CN112972334B

CN112972334B - Anti-inflammatory whitening essence milk containing hairyvein agrimony extract and preparation method thereof

Info

Publication number: CN112972334B
Application number: CN202110265973.8A
Authority: CN
Inventors: 肖锦婷; 游瑞云; 卢仲柱
Original assignee: Fuzhou Qiulong Xintian Agricultural Technology Co ltd
Current assignee: Fuzhou Qiulong Xintian Agricultural Technology Co ltd
Priority date: 2021-03-11
Filing date: 2021-03-11
Publication date: 2022-07-08
Anticipated expiration: 2041-03-11
Also published as: CN112972334A

Abstract

The invention discloses an anti-inflammatory whitening essence milk containing hairyvein agrimonia herb and bud extract, which comprises the following raw materials in percentage by mass: the functional component of the hairyvein agrimony extract is 10-25%, camellia oil is 1-3%, litsea cubeba kernel oil is 2-5%, peony seed oil is 2-5%, tremella polysaccharide is 2-5%, cetearyl glucoside is 2-5%, cetearyl alcohol is 3.5-5%, camellia oil modifier is 2-5%, sodium hyaluronate is 0.25-1.2%, peach gum hydrolysate is 2-5%, sodium acrylate/sodium acryloyldimethyl taurate copolymer is 1-1.5%, litsea cubeba essential oil is 0.05-0.5%, and deionized water is used for balancing; the anti-inflammatory whitening essence milk containing hairyvein agrimony prepared by the invention has good anti-inflammatory whitening effect on skin, is free of additives, safe and non-irritant, and has good anti-inflammatory whitening effect, simple preparation process and lower preparation cost compared with the existing anti-inflammatory whitening products.

Description

Anti-inflammatory whitening essence milk containing hairyvein agrimony extract and preparation method thereof

Technical Field

The invention belongs to the field of cosmetics, and particularly relates to anti-inflammatory whitening essence milk containing a hairyvein agrimonia herb extract and a preparation method of the essence milk.

Background

With the continuous improvement of living standard, people's pursuit of life is not only on the level of satiety. Under the condition of meeting basic living conditions, people pay more and more attention to skin care. The skin is exposed in the environment and is easily affected by various external irritants and allergens, so that the skin is subjected to oxidative stress and inflammatory reaction is induced; the inflamed skin can have symptoms of redness, swelling, heat, pain (itching) and the like on the surface, the skin permeability is increased, the transdermal water loss rate is increased, and the skin is dry; in the skin, dermatitis reduces the skin tolerance, microorganisms and chemical irritants/allergens easily enter the skin through the horny layer, the dermatitis is worsened, and simultaneously, various proteases in the skin are released to degrade collagen and elastin, so that the skin is in a loose and aging state.

The skin exhibits inflammatory phenomena, mainly because it is damaged by "chemical" factors. Thus, the presence of metal ions has a considerable role in skin health, some of which have anti-inflammatory, repair-promoting and antioxidant activity. At present, the most used metal element in skin care products is zinc, and 55 different zinc-containing materials are listed in international cosmetic ingredient dictionaries and manuals (raw material tables of cosmetics and personal care products); the U.S. food and drug administration approved a relatively broad range of uses for zinc-containing materials, indicating that zinc can be effective in treating a variety of skin conditions and can be prescribed over the counter. Materials containing zinc components are useful for treating various inflammatory skin conditions such as poison ivy dermatitis and diaper rash; at the damaged position of the skin, the skin is subjected to a process from inflammation to epidermis regeneration, granulation tissue growth, wound contraction and tissue remodeling, in the process, the zinc content around the wound is increased, which is the adjustment of the body for accelerating wound healing, and the aggregation of the zinc around the wound can accelerate the protein synthesis speed, so that the repair speed of the skin can be accelerated by externally supplying the zinc during the wound recovery period. For non-invasive skin lesions, it has also been shown that zinc metal can help the skin repair more quickly by anti-inflammatory effect. Besides zinc, the metal components applied to the anti-inflammatory skin care product also comprise copper, calcium, selenium and the like. However, the instability of metal ions causes that the metal ions in the skin care products containing metal ions on the market are difficult to be absorbed by the skin, thereby limiting the use of the metal ions in the cosmetic industry.

The agrimony is rich in wild resources, wide in distribution, contains various active ingredients, has wide pharmacological effects, is a Chinese herbal medicine, is bitter and astringent in taste, has mild nature, enters lung, liver and spleen channels, is commonly used for treating diseases such as tumor, Meniere syndrome, trichomonas vaginitis and the like, and has pharmacological effects of resisting tumor, stopping bleeding, resisting bacteria, killing insects and the like. The agrimony is rich in polyphenol, the polyphenol molecular structure contains a plurality of phenolic hydroxyl groups, and a large n-bond conjugated system and a strong coordinated oxygen atom are arranged in the molecule, so that the spatial configuration enables the agrimony to have stronger capability of complexing metal ions and is a good ligand of the metal ions; and the electron-withdrawing action of the metal ions can promote the H dissociation on the phenolic hydroxyl. In addition, the polyphenol not only has good oxidation resistance, but also has strong whitening capacity, and the most prominent oxidation resistance is as follows: the complexing ability of metal ions, the elimination of free radicals and active oxygen, the regeneration and anti-allergy repair effects on endogenous antioxidants are improved, the stabilizing habit of the metal ions is improved, the oxidation resistance of the metal ions is enhanced, and the skin transmittance can be improved.

