE 5
Figure BDA0002419080400000151
Acne treatment test
Volunteer experiments: 220 persons of the volunteers of the acne patients are divided into 11 groups, 20 persons of each invention group and each comparison group continuously use the essence for 15 days and 30 days, then the complete elimination rate of the acne is counted, the average value is taken, and the result is shown in table 6, so that the acne removing effect of the acne removing product is obvious.
TABLE 6
Figure BDA0002419080400000152
Figure BDA0002419080400000161
The embodiment data of the invention is representative/exemplary data, a scheme adopting other values in the numerical range required by the invention is also implemented, and the experimental data has no obvious difference from the exemplary data, namely, the technical effect of the invention can be realized; limited to space, not to an array.

Claims (18)

1. A modified attapulgite is characterized in that the attapulgite powder is obtained by modifying polysaccharide, wherein the polysaccharide is one or more selected from zymosan, aloe barbadensis leaf polysaccharide, Aphanothece crispa polysaccharide, lima bean seed polysaccharide, tuberose polysaccharide, euglena minuta polysaccharide and Cassia angustifolia seed polysaccharide;
the modified attapulgite is obtained by uniformly mixing attapulgite powder and polysaccharide in an organic solvent, adding an acid solution, and removing generated water until no water is generated.
2. The modified attapulgite of claim 1, wherein: the polysaccharide is
Is zymosan;
the attapulgite powder is more than 2000 meshes.
3. The modified attapulgite of claim 2, wherein: the attapulgite powder is 2000-3000 meshes.
4. A process for preparing the modified attapulgite of any of claims 1 to 3, characterized in that: preparing attapulgite powder into organic solvent suspension, adding polysaccharide, stirring, adding concentrated sulfuric acid or nitric acid, stirring, removing water until no water is generated, press filtering, washing, and drying.
5. The method according to claim 4, wherein the organic solvent is dehydrated ether or petroleum ether or ethyl acetate.
6. The preparation method according to claim 4, wherein the attapulgite powder is prepared into an anhydrous ether suspension with a mass concentration of 5%, the polysaccharide is added, after uniform stirring, concentrated sulfuric acid with one ten-thousandth of the mass of the attapulgite is added dropwise, the reaction is carried out under stirring at 45 ℃, and the generated water is removed under stirring until no water is generated.
7. The method of claim 4, wherein: the feeding amount of the polysaccharide is 1-10% of the mass of the attapulgite powder.
8. The method of claim 4, wherein: the feeding amount of the polysaccharide is 3-8% of the mass of the attapulgite powder.
9. The method of claim 4, wherein: the feeding amount of the polysaccharide is 5% of the mass of the attapulgite powder.
10. Use of the modified attapulgite of any one of claims 1-3 in the preparation of a medicament for external use or a skin care product.
11. The use of claim 10, wherein in the external medicament or skin care product, the modified attapulgite comprises the following components in percentage by mass: 0.1-5%;
the external medicine is antibacterial and anti-inflammatory ointment;
the skin care product refers to a daily skin care product.
12. The use according to claim 11, wherein the modified attapulgite is present in the medicament or skin care product for external use in an amount of 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1.0%, 1.1%, 1.2%, 1.5%, 2.0%, 3.0%, 4.0%, 5.0% by mass.
13. An external preparation for skin, wherein the modified attapulgite in any one of claims 1 to 3 is prepared from the following components in percentage by mass: 0.1-5%, wherein the skin external preparation is an external medicine or a skin care product;
the external medicine is antibacterial and anti-inflammatory ointment;
the skin care product refers to a daily skin care product.
14. The external skin preparation according to claim 13, wherein the modified attapulgite is present in the external medicament or skin care product in an amount of 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1.0%, 1.1%, 1.2%, 1.5%, 2.0%, 3.0%, 4.0%, 5.0% by mass.
15. An external preparation for skin according to claim 13, wherein: the composite material comprises the following components in parts by weight: 0.1-5 parts of modified attapulgite, 25-40 parts of astragalus extract, 10-25 parts of angelica extract, 1-10 parts of aloe vera gel, 0.1-1 part of pearl powder and 10-20 parts of hyaluronic acid.
16. An external preparation for skin according to claim 15, wherein: the particle size of the radix astragali extract powder and the radix Angelicae sinensis extract powder is above 250 mesh.
17. An external preparation for skin according to claim 15, wherein: also contains 20-35 parts of sterile water.
18. An external preparation for skin according to claim 15, wherein: the astragalus extract or the angelica extract is prepared by the following method: cleaning radix astragali or radix Angelicae sinensis, slicing, drying, pulverizing, adding water, stirring, extracting water soluble components by low temperature and high pressure difference continuous cell wall breaking extraction technology, concentrating the water solution, freeze drying, and pulverizing.
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