CN114504533A - Moisture mask and preparation method thereof - Google Patents

Moisture mask and preparation method thereof Download PDF

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Publication number
CN114504533A
CN114504533A CN202011281759.3A CN202011281759A CN114504533A CN 114504533 A CN114504533 A CN 114504533A CN 202011281759 A CN202011281759 A CN 202011281759A CN 114504533 A CN114504533 A CN 114504533A
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hyaluronic acid
mask
dendrobium
dendrobium nobile
moisture mask
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CN114504533B (en
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董银卯
曲召辉
赵迪
刘盼玉
刘有停
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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]
    • A61K8/9794Liliopsida [monocotyledons]
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/02Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/0212Face masks
    • 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
    • A61K8/735Mucopolysaccharides, e.g. hyaluronic acid; Derivatives thereof
    • 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
    • A61K2800/20Chemical, physico-chemical or functional or structural properties of the composition as a whole
    • A61K2800/30Characterized by the absence of a particular group of ingredients
    • 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
    • A61K2800/805Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95

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Abstract

The invention discloses a moisturizing mask and a preparation method thereof. The dendrobium nobile hyaluronic acid extract is prepared from dendrobium nobile and hyaluronic acid according to the mass ratio of 1:2-6:1 under the conditions of high temperature and high pressure, and the molecular weight of the raw material hyaluronic acid is 120-180 ten thousand Da. The moisturizing mask disclosed by the invention can solve the problem of poor film cloth carrying capacity without adding a thickening agent, simplifies the formula components and reduces unnecessary raw material risks. Meanwhile, experiments prove that the mask has a good moisturizing effect, and compared with commercially available competitive products, the mask is longer in skin adhering time and free of tight feeling after adhering.

Description

Moisture mask and preparation method thereof
Technical Field
The invention relates to the field of skin care products, and in particular relates to a moisturizing mask containing dendrobium nobile hyaluronic acid and a preparation method thereof.
Background
The reason for skin dryness is researched and mainly comprises the following three aspects: firstly, the external environment is rapidly deteriorated due to global climate change, the skin is dry, tight, itchy and peeled due to high-intensity ultraviolet rays, dust smoke pollution and excessive use of a surfactant, and the skin barrier is damaged and accelerated to age to form a vicious circle in severe cases; secondly, with the age, the moisture content in the skin also decreases year by year, and when the moisture content of the horny layer decreases below 10%, the skin also becomes dry obviously, loses elasticity and is easy to wrinkle; thirdly, dark, dull and rough skin color caused by long-term living stress and irregular work and rest is also one of the troubling problems. Therefore, moisturizing plays an important role in maintaining the normal state of skin and is a prerequisite for ensuring the health of skin, so that the effect of moisturizing products is also valued by consumers.
The facial mask is a common skin care product, has various types and functions, and is divided into a common paste type facial mask, a coating type powder facial mask, a paste type facial mask, a tearing facial mask and the like from the aspect of using methods; it is also classified into moisturizing, whitening, anti-aging, anti-acne, etc. in terms of efficacy. The facial mask with the moisturizing effect is mainly a patch facial mask, and is more popular and concerned by consumers than other effects.
At present, the number of moisturizing facial masks in the market is small, but the problem that the liquid carrying amount of a mask cloth is not good is common. In order to solve the problem of poor liquid distribution quantity of the membrane, a thickening agent which takes xanthan gum, carbomer and other raw materials as main materials is added. However, the addition of the thickener causes the mask to have poor skin feel, and further causes the mask to have short skin-attaching time.
Therefore, it is a technical problem to be solved by those skilled in the art to develop a facial mask which improves the problem of poor liquid carrying capacity of a mask cloth without adding a thickener, and ensures good skin feel, long skin-contact time, and excellent moisture retention performance.