Disclosure of Invention

In order to solve the problem of unstable metal ions in the anti-inflammatory skin care products in the prior art, the invention utilizes the hairyvein agrimony modified polyphenol extract and applies the polyphenol extract to the anti-inflammatory whitening essence milk, the hairyvein agrimony is taken as an excellent natural product extract, the ethanol extract of the hairyvein agrimony has the effects of whitening, diminishing inflammation and the like, has complexation on the metal ions, and can chelate Zn²⁺、Cu²⁺、Ca²⁺The metal ions are mixed with various traditional Chinese medicinal materials, so that the anti-inflammatory and whitening effects of the Chinese medicinal composition are improved. Compared with the existing product, the anti-inflammatory whitening essence milk prepared by the invention is natural and environment-friendly, does not contain raw materials which can stimulate the skin, and has high anti-inflammatory whitening speed.

The purpose of the invention is realized by the following technical scheme:

the invention discloses an anti-inflammatory whitening essence milk containing hairyvein agrimonia herb and bud extract, which comprises the following raw materials in percentage by mass: the functional component of the hairyvein agrimony extract is 10-25%, camellia oil is 1-3%, litsea cubeba kernel oil is 2-5%, peony seed oil is 2-5%, tremella polysaccharide is 2-5%, cetearyl glucoside is 2-5%, cetearyl alcohol is 3.5-5%, camellia oil modifier is 2-5%, sodium hyaluronate is 0.25-1.2%, peach gum hydrolysate is 2-5%, sodium acrylate/sodium acryloyldimethyl taurate copolymer is 1-1.5%, litsea cubeba essential oil is 0.05-0.5%, and deionized water is used for balancing.

Further, the effective components containing the hairyvein agrimony extract comprise the following raw materials in parts by weight:

further, the preparation method of the functional component containing the agrimony extract comprises the following steps:

(1) crushing the hairyvein agrimony by using a traditional Chinese medicine crusher, sieving the crushed hairyvein agrimony by using a sieve of 60 meshes to obtain hairyvein agrimony powder, adding 60 mass percent of ethanol solution, wherein the material-to-liquid ratio is 1-1.5 g: 25-30 mL, carrying out reflux extraction for multiple times at the temperature of 70-80 ℃ for 40-50 min each time, carrying out reduced pressure filtration, combining extracting solutions extracted for multiple times, carrying out rotary evaporation concentration, recovering ethanol, extracting for at least 2 times by using n-butyl alcohol, and volatilizing the n-butyl alcohol to obtain a hairyvein agrimony extracting solution;

(2) mixing honeysuckle, phellodendron and liquorice, crushing the mixture by using a traditional Chinese medicine crusher, sieving the mixture by using a 60-mesh sieve to obtain a mixture, adding the mixture into an ethanol solution with the mass fraction of 60%, adopting an ultrasonic-assisted extraction method, setting the extraction temperature to be 65-75 ℃, the power to be 130-150W, extracting for 25-30 min, taking the precipitate, repeating the step 1 time again, combining the extracting solutions, filtering under reduced pressure, carrying out rotary evaporation at the rotary evaporation temperature of 55-65 ℃ and the pressure of 0.9-0.95atm until the concentration is 0.5g/mL, and obtaining a mixed extracting solution A;

(3) mixing radix rehmanniae and Chinese ladybell herb into a traditional Chinese medicine grinder for grinding, sieving by a 40-mesh sieve to obtain a mixture, adding the mixture into an ethanol solution with the mass fraction of 40%, extracting for 30-35 min under the conditions that the microwave temperature is 50-60 ℃ and the power is 600-650W, taking the precipitate, and repeating the step for 1 time; filtering under reduced pressure, rotary evaporating and concentrating to concentration of 0.5g/mL to obtain mixed extractive solution B;

(4) mixing the herba et Gemma Agrimoniae extractive solution, mixed extractive solution A and mixed extractive solution B to obtain functional component containing herba et Gemma Agrimoniae extract.

Further, acrylamide is added into the hairyvein agrimonia herb and bud extracting solution in the step (1) for modification, and the specific modification steps are as follows: adding deionized water and acrylamide in a mass ratio of 9:1 into a reaction container, heating the mixed solution in a water bath at 50-75 ℃, adding hydrogen peroxide in an amount of 1% by mass of acrylamide into the reaction container as an initiator, adding 5-10% acetic acid to adjust the pH value to 3.5-4.0, reacting for 40min, adding hairyvein agrimony extracting solution, and reacting for 1min to obtain the modified hairyvein agrimony polyphenol extracting solution.

Further, the mass ratio of the mixture in the step (2) to the ethanol solution with the mass fraction of 60% is 1: 19-20.

Further, the mass ratio of the mixture in the step (3) to the ethanol solution with the mass fraction of 40% is 1: 20-25.

Further, the mass ratio of the hairyvein agrimonia herb and bud extract, the mixed extract A and the mixed extract B in the step (4) is 8-10: 7: 5.

Further, the preparation method of the camellia oil modified product comprises the following steps: weighing camellia oil, placing the camellia oil in a reaction kettle, adding diethanolamine in an amount of 1:3.3 of the camellia oil, adding KOH solution in an amount of 2.0% of the mass of the camellia oil, and carrying out mixing reaction at the reaction temperature of 80-90 ℃ for 3-4 h to obtain amidated modified camellia oil.

The invention also discloses a preparation method of the anti-inflammatory whitening essence milk containing the hairyvein agrimonia herb extract, which specifically comprises the following steps:

s1: mixing camellia oil, litsea cubeba oil, peony seed oil and camellia oil modified substances, heating to 85-95 ℃ while stirring to melt the mixture into an oil phase, heating cetearyl glucoside, cetearyl alcohol, sodium hyaluronate, peach gum hydrolysate and sodium acrylate/sodium acryloyldimethyl taurate copolymer to 85-95 ℃ while stirring to melt and swell into a water phase, mixing tremella polysaccharide, the oil phase and the water phase, heating to dissolve, and continuing to stir for 30-60 min to obtain emulsion C;

s2: cooling the emulsion C obtained in the step S1 to 50-55 ℃, adding the efficacy components of the hairyvein agrimony extract, and uniformly stirring to obtain a mixed solution D;

s3: cooling the mixture D obtained in the step S2 to 35-45 ℃, adding litsea cubeba essential oil, and uniformly stirring to obtain an ointment E;

s4: and cooling the paste E to obtain the anti-inflammatory whitening essence milk.

The invention has the beneficial effects that:

1. the invention provides an anti-inflammatory whitening essence milk containing hairyvein agrimony extract, which adopts unique Chinese herbal medicines of hairyvein agrimony, honeysuckle, phellodendron, radix rehmanniae recen, Chinese ladybell root and liquorice extract, has reasonable formula and good anti-inflammatory whitening effect, contains the efficacy components of the hairyvein agrimony extract, has good anti-inflammatory sterilization and whitening and repairing effects, has small difficulty in manufacturing process, simple extraction steps and low economic cost, is natural and environment-friendly compared with the existing anti-inflammatory whitening, does not contain raw materials which can stimulate the skin, and can also achieve good anti-inflammatory whitening effect;

the agrimony extract contains various compounds such as flavonoids, phenols, isocoumarins, pentacyclic triterpenes, organic acids and the like, has exact pharmacological action in the treatment fields of inflammation resistance, oxidation resistance and bacteria resistance, and the whole herb contains agrimophol A, B, C, D, E, F, G, quercetin, caffeic acid, gallic acid and the like, and modern pharmacology shows that the agrimony extract is an antioxidant with very strong biological property, has the effects of inflammation resistance and whitening, can complex metal ions and inhibit the generation of hydroxyl radicals; can effectively remove various oxygen radicals; can effectively activate the antioxidant enzyme of the organism or prevent the oxidation of the antioxidant enzyme when in trace concentration;

the honeysuckle flower is sweet and cold in nature, capable of clearing heat without hurting the stomach, and thoroughly capable of eliminating pathogenic factors, has the effects of clearing heat and removing toxicity, resisting inflammation, tonifying deficiency and treating wind, and has a strong inhibiting effect on various acne-causing bacteria such as staphylococcus aureus and the like; the phellodendron bark contains a large amount of flavone compounds, the concentration of which is in direct proportion to the oxidation resistance, and has unique curative effects in the aspects of antibiosis and antiphlogosis, blood sugar reduction, cancer resistance, immune system diseases and the like; the liquorice contains various chemical components, the main components comprise glycyrrhizic acid, liquiritin and the like, and the liquorice has the effects of clearing away heat and toxic materials, eliminating phlegm and stopping cough and the like, and can be used for harmonizing the medicines and eliminating the toxic and side effects of the medicines; the honeysuckle, the phellodendron and the liquorice are used together, so that the effects of clearing heat and drying dampness, purging fire and removing toxicity are more obvious;

the dried rehmannia root has the effects of clearing heat and cooling blood, promoting the production of body fluid and moistening dryness, contains chemical substances such as beta-sitosterol, mannitol, a small amount of stigmasterol, a trace amount of campesterol and the like, the extract of the dried rehmannia root has the effects of resisting inflammation, resisting allergy and the like, and the water extract has the effect of resisting fungi;

the camellia oil contains various unsaturated fatty acids, has good skin compatibility, is cool and hemostatic, and is used as an effective moisturizing and antioxidant component in cosmetics. The modified camellia oil prepared by amidation not only keeps the characteristics of mild camellia oil, no stimulation, good permeability, strong oxidation resistance and the like, but also has good surface activity, and compared with other nonionic surfactants, the modified camellia oil has no cloud point, good foamability, low toxicity, small stimulation to eyes and skin and better conditioning effect on the skin;

the litsea cubeba essential oil is fragrant and nontoxic, and is a natural preservative and additive. The litsea cubeba essential oil has remarkable bacteriostatic activity on listeria monocytogenes, fusarium oxysporum, escherichia coli, vibrio parahaemolyticus, lactobacillus plantarum, aflatoxin and the like, is compounded with other traditional preservatives to be used in a daily chemical product system, can greatly reduce the addition amount of the traditional preservatives, can remarkably reduce the toxicity of the preservative system while synergistically inhibiting and preserving bacteria, and is safe and non-irritant;

the tremella polysaccharide can keep the viscosity of the anti-whitening essence milk and can absorb heavy metal components remained on the surface layer of the skin.