Hyaluronic acid is one of glycosaminoglycans, belongs to acidic mucopolysaccharide, and is widely distributed in various parts of the human body. Hyaluronic acid has a special water retention effect, is the substance which is found to have the best moisture retention in nature at present, and is called an ideal natural moisture retention factor. Hyaluronic acid is often added into cosmetics to enhance the effects of moisturizing, resisting aging and the like. Dendrobium officinale is a perennial epiphytic herb plant, has a long medicinal history and is listed as the head of 'Jiudao sianchau', and the dendrobium officinale contains substances such as polysaccharide, flavonoid, phenols, vitamins, amino acid and the like. At present, the dendrobium officinale polysaccharide is mainly composed of mannose and glucose, contains rich O-acetyl, and has strong oxidizing capability and free H + ions. The dendrobium extract has unique moistening feeling, and can make the product have unique skin feeling such as skin affinity, moistening, smoothness and the like when being used in cosmetics.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide the moisturizing mask and the preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
in one aspect, the present invention provides a moisturizing mask, comprising: herba dendrobii hyaluronic acid extract and common auxiliary materials in the field of skin care products.
According to the invention, the dendrobium nobile and the hyaluronic acid are prepared from the following components in parts by mass: dendrobe: hyaluronic acid =1:2-6:1, and may be, for example, 1:2, 3:5, 7:10, 3:4, 4:5, 1:1, 2:1, 3:1, 4:1, 5:1, 6:1, and the points between the above ratios, which are not described in detail for reasons of space limitation.
According to the invention, the molecular weight of the starting material hyaluronic acid is between 120 and 180 million Da.
According to the invention, the raw material dendrobium is preferably dendrobium officinale.
According to the invention, the dendrobium nobile hyaluronic acid extract is prepared by a preparation method comprising the following steps:
(a) weighing a certain mass part of dendrobium, and soaking in deionized water for 0.5-1.5 h;
(b) pouring out the soaked water, and adding deionized water according to the material-liquid ratio of 1:20-1:100 (m/m);
(c) adding a certain mass part of hyaluronic acid, wherein the hyaluronic acid is uniformly dispersed by using 5-15 wt% of a dispersing agent based on the mass of deionized water;
(d) extracting in high temperature and high pressure equipment at the pressure of 0.05-0.13 MPa and the temperature of 110-.
According to the invention, in the step (a), the dendrobium nobile is soaked after being cut into small sections of about 1 cm.
According to the invention, in the step (b), the ratio of the dendrobium to the deionized water is 1:20-1:100, for example, 1:20, 1:21, 1:22, 1:23, 1:24, 1:25, 1:30, 1:32, 1:35, 1:36, 1:38, 1:39, 1:40, 1:41, 1:42, 1:43, 1:45, 1:46, 1:47, 1:48, 1:50, 1:51, 1:52, 1:53, 1:54, 1:55, 1:56, 1:57, 1:58, 1:59, 1:60, 1:62, 1:63, 1:64, 1:65, 1:67, 1: 68. 1:69, 1:70, 1:72, 1:73, 1:74, 1:75, 1:76, 1:78, 1:80, 1:82, 1:83, 1:84, 1:85, 1:86, 1:87, 1:88, 1:90, 1:92, 1:93, 1:94, 1:95, 1:96, 1:97, 1:98, 1:99, 1:100, and the values therebetween, and are not repeated for reasons of brevity.
According to some preferred embodiments of the invention, the feed-liquid ratio of the dendrobium to the deionized water is 1:50-1: 80.
According to the invention, the dispersant in the step (c) is a dispersant which is conventional in the field of skin care products.
According to the invention, the dispersant is glycerol.
According to some preferred embodiments of the present invention, the step (d) is extracting in a high temperature and high pressure device at an extraction pressure of 0.07-0.10 MPa and a temperature of 115-120 ℃ for 1-3h to obtain the hyaluronic acid extract of dendrobe.
According to some preferred embodiments of the present invention, the step (d) is extracting in a high temperature and high pressure device for 1-3h, wherein the extraction pressure is 0.07MPa and the temperature is 115 ℃ to obtain the hyaluronic acid extract of dendrobium nobile lindl.
According to the invention, the molecular weight of the dendrobium nobile hyaluronic acid extract is 600 Da-70 ten thousand Da.
According to the invention, the viscosity of the dendrobium nobile hyaluronic acid extract is 675-1026 mPa-s.
According to the invention, the common auxiliary materials in the field of skin care products in the moisture mask comprise one or more of a preservative, a chelating agent and polyhydric alcohol.
According to the invention, the auxiliary material components account for 0.10-1.00wt% of preservative, 0.02-0.10wt% of chelating agent and 0.0-30.00wt% of polyalcohol based on the total weight of the mask.