2. The invention provides an anti-inflammatory whitening essence emulsion containing hairyvein agrimonia herb extract, which takes the efficacy component of the hairyvein agrimonia herb extract as the main raw material, and the hairyvein agrimonia herb extract is modified to obtain a modified hairyvein agrimonia herb polyphenol extract, wherein the modified hairyvein agrimonia herb polyphenol extract has a plurality of ortho-position hydroxyl groups, and can generate chelation and complexation with heavy metal ions to form a five-membered or six-membered chelate ring compound, so as to achieve the effect of removing the heavy metal ions, although the unmodified phenolic hydroxyl groups can also generate complexation with metals, the stability and the complexation easiness of the modified hairyvein agrimonia herb polyphenol extract are relatively strong, and the problems that the prior emulsion breaking phenomenon of oil-water separation of the emulsion is caused by the impurity of mineral substances in plant extract, the prepared cosmetic product is easy to deteriorate and the like in the prior art can be effectively solved.

3. According to the invention, the agrimony extract is modified by using acrylamide, metal ions can form complex precipitates with polyphenol, other substances cannot form complex precipitates, the polyphenol is rich in phenolic hydroxyl, and Zn can be better complexed by acrylamide graft copolymerization²⁺、Mg²⁺、Ca²⁺And the metal ions are used for improving the skin transmittance of the metal ions and enhancing the anti-inflammatory and whitening effects.

4. The invention adopts different extraction processes aiming at different Chinese herbal medicines, more effectively retains active ingredients in the Chinese herbal medicines and improves the utilization rate of the Chinese herbal medicines.

Detailed Description

In order to better understand the present invention, the following examples are further described, which are only used to explain the present invention and do not limit the present invention. Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art, and the raw materials used are commercially available products.

Example 1

An anti-inflammatory whitening essence milk containing hairyvein agrimony extract comprises the following raw materials in percentage by mass: contains 10 percent of efficacy components of hairyvein agrimony extract, 1 percent of camellia oil, 2 percent of litsea cubeba kernel oil, 2 percent of peony seed oil, 2 percent of tremella polysaccharide, 2 percent of cetearyl glucoside, 3.5 percent of cetearyl alcohol, 2 percent of camellia oil modifier, 0.25 percent of sodium hyaluronate, 2 percent of peach gum hydrolysate, 1 percent of sodium acrylate/sodium acryloyldimethyl taurate copolymer, 0.05 percent of litsea cubeba essential oil and 67.43 percent of deionized water.

The effective components containing the hairyvein agrimony extract comprise the following raw materials in parts by weight: 40 parts of hairyvein agrimony, 15 parts of honeysuckle, 10 parts of golden cypress, 10 parts of radix rehmanniae recen, 15 parts of Chinese ladiestresses root and 10 parts of liquorice.

The preparation method of the efficacy component containing the hairyvein agrimonia herb and bud extract comprises the following steps:

(1) pulverizing herba et Gemma Agrimoniae with a traditional Chinese medicine pulverizer, sieving with 60 mesh sieve to obtain herba et Gemma Agrimoniae powder, adding 60% ethanol solution at a material-liquid ratio of 1g:25mL, reflux-extracting at 70 deg.C for several times (40 min each time), filtering under reduced pressure, mixing extractive solutions, rotary evaporating for concentration, recovering ethanol, extracting with n-butanol for at least 2 times, and volatilizing n-butanol to obtain herba et Gemma Agrimoniae extractive solution;

(2) mixing honeysuckle, phellodendron and liquorice, crushing the mixture by using a traditional Chinese medicine crusher, sieving the crushed mixture by using a 60-mesh sieve to obtain a mixture, adding the mixture into an ethanol solution with the mass fraction of 60%, setting the mass ratio of the mixture to the ethanol solution with the mass fraction of 60% to be 1:19, adopting an ultrasonic-assisted extraction method, setting the extraction temperature to be 65 ℃ and the power to be 150W, extracting for 25min, taking precipitates, repeating the step for 1 time, combining extracting solutions, filtering under reduced pressure, carrying out rotary evaporation at the temperature of 55 ℃ and the pressure of 0.9atm, and carrying out rotary evaporation and concentration until the concentration is 0.5g/mL to obtain a mixed extracting solution A;

(3) mixing radix rehmanniae and radix seu herba Spiranthis Lanceae, pulverizing in a traditional Chinese medicine pulverizer, sieving with a 40 mesh sieve to obtain a mixture, adding the mixture into 40% ethanol solution at a mass ratio of 1:20, extracting for 32min at microwave temperature of 50 deg.C and power of 650W, and repeating the above steps for 1 time; filtering under reduced pressure, and rotary evaporating to concentrate to concentration of 0.5g/mL to obtain mixed extractive solution B;

(4) and mixing the hairyvein agrimony extract, the mixed extract A and the mixed extract B to obtain the functional component containing the hairyvein agrimony extract, wherein the mass ratio of the hairyvein agrimony extract to the mixed extract A to the mixed extract B is 8:7: 5.

The preparation method of the camellia oil modifier comprises the following steps: weighing camellia oil, placing the camellia oil in a reaction kettle, adding diethanolamine in a dosage ratio of 1:3.3 with the camellia oil, simultaneously adding KOH solution in an amount of 2.0% of the mass of the camellia oil, and carrying out mixing reaction at the reaction temperature of 80 ℃ for 4h to obtain amidated modified camellia oil.