According to the invention, the preservative is a preservative acceptable in the field of skin care products, such as: one or more of caprylyl hydroximic acid/1, 2-hexanediol/1, 3-propanediol, phenoxyethanol, carnation ketone, glyceryl caprylate/caprylyl hydroximic acid/1, 2-pentanediol and 1, 2-hexanediol.
According to some preferred embodiments of the invention, the preservative is phenoxyethanol.
According to the invention, the polyols are polyols acceptable in the field of skin care products, such as: one or more of glycerol, butanediol, propylene glycol and dipropylene glycol.
According to some preferred embodiments of the invention, the polyol is glycerol.
According to the invention, the chelating agent is a chelating agent acceptable in the field of skin care products, such as: one or more of disodium EDTA, sodium glucoheptonate, trisodium EDTA and tetrasodium EDTA.
According to some preferred embodiments of the invention, the chelating agent is disodium EDTA.
In another aspect, the present invention provides a method for preparing a moisturizing mask, the method comprising: the raw materials are added in sequence according to the adding sequence and stirred evenly.
According to the invention, the raw materials are added with the dendrobium nobile hyaluronic acid extract, the preservative, the polyalcohol and the chelating agent in sequence.
Compared with the prior art, the invention has the beneficial effects that at least:
(1) the dendrobium hyaluronic acid extract used in the mask is obtained by high-temperature high-pressure extraction, the molecular weight of the hyaluronic acid is reduced, the stability of dendrobium is improved, and the dendrobium hyaluronic acid extract has good skin feel and moisturizing effect.
(2) The facial mask liquid provided by the invention utilizes the viscosity of the extracting solution, and the viscosity is still higher than that of a commercially available facial mask liquid under the condition of not adding a thickening agent, so that the aims of not adding a thickening agent, simplifying formula components and reducing unnecessary raw material risks are fulfilled.
(3) The mask disclosed by the invention is not added with a thickening agent, so that the skin feel is improved, the moisturizing effect is good, the skin attaching time of the mask is prolonged, and meanwhile, the tight feeling is not brought to a user.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the following will be briefly described.
FIG. 1 is a picture of extracts prepared in example 1 (center), comparative example 1 (right), and comparative example 2 (left);
FIG. 2 is a graph showing the results of skin feel tests of extracts prepared in example 1, comparative example 1 and comparative example 2;
FIG. 3 shows the stability observation results of the dendrobe extract in comparative example 3 (left) and the dendrobe extract in comparative example 4 (right);
FIG. 4 is a graph showing the results of observing the stability of the extract prepared in example 1;
FIG. 5 shows the moisture content test results of the masks of example 4 and comparative example 5;
FIG. 6 is a graph showing the results of the residual membrane liquid amount test in example 4 and comparative example 5;
FIG. 7 is a graph showing the results of the facial masks applied for 0min, 15min, 20min and 25min in example 4 and comparative example 5.
The specific implementation mode is as follows:
to further illustrate the technical means and effects of the present invention, the present invention is further described with reference to the following examples. It is to be understood that the specific embodiments described herein are merely illustrative of the invention and are not limiting of the invention. The examples, which are not specifically shown for the specific methods, are all routine in the art or according to the product specifications. The reagents or apparatus used are conventional products commercially available from normal sources, not indicated by the manufacturer.
Table 1 raw materials supplier list
Figure 149731DEST_PATH_IMAGE002
The apparatus used in the present invention is shown in table 2 below:
TABLE 2 Instrument information and uses
Figure 879921DEST_PATH_IMAGE004
Example 1
(1) Weighing 20g of dendrobium, soaking in deionized water for 1h, and pouring out the soaked water;
(2) adding 1400g of water according to the dendrobium water ratio of 1: 70;
(3) then adding 14g of hyaluronic acid, and uniformly dispersing the hyaluronic acid by using 140g of glycerol;
(4) extracting in high temperature and high pressure equipment at 0.07MPa and 115 deg.C for 1 hr to obtain herba Dendrobii hyaluronic acid extract.
Example 2
(1) Weighing 20g of dendrobe, soaking in deionized water for 0.5h, and pouring out the soaked water;
(2) adding 400g of water according to the dendrobium water ratio of 1: 20;
(3) then adding 4g of hyaluronic acid, and uniformly dispersing the hyaluronic acid by using 60g of glycerol;
(4) extracting in high temperature and high pressure equipment at 0.07MPa and 115 deg.C for 3 hr to obtain herba Dendrobii hyaluronic acid extract.
Example 3
(1) Weighing 10g of dendrobe, soaking in deionized water for 1.5h, and pouring out the soaked water;
(2) adding 1000g of water according to the dendrobium water ratio of 1: 100;
(3) adding 20g of hyaluronic acid, and uniformly dispersing the hyaluronic acid by using 50g of glycerol;
(4) extracting in high temperature and high pressure equipment for 2h at 0.10 MPa and 120 deg.C to obtain herba Dendrobii hyaluronic acid extract.
Example 4
The formulation of the moisturizing mask is shown in table 3.
Table 3 dendrobium nobile hyaluronic acid moisturizing mask formula
Figure 721975DEST_PATH_IMAGE006
And (3) sequentially adding the raw materials according to the sequence numbers and the corresponding addition amounts, and uniformly stirring to obtain the moisturizing mask liquid.
Example 5
The formulation of the moisturizing mask is shown in table 4.
Table 4 dendrobium nobile hyaluronic acid moisturizing mask formula
Figure 933163DEST_PATH_IMAGE008
And (3) sequentially adding the raw materials according to the sequence numbers and the corresponding addition amounts, and uniformly stirring to obtain the moisturizing mask liquid.
Example 6
The formulation of the moisturizing mask is shown in table 5.
TABLE 5 Dendrobium nobile hyaluronic acid moisturizing mask formula
Figure 809852DEST_PATH_IMAGE010
And (3) sequentially adding the raw materials according to the sequence numbers and the corresponding addition amounts, and uniformly stirring to obtain the moisturizing mask liquid.
Example 7
The formulation of the moisturizing mask is shown in table 6.
TABLE 6 Dendrobium nobile hyaluronic acid moisturizing mask formula
Figure 445364DEST_PATH_IMAGE012
And (3) sequentially adding the raw materials according to the sequence numbers and the corresponding addition amounts, and uniformly stirring to obtain the moisturizing mask liquid.
Comparative example 1
(1) Weighing 20g of dendrobium, soaking in deionized water for 1h, and pouring out the soaked water;
(2) adding 1400g of water according to the dendrobium water ratio of 1: 70;
(3) adding 14g of hyaluronic acid, and uniformly dispersing the hyaluronic acid by using 140g of glycerol;
(4) extracting at 85 deg.C under normal pressure for 1 hr to obtain herba Dendrobii hyaluronic acid extract.
Comparative example 2
The preparation process is the same as that in example 1 except that dendrobium is not added, so that the hyaluronic acid extract without dendrobium is obtained.
(1) Weighing 14g of hyaluronic acid, and uniformly dispersing the hyaluronic acid by using 140g of glycerol;
(2) extracting in high temperature and high pressure equipment at 0.07MPa and 115 deg.C for 1 hr to obtain hyaluronic acid extract.
Comparative example 3
The same procedure as in example 1 was repeated except that hyaluronic acid was not added to obtain a dendrobe extract.
(1) Weighing 20g of dendrobium, soaking in deionized water for 1h, and pouring out the soaked water;
(2) adding 1400g of water according to the dendrobium water ratio of 1: 70;
(3) extracting in high temperature and high pressure equipment at 0.07MPa and 115 deg.C for 1 hr to obtain herba Dendrobii extract.
Comparative example 4
The same as in comparative example 3 except for the temperature and pressure, the dendrobe extract under normal pressure water extraction was obtained.
(1) Weighing 20g of dendrobium, soaking in deionized water for 1h, and pouring out the soaked water;
(2) adding 1400g of water according to the dendrobium water ratio of 1: 70;
(3) extracting at 85 deg.C under normal pressure for 1 hr to obtain herba Dendrobii extract.