Example 2

An anti-inflammatory whitening essence milk containing hairyvein agrimony extract comprises the following raw materials in percentage by mass: contains 15 percent of hairyvein agrimony extract functional component, 2 percent of camellia oil, 3 percent of litsea cubeba kernel oil, 3 percent of peony seed oil, 3 percent of tremella polysaccharide, 3 percent of cetearyl glucoside, 4.5 percent of cetearyl alcohol, 3.5 percent of camellia oil modifier, 0.5 percent of sodium hyaluronate, 4 percent of peach gum hydrolysate, 1 percent of sodium acrylate/sodium acryloyldimethyl taurate copolymer, 0.1 percent of litsea cubeba essential oil and 57.4 percent of deionized water.

The effective components containing the hairyvein agrimony extract comprise the following raw materials in parts by weight: 40 parts of hairyvein agrimony, 25 parts of honeysuckle, 20 parts of phellodendron, 20 parts of radix rehmanniae recen, 25 parts of Chinese ladybell root and 15 parts of liquorice.

(1) pulverizing herba et Gemma Agrimoniae with a traditional Chinese medicine pulverizer, sieving with 60 mesh sieve to obtain herba et Gemma Agrimoniae powder, adding 60% ethanol solution at a material-liquid ratio of 1.5g:30mL, reflux-extracting at 75 deg.C for multiple times, each time for 50min, filtering under reduced pressure, mixing extractive solutions, rotary evaporating and concentrating, recovering ethanol, extracting with n-butanol for at least 2 times, and volatilizing n-butanol to obtain herba et Gemma Agrimoniae extractive solution;

(2) mixing honeysuckle, phellodendron and liquorice, crushing by using a traditional Chinese medicine crusher, sieving by using a 60-mesh sieve to obtain a mixture, adding the mixture into an ethanol solution with the mass fraction of 60%, setting the mass ratio of the mixture to the ethanol solution with the mass fraction of 60% to be 1:20, adopting an ultrasonic-assisted extraction method, setting the extraction temperature to be 75 ℃, the power to be 130W, extracting for 30min, taking precipitates, repeating the step for 1 time, combining the extracting solutions, filtering under reduced pressure, carrying out rotary evaporation at the temperature of 65 ℃ and the pressure of 0.95atm, and carrying out rotary evaporation and concentration to the concentration of 0.5g/mL to obtain a mixed extracting solution A;

(3) mixing radix rehmanniae and radix seu herba Spiranthis Lanceae, pulverizing in a traditional Chinese medicine pulverizer, sieving with a 40 mesh sieve to obtain a mixture, adding the mixture into 40% ethanol solution at a mass ratio of 1:25, extracting for 30min at microwave temperature of 55 deg.C and power of 630W, and repeating the above steps for 1 time; filtering under reduced pressure, rotary evaporating and concentrating to concentration of 0.5g/mL to obtain mixed extractive solution B;

(4) mixing the hairyvein agrimony extract, the mixed extract A and the mixed extract B to obtain a functional component containing the hairyvein agrimony extract, wherein the mass ratio of the hairyvein agrimony extract to the mixed extract A to the mixed extract B is 9:7: 5.

The preparation method of the camellia oil modifier comprises the following steps: weighing camellia oil, placing the camellia oil in a reaction kettle, adding diethanolamine in a dosage ratio of 1:3.3 with the camellia oil, simultaneously adding KOH solution in an amount of 2.0% of the mass of the camellia oil, and carrying out mixing reaction at the reaction temperature of 90 ℃ for 3h to obtain amidated modified camellia oil.

Example 3

An anti-inflammatory whitening essence milk containing hairyvein agrimonia herb and bud extract comprises the following raw materials in percentage by mass: contains the effective components of hairyvein agrimony extract 25%, camellia oil 3%, litsea cubeba kernel oil 5%, peony seed oil 5%, tremella polysaccharide 5%, cetearyl glucoside 5%, cetearyl alcohol 5%, camellia oil modifier 5%, sodium hyaluronate 1.2%, peach gum hydrolysate 5%, sodium acrylate/sodium acryloyldimethyl taurate copolymer 1.5%, litsea cubeba essential oil 0.5% and deionized water 33.8%.

The effective components containing the hairyvein agrimony extract comprise the following raw materials in parts by weight: 45 parts of hairyvein agrimony, 20 parts of honeysuckle, 15 parts of phellodendron, 15 parts of radix rehmanniae recen, 20 parts of Chinese ladybell root and 12 parts of liquorice.

(1) pulverizing herba et Gemma Agrimoniae with a Chinese medicinal pulverizer, sieving with 60 mesh sieve to obtain herba et Gemma Agrimoniae powder, adding 60% ethanol solution at a ratio of 1.2g to 28mL, reflux-extracting at 80 deg.C for 45min each time, filtering under reduced pressure, mixing extractive solutions, rotary evaporating for concentrating, recovering ethanol, extracting with n-butanol for at least 2 times, and volatilizing n-butanol to obtain herba et Gemma Agrimoniae extractive solution;

(2) mixing honeysuckle, phellodendron and liquorice, crushing by using a traditional Chinese medicine crusher, sieving by using a 60-mesh sieve to obtain a mixture, adding the mixture into an ethanol solution with the mass fraction of 60%, setting the mass ratio of the mixture to the ethanol solution with the mass fraction of 60% to be 1:20, adopting an ultrasonic-assisted extraction method, setting the extraction temperature to be 70 ℃, the power to be 140W, extracting for 28min, taking precipitates, repeating the step 1 time, combining the extracting solutions, filtering under reduced pressure, carrying out rotary evaporation at the temperature of 60 ℃ and the pressure of 0.92atm, and carrying out rotary evaporation and concentration to the concentration of 0.5g/mL to obtain a mixed extracting solution A;

(3) mixing radix rehmanniae and radix seu herba Spiranthis Lanceae, pulverizing in a traditional Chinese medicine pulverizer, sieving with a 40 mesh sieve to obtain a mixture, adding the mixture into 40% ethanol solution at a mass ratio of 1:22, extracting for 35min at microwave temperature of 60 deg.C and power of 600W, and repeating the above steps for 1 time; filtering under reduced pressure, rotary evaporating and concentrating to concentration of 0.5g/mL to obtain mixed extractive solution B;

(4) mixing the hairyvein agrimony extract, the mixed extract A and the mixed extract B to obtain a functional component containing the hairyvein agrimony extract, wherein the mass ratio of the hairyvein agrimony extract to the mixed extract A to the mixed extract B is 10:7: 5.

The preparation method of the camellia oil modifier comprises the following steps: weighing camellia oil, placing the camellia oil in a reaction kettle, adding diethanolamine in a dosage ratio of 1:3.3 with the camellia oil, simultaneously adding KOH solution in an amount of 2.0% of the mass of the camellia oil, and carrying out mixing reaction at a reaction temperature of 85 ℃ for 3h to obtain amidated modified camellia oil.

Example 4

A preparation method of an anti-inflammatory whitening essence milk containing hairyvein agrimonia herb and bud extract comprises the following steps:

s1: heating modified litsea cubeba oil, peony seed oil and camellia oil to 85-95 ℃ while stirring, heating cetearyl glucoside, cetearyl alcohol, sodium hyaluronate, peach gum hydrolysate and sodium acrylate/sodium acryloyldimethyl taurate copolymer to 85-95 ℃ while stirring, adding tremella polysaccharide, heating and dissolving the oil phase and the water phase respectively, and continuing stirring for 30-60 min to obtain emulsion C;

s2: cooling the emulsion C obtained in the step S1 to 50-55 ℃, adding the efficacy components of the hairyvein agrimony, and uniformly stirring to obtain a mixed solution D;

s3: cooling the mixture D obtained in the step S2 to 35-45 ℃, adding litsea cubeba essential oil, and uniformly stirring to obtain paste E;

s4: and (5) cooling the paste E obtained in the step (S3) to obtain the anti-inflammatory whitening essence milk.

Comparative example 1

The difference between the comparative example 1 and the example 1 is that the extract of the effective component does not contain the extract of hairyvein agrimony; the procedure and the starting materials and preparation were as described in example 1 above.

Testing and analysis

1. Determination of complexing ability of agrimony polyphenol to metal ions

Test subjects: the anti-inflammatory and whitening essence milk prepared according to the raw materials and the method of example 1.

(1) Determination of the proton addition constant

The test method comprises the following steps: taking 0.05mol/L modified herba et Gemma Agrimoniae polyphenol solution, maintaining the ionic strength (1) of the solution at 0.1mol/L with NaCl solution, fixing the volume at 100mL, transferring to a triangular flask, placing in a constant temperature water bath, titrating with NaOH standard solution under the protection of nitrogen, and adopting the method proposed by Bjerrum

The semi-integer method is used for obtaining the proton addition constant (lgKnH) of polyphenol, and the main formula of the protonation constant is as follows:

α＝V(NaOH)×C(NaOH)/C₀(HnL)×V₀(HnL)

in the formula:

the average number of adducted protons of the ligand L; n- - -the number of protons that the ligand HnL can release; c_L-total concentration of ligands, mol/L; degree of neutralization of α - - -HnL; [ H ]⁺]，[OH^A]---H⁺And OH^AConcentration of (2), mol/L.

Calculating alpha and HnL by the computer program; from pH value to pH value

Plotting to obtain a curve of the generating function of the ligand, in

Obtaining the proton constants of each stage of the ligand for half-integer points, obtaining the accumulative proton constants of each stage, calculating the negative logarithm pK of the dissociation constants of water at 15, 20, 25 and 30 ℃ required for the proton constants of different temperatures_W；

In ion adsorption, the coordination constant of the ligand is closely related to the proton addition constant, and the proton addition constant of the modified agrimonia polyphenol at each temperature is shown in table 1;

TABLE 1 comparison of the proton addition constants (I ═ 0.1mol/LNaCl)

As can be seen from Table 1, the proton addition constant values of the modified Agrimonia pilosa polyphenol in the experimental temperature range of the present study are all decreased with the increase of the temperature, which conforms to the law that the ionization balance of weak electrolyte in aqueous solution changes with the temperature. Ionization of a weak electrolyte is generally an endothermic process. The increased temperature is favorable for the ionization of weak electrolyte, i.e. for adding protons; the research result shows that the complexation reaction of polyphenol is divided into two steps, the phenolic hydroxyl group is firstly dissociated into oxygen anion and then coordinated with metal ion, therefore, the fact that the proton constant value of polyphenol is reduced along with the increase of temperature means that the dissociation constant is increased along with the increase of temperature, and the complexation reaction of polyphenol and metal ion is facilitated.