Comparative example 5
The moisture-keeping mask comprises the following components in parts by weight:
water, butylene glycol, glycerin, caprylyl hydroxamic acid, glyceryl caprylate, propylene glycol, hydroxyethyl cellulose, betaine, trehalose, glyceryl acrylate/acrylic acid copolymer, PVM/MA copolymer, p-hydroxyacetophenone, 1, 2-pentanediol, hydroxyphenyl propionamide benzoic acid, allantoin, acrylic acid/C10-30 alkanol acrylate crosspolymer, tromethamine, sodium hyaluronate, disodium EDTA, PEG-40 hydrogenated castor oil, DENDROBIUM officinale (Dendrobium CANDIDUM) stem extract, hyaluronic acid, essence, tridecyl alcohol polyether-9, xanthan gum, hydrolyzed sodium hyaluronate, sodium acetylated hyaluronate, and the like.
Efficacy evaluation experiments.
Skin feeling and appearance evaluation of dendrobium nobile hyaluronic acid extract
The inventors evaluated skin feel and appearance of the extracts prepared in the above examples and comparative examples. The result shows that the dendrobium hyaluronic acid extract solution prepared by the high-temperature high-pressure method in the embodiment of the invention is clear and transparent, has moderate viscosity, and has moist and non-sticky skin feel. The extracts prepared in the comparative examples were different in skin feel or appearance. Wherein, the dendrobium hyaluronic acid (right part of figure 1) solution prepared by the normal pressure water extraction method in the comparative example 1 is turbid, has a dark color, is slightly thick, has sticky and greasy skin feel, has astringent feel on hands, and has membrane forming feel after being dried and poor skin feel. Comparative example 2 hyaluronic acid (left in fig. 1) prepared at high temperature and high pressure was thick, sticky to the skin, astringent to the upper hand, and tight.
The extracts prepared in example 1 (middle), comparative example 1 (right) and comparative example 2 (left) are shown in fig. 1.
(II) testing viscosity and molecular weight of dendrobium nobile hyaluronic acid extract
The dendrobium polysaccharide has active H ions under the high-temperature and high-pressure environment of the solution, so that the pH value of the solution environment reaches about 4.5. It is reported that in an acidic environment (pH = 2-4.5), the degree of deprotonation of hydroxyl groups of hyaluronic acid is reduced, and mainly negatively charged carboxyl groups attack epoxy groups to form ester bonds, so that hydroxyl groups are modified to form mainly ether-based products, and carbon-carbon double bonds can be cleaved to form relatively independent small hyaluronic acid molecules. Therefore, the combination of dendrobium and hyaluronic acid can effectively reduce the molecular weight of hyaluronic acid.
The viscosity has a certain relationship with the molecular weight of hyaluronic acid, and the size of the molecular weight can be expressed by the viscosity. According to a Mark-Houwink formula:
Figure 774714DEST_PATH_IMAGE013
wherein, the [ alpha ], [ beta ] -aƞ]Which represents the viscosity of the hyaluronic acid and,Mrepresents the molecular weight of hyaluronic acid, K is an characterizing linear constant,αis a coefficient relating to the shape of the hyaluronic acid chain, K andαis a constant. From the Mark-Houwink formula, the viscosity of hyaluronic acid is higher and the molecular weight is higher when the solvent and the temperature are fixed.
TABLE 7 comparison of viscosity of different examples or comparative examples
Figure DEST_PATH_IMAGE015
The viscosities of examples 1-3, comparative example 1 and comparative example 2 were measured using a digital rotational viscometer with a number 2 spindle at 6 RPM.
As shown in Table 7, the hyaluronic acid of Dendrobium nobile in comparative example 2, i.e., high temperature and high pressure, had a viscosity of 1050 mPas, the hyaluronic acid of Dendrobium nobile in example 1, i.e., high temperature and high pressure, had a viscosity of 675 mPas, and the hyaluronic acid of Dendrobium nobile in comparative example 1, i.e., water extract, had a viscosity of 3045 mPas. Compared with the high-temperature high-pressure hyaluronic acid (comparative example 2), the viscosity of the high-temperature high-pressure dendrobium hyaluronic acid (example 1) is reduced, which shows that the addition of dendrobium nobile of the invention greatly reduces the molecular weight of hyaluronic acid. Through the comparison of the viscosities of the example 1 and the comparative example 1, the viscosity of the hyaluronic acid of dendrobium under the normal pressure condition is much higher than that of the hyaluronic acid of dendrobium under the high temperature and high pressure process. The molecular weight of hyaluronic acid is greatly reduced by the high-temperature high-pressure process and the addition of dendrobium.
Comparative example 2, i.e., the viscosity of hyaluronic acid extracted under high temperature and high pressure conditions was also reducedSince the degradation rate of the molecular weight of hyaluronic acid increases with the increase of temperature, the molecular weight of hyaluronic acid is decreased under the conditions of high temperature and high pressure. But compared with the high-temperature high-pressure dendrobium hyaluronic acid (example 1), dendrobium is lacked, and the skin feel of the high-temperature high-pressure dendrobium hyaluronic acid is poor; although the viscosity of hyaluronic acid is also reduced by the high-temperature and high-pressure process, the molecular weight of hyaluronic acid is reduced by breaking the C = C bond under the high-temperature condition, and the viscosity is also reduced, unlike the mechanism of adding dendrobium. The dendrobium hyaluronic acid extract prepared by the embodiment of the invention combines dendrobium with hyaluronic acid, and dendrobium polysaccharide contains free H+Ions, providing acidic conditions, with OH groups in the hyaluronic acid molecule-A chemical reaction occurs, thereby reducing the molecular weight of the hyaluronic acid. And the dendrobium has unique moistening feeling, and dendrobium polysaccharide is combined with hyaluronic acid to react, so that the molecular weight of hyaluronic acid is reduced, the moistening feeling of a dendrobium hyaluronic acid system is greatly improved, and the skin feeling of the whole system is improved. The hyaluronic acid added with the dendrobium not only solves the skin feeling of tight film formation caused by too large molecular weight, but also improves the moistening feeling and the smooth feeling.
(III) skin feel test of dendrobium nobile hyaluronic acid extract
20 subjects were recruited, 3 areas 1,2, 3 were drawn on the arm, and the samples of example 1, comparative example 1 and comparative example 2 were applied, respectively. And (4) scoring the skin feel after trial, wherein the total score of each item is 5 points.
A skin-feel radar plot is shown in fig. 2.
Compared with the comparative example, the dendrobium nobile hyaluronic acid extract prepared by the embodiment of the invention has excellent effects in the aspects of sticky feeling, moistening degree, absorption speed, tender feeling and the like.
(IV) testing physical and chemical properties of dendrobium nobile hyaluronic acid extract
The pH, molecular weight, color, consistency and skin feel of examples 1-3 and comparative examples 1-2 were evaluated and the extracts prepared in the examples and comparative examples were compared for differences in various indices.
Table 8 comparison of indexes of extracts prepared in inventive example and comparative example
Figure DEST_PATH_IMAGE017
The pH value of hyaluronic acid is generally between 6 and 7.5, and the pH value of dendrobe polysaccharide is generally about 4.5. As shown in table 8, the hyaluronic acid (comparative example 2) at high temperature and high pressure had a pH of 6.38, and the molecular weight was slightly decreased; after hyaluronic acid reacts with dendrobium under the high-temperature high-pressure process (example 1), the pH value is changed to 5.02, and the reaction between dendrobium and hyaluronic acid can be shown through the change of pH. The pH value of the dendrobium hyaluronic acid prepared by the water extraction method (comparative example 1) is also reduced, but the reduction range is smaller compared with that of the high-temperature high-pressure process. From the view of molecular weight, the high-temperature and high-pressure process has small influence on the molecular weight of the hyaluronic acid, which indicates that dendrobium is an essential factor for the change of the molecular weight of the hyaluronic acid. The addition of the dendrobium and the high-temperature and high-pressure process play a role in reducing the molecular weight of hyaluronic acid.
(V) Dendrobium nobile hyaluronic acid extract stability observation experiment
The dendrobium extract has poor stability in the raw material end of cosmetics, and is easy to precipitate. The stability of the dendrobium is enhanced through the combination of the dendrobium hyaluronic acid. Fig. 3 shows that the dendrobium extract prepared by the method of comparative example 3 and comparative example 4 is not precipitated and has stable state after being placed for two days under daily conditions, and the finished product is unstable and has unnecessary troubles when being directly applied to cosmetics due to shaking, but the dendrobium extract is greatly improved in stability after being combined with hyaluronic acid, and the hyaluronic acid of dendrobium under high temperature and high pressure is observed after 30 days (example 1). As shown in fig. 4.
(VI) mask liquid viscosity test
And (3) viscosity testing: standing the facial mask solution to be measured in a straight-tube container, discharging air, keeping the temperature constant at 25 ℃, and measuring the viscous resistance and the dynamic viscosity of the liquid by using a digital display rotational viscometer. The larger the viscous resistance of the rotor to the tested mask liquid is, the larger the reading is, and the higher the viscosity of the mask liquid is; conversely, the lower the viscous resistance of the rotor to the tested mask liquid, the lower the reading, indicating the lower the viscosity of the mask liquid.
And (3) testing a sample: example 4 and comparative example 5
And (3) testing results: as shown in Table 9, the viscosity of the mask solution of example 4 was 186 mPas, and the viscosity of the mask solution of comparative example 5 was 131 mPas.
Table 9 comparison of facial mask fluid viscosity for inventive examples and comparative examples
EXAMPLE 4 facial mask solutions Comparative example 5 facial mask liquid
Viscosity of the oil 186mPa·s 131mPa·s
And (4) conclusion: the viscosity of the dendrobium hyaluronic acid extracting solution is still higher than that of the commercially available competitive product facial mask solution under the condition of not adding a thickening agent by using the viscosity of the dendrobium hyaluronic acid extracting solution, so that the addition of the thickening agent is not needed, the formula components are simplified, the requirement on the facial mask viscosity can be met, and the risk problem caused by complex raw material components can be reduced.
(VII) mask moisturizing efficacy test
And (3) testing the moisture content: water has a dielectric constant of 81, other substances generally have a dielectric constant of less than 7, and water is the substance with the highest dielectric constant on the skin. When the moisture content changes, the capacitance of the skin also changes, so the moisture content on the skin surface can be analyzed by measuring the capacitance of the skin, and the measured value is a relative value. A higher value indicates a higher moisture content of the stratum corneum and a better moisturizing effect.
The test method comprises the following steps: 30 subjects with normal skin were selected, and they were all male and female. The test subjects performed a half-face test according to the use requirements, and the facial mask of example 4 was applied to one side face and the facial mask of comparative example 5 was applied to the other side face. The moisture content of the stratum corneum was measured before, 10min after, 30min after, 1h after, and 2h after the application on the cheek areas of the subjects.
A detection instrument: corneometer for water content tester
And (3) testing a sample: example 4 and comparative example 5
And (3) testing results: as shown in table 10, the results of the moisture content test of example 4 were better than those of comparative example 5 at 10 minutes, 30 minutes, 1 hour and 2 hours after application of the masks of example 4 and comparative example 5.
Table 10 test results (unit C.U.) for skin moisture content of inventive and comparative facial masks
Product(s) Initial value 10min after application 30min after application 1h after application 2h after application
Example 4 26.93 36.92 35.77 33.26 34.47
Comparative example 5 27.45 35.36 33.80 31.49 30.22
And (4) conclusion: the moisturizing effect of the moisturizing mask disclosed by the invention within 2 hours after application is superior to that of a market competitive product.
(VIII) Membrane liquid Loading test
Testing the membrane liquid carrying capacity: respectively taking 30g of commercially available facial mask liquid and dendrobium hyaluronic acid moisturizing facial mask liquid, soaking for 20min by using the same facial mask cloth, taking out the facial mask cloth, standing over the rest of the facial mask liquid until the facial mask cloth does not drip, measuring the amount of the rest of the facial mask liquid, and calculating the carrying amount of the facial mask liquid. Membrane liquid deposition amount (g) = initial membrane liquid amount (g) -remaining membrane liquid amount (g).
And (3) testing a sample: example 4 and comparative example 5
And (3) testing results: as shown in Table 11, the amount of facial mask was 26.85g in example 4 and 23.53g in comparative example 5. The test procedure is shown in figure 6.
TABLE 11 test results of the membrane liquid-carrying capacity of the inventive and comparative examples
Product name Initial amount of Membrane liquid (g) Residual film liquid amount (g) Amount of suspension (g)
Comparative example 5 30.05g 6.52g 23.53g
Example 4 30.03g 3.18g 26.85g
And (4) conclusion: the experiment can obviously show that the mask liquid has obvious advantages when being compared with the hanging amount of the mask liquid sold in the market, and still has good film liquid hanging amount under the condition of not using a thickening agent.
(ninth) mask application time test
Testing the application time of the mask: the commercially available facial mask and the dendrobium hyaluronic acid moisturizing facial mask are respectively used, the facial mask is applied for about 15min according to the application requirements of the common facial masks, and the application conditions are respectively photographed at 0min, 15min, 20min and 25 min.
And (3) testing a sample: example 4 and comparative example 5
And (3) testing results: as shown in fig. 7, in comparative example 5, the mask started to be applied less frequently from 15 minutes to the mouth and nose, and was not applied more frequently than 25 minutes, and both the eyes, nose and edge were not applied. Example 4 the fit did not change significantly until 20 minutes of application, with a slight fit beginning at the nose and mouth at 25 minutes.
And (4) conclusion: the commercially available mask felt slightly dry at 15 minutes of application, and dried up around the nose, eyes, cheeks and lips at 20 minutes of application, and had a moist feel only at the edges of the mask cloth, so the commercially available mask application test was terminated at 20 minutes; the dendrobium hyaluronic acid moisturizing facial mask has no obvious drying within 0-20 minutes of application, and has tight feeling around lips within 25 minutes of application, and the tight degree is within the acceptance range of a subject.

Claims (10)

1. A moisture mask is characterized by comprising a dendrobium nobile hyaluronic acid extract and common auxiliary materials in the field of skin care products; the dendrobium nobile hyaluronic acid extract is prepared from dendrobium nobile and hyaluronic acid according to the mass ratio of 1:2-6:1, and the molecular weight of the raw material hyaluronic acid is 120-180 ten thousand Da.
2. The moisture mask as claimed in claim 1, wherein the dendrobium nobile hyaluronic acid extract is prepared by a method comprising the following steps:
(a) weighing a certain mass part of dendrobium, and soaking in deionized water for 0.5-1.5 h;
(b) pouring out the soaked water, and adding deionized water according to the material-liquid ratio of 1:20-1:100 (m/m);
(c) adding a certain mass part of hyaluronic acid;
(d) extracting in high temperature and high pressure equipment at the pressure of 0.05-0.13 MPa and the temperature of 110-.
3. The moisture mask as claimed in any one of claims 1 or 2, wherein in the preparation method of the dendrobium nobile hyaluronic acid extract, the extraction pressure is 0.07-0.1MPa, and the extraction temperature is 115-120 ℃.
4. The moisture mask as claimed in any one of claims 1 to 3, wherein hyaluronic acid is uniformly dispersed in step (c) of preparing hyaluronic acid extract of Dendrobium nobile by using dispersant in an amount of 5wt% -15wt% of deionized water in step (b).
5. The moisture mask as set forth in claim 4, wherein the dispersant is glycerin.
6. The moisture mask as claimed in any one of claims 1 to 5, wherein the hyaluronic acid extract of dendrobe has a molecular weight of 600 Da to 70 ten thousand Da; the viscosity is 675 to 1026 mPa.s.
7. The moisture mask as claimed in any one of claims 1 to 6, wherein the moisture mask auxiliary material comprises one or more of a preservative, a chelating agent, and a polyhydric alcohol.
8. The moisture mask as claimed in claim 7, wherein the auxiliary materials comprise 0.10-1.00wt% of preservative, 0.02-0.10wt% of chelating agent and 0.0-30.00wt% of polyhydric alcohol based on the total weight of the moisture mask.
9. The moisture mask pack according to any one of claims 7 or 8, wherein the preservative is a preservative acceptable in the field of skin care products, such as: one or more of caprylyl hydroximic acid/1, 2-hexanediol/1, 3-propanediol, phenoxyethanol, menthone, glyceryl caprylate/caprylyl hydroximic acid/1, 2-pentanediol and 1, 2-hexanediol; the chelating agent is acceptable in the field of skin care products, such as: one or more of disodium EDTA, sodium glucoheptonate, trisodium EDTA and tetrasodium EDTA; the polyol is a skin care acceptable polyol, such as: one or more of glycerol, butanediol, propylene glycol and dipropylene glycol.
10. The method for preparing the moisturizing mask pack according to any one of claims 1 to 9, wherein the hyaluronic acid extract of dendrobium nobile according to any one of claims 1 to 6 and the preservative, the polyol and the chelating agent according to any one of claims 7 to 9 are sequentially added and uniformly stirred.
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