(2) Determination of the stability constant

Taking 0.05mol/L modified agrimonia pilosa polyphenol solution and Zn²⁺、Mg²⁺、Ca²⁺2.5mL of each solution, using NaCl solution to maintain the ionic strength of the solution at 0.10mol/L and the constant volume at 100mL, transferring to a triangular flask, placing in a constant-temperature water bath, titrating with NaOH standard solution under the protection of nitrogen, and obtaining the stability constant logarithm value lgK of the complex generated by the modified agrimony polyphenol and the metal ions and the calculation formula of the stability constant of the complex:

[L]＝((n-α)×CL-[H⁺]+[OH^a])/(β1H×[H+]+2×β2H×[H+]2+…+n×βnH×[H+]n)

In the formula:

the average coordination number of the ligand L complexed with the metal; cm- -total concentration of metal ions, mol/L

With [ L ]]Negative logarithm of pL pair

Making a generating function curve graph, wherein the pL value corresponding to the point with the element of a half integer is the logarithm value lgK of the complex stability constant, and the logarithm values of the stability constants of the modified agrimony polyphenol and various metal ions are shown in table 2;

TABLE 2 Metal ion complexation stability constant of modified Agrimonia pilosa Polyphenol (lgK) (I ═ 0.1mol/LNaCl)

As can be seen from Table 2, Zn is modified by agrimony polyphenol at the same temperature²⁺、Mg²⁺、Ca²⁺The order of the complex size of (A) is Zn²⁺＞Mg²⁺＞Ca²⁺Modified agrimony polyphenol pair Zn²⁺The adsorbability of (A) is most preferable.

2. Test for anti-inflammatory Effect

(1) The cell culture method comprises the following steps:

the cells were cultured in a constant temperature incubator at 30 ℃ and 5% CO2, NIH3T3 and HaCaT cell lines were cultured in DMEM medium containing 10% fetal bovine serum, RAW264.7 cell lines were cultured in 1640s medium containing 10% fetal bovine serum, all cell lines were changed daily, passaged every other day, and inflammatory factor IL-6 was detected by real-time quantitative ELISA.

(2) ELISA detection

Firstly, after the cells are treated, sucking cell culture fluid, centrifuging at 13500rpm for 10min, and taking supernatant; storing at-20 deg.C;

secondly, adding 100 microliter of cell culture samples, standard substances and contrast into the micro-pores, wherein each sample is repeated for 3 times; sealing and incubating for 2h at room temperature;

finally, LPS (100mg/mL) was added to stimulate the macrophages to produce inflammation, and the cells were incubated for 24h while incubatingThe control group without LPS was set, and 2.5mLZn was added to macrophages after stimulation with LPS²⁺The solution, containing modified Agrimonia pilosa polyphenol extract solution of compounds 1-4(7.5, 15, 30 mug/mL) with different concentrations, is put into a cell incubator to be continuously cultured for 24h, meanwhile, an LPS group without 1-4 modified Agrimonia pilosa polyphenol extract solution is set as a negative control, after experimental operation is carried out according to the specification of an ELISA kit, each OD value is measured at 450nm, and the test results are shown in Table 3;

TABLE 3 Tetraselaginella arborvitae biological ELISA KIT Mouse IL-6 test results

Test specimen	OD value 1	OD value 2	Concentration of inflammatory factor
				Experimental group	0.119	0.112	125
Negative control group	2.599	2.600	250
				Control group	0.334	0.334	1000

The higher the concentration of the anti-inflammatory factor is, the worse the anti-inflammatory effect is, which indicates that the modified agrimonia polyphenol extracting solution is complexed with Zn²⁺1-4 has obvious inhibition effect on the release of macrophage IL-6 in inflammatory response induced by LPS, and reflects excellent anti-inflammatory property.

3. Test of antioxidant Effect

(1) Taking 1mg of DPPH in a beaker, and then fixing the volume to a 100ml volumetric flask to prepare 0.001mg/ml DPPH solution; taking 50uL of the modified agrimonia pilosa polyphenol extracting solution to fix the volume in a 50mL volumetric flask.

A₁Value measurement: adding DPPH solution 2ml into test tube, adding sample solution 0.7ml, adding sample solution solvent (1.2-0 ml), mixing, standing for 30min, and measuring A at wavelength of 517nm₁The value is obtained. The modified agrimony polyphenol sample solution has the dosage gradient of 0.7ml, 0.9ml, 1.1ml, 1.3ml, 1.5ml, 1.7ml and 1.9ml, and the test results are shown in table 4;

TABLE 4 modified Agrimonia pilosa Polyphenol A₁Result of value measurement

Sample liquid/ml	Sample solution solvent/ml	DPPH solution/ml	Total volume/ml
				0.7	1.2	2	3.9
0.9	1.0	2	3.9
				1.1	0.8	2	3.9
1.3	0.6	2	3.9
				1.5	0.4	2	3.9
1.7	0.2	2	3.9
				1.9	0	2	3.9

A₂Value measurement: adding 2ml of ethanol into a test tube, adding 0.7ml of sample solution, adding 1.2-0 ml of sample solution solvent, mixing, standing for 30min, and measuring A at wavelength of 517nm₂Value (solution configuration and measurement method same as A)₁Replacing the DPPH solution with an ethanol solution to eliminate the influence of color change of the sample solution along with concentration on absorbance when the values are the same);

A₃value measurement: adding 2ml of DPPH solution into a test tube, adding 1.2ml of sample solution solvent, mixing, and standingAfter 30min, A was measured at a wavelength of 517nm₃A value;

(2) and (4) calculating a result: oxygen radical clearance calculation formula:

(3) drawing a standard curve of sample concentration-clearance

Drawing a sample concentration-clearance curve according to the measurement result, fitting a linear regression equation, and calculating a median clearance (EC50) according to the equation, wherein the results are shown in Table 5;

TABLE 5 modified Agrimonia pilosa Polyphenol DPPH clearance results

Sample volume (ml)	Sample quality (ug)	Concentration (ug/ml)	A1	A2	A3	Elimination rate/%)
							0.7	0.5420	0.1389	0.033	-0.001	0.041	17.07
0.9	0.6960	0.1787	0.030	0	0.041	26.82
							1.1	0.8515	0.2184	0.025	0	0.041	39.02
1.3	1.0067	0.2581	0.021	-0.001	0.041	46.34
							1.5	1.1616	0.2978	0.017	0	0.041	58.53
1.7	1.3165	0.3375	0.014	0.001	0.041	68.29
							1.9	1.4713	0.3772	0.010	0	0.041	75.60

The experimental result shows that the modified agrimonia pilosa polyphenol extracting solution has good oxidation resistance.

The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by the present specification, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.

Claims

1. An anti-inflammatory whitening essence milk containing hairyvein agrimonia herb extract is characterized in that: the material comprises the following raw materials in percentage by mass: the functional component of the hairyvein agrimony extract is 10-25%, camellia oil is 1-3%, litsea cubeba kernel oil is 2-5%, peony seed oil is 2-5%, tremella polysaccharide is 2-5%, cetearyl glucoside is 2-5%, cetearyl alcohol is 3.5-5%, camellia oil modifier is 2-5%, sodium hyaluronate is 0.25-1.2%, peach gum hydrolysate is 2-5%, sodium acrylate/sodium acryloyldimethyl taurate copolymer is 1-1.5%, litsea cubeba essential oil is 0.05-0.5%, and deionized water is used for balancing;

the preparation method of the functional component containing the agrimony extract comprises the following steps:

(2) mixing honeysuckle, phellodendron and liquorice, crushing the mixture by using a traditional Chinese medicine crusher, sieving the crushed mixture by using a 60-mesh sieve to obtain a mixture, adding the mixture into an ethanol solution with the mass fraction of 60%, setting the extraction temperature to be 65-75 ℃ by using an ultrasonic-assisted extraction method, extracting the mixture for 25-30 min at the power of 130-150W, taking precipitate, repeating the step 1 again, combining extracting solutions, filtering the mixture under reduced pressure, performing rotary evaporation at the temperature of 55-65 ℃ under the pressure of 0.9-0.95atm until the concentration is 0.5g/mL, and obtaining a mixed extracting solution A;

(3) mixing radix rehmanniae and Chinese ladybell herb into a traditional Chinese medicine grinder for grinding, sieving by a 40-mesh sieve to obtain a mixture, adding the mixture into an ethanol solution with the mass fraction of 40%, extracting for 30-35 min under the conditions that the microwave temperature is 50-60 ℃ and the power is 600-650W, taking the precipitate, and repeating the step for 1 time; filtering under reduced pressure, and rotary evaporating to concentrate to concentration of 0.5g/mL to obtain mixed extractive solution B;

(4) mixing the herba et Gemma Agrimoniae extractive solution, mixed extractive solution A and mixed extractive solution B to obtain functional component containing herba et Gemma Agrimoniae extract;

wherein, the agrimony extract in the step (1) is modified by adding acrylamide, and the specific modification steps are as follows: adding deionized water and acrylamide in a mass ratio of 9:1 into a reaction container, heating the mixed solution in a water bath at 50-75 ℃, adding hydrogen peroxide in an amount of 1% by mass of acrylamide into the reaction container as an initiator, adding 5-10% acetic acid to adjust the pH value to 3.5-4.0, reacting for 40min, adding hairyvein agrimony extracting solution, and reacting for 1min to obtain the modified hairyvein agrimony polyphenol extracting solution.

2. The anti-inflammatory whitening essence milk containing agrimonia pilosa extract according to claim 1, which is characterized in that: the efficacy components containing the hairyvein agrimony extract comprise the following raw materials in parts by weight:

3. the anti-inflammatory whitening essence milk containing agrimonia pilosa extract according to claim 1, which is characterized in that: the mass ratio of the mixture in the step (2) to the ethanol solution with the mass fraction of 60% is 1: 19-20.

4. The anti-inflammatory whitening essence milk containing agrimonia pilosa extract according to claim 1, which is characterized in that: the mass ratio of the mixture in the step (3) to the ethanol solution with the mass fraction of 40% is 1: 20-25.

5. The anti-inflammatory whitening essence milk containing agrimonia pilosa extract according to claim 1, which is characterized in that: the mass ratio of the hairyvein agrimonia herb and bud extract, the mixed extract A and the mixed extract B in the step (4) is 8-10: 7: 5.

6. The anti-inflammatory whitening essence milk containing agrimonia pilosa extract according to claim 1, which is characterized in that: the preparation method of the camellia oil modifier comprises the following steps: weighing camellia oil, placing the camellia oil in a reaction kettle, adding diethanolamine in a dosage ratio of 1:3.3 with the camellia oil, simultaneously adding KOH solution in an amount of 2.0% of the mass of the camellia oil, and carrying out mixing reaction at the reaction temperature of 80-90 ℃ for 3-4 h to obtain amidated modified camellia oil.

7. The preparation method of the anti-inflammatory and whitening essence milk containing agrimony extract as claimed in claim 1, which comprises the following steps: