Blood-enriching motherwort plant extract and skin care application thereof

Abstract

The invention discloses a blood-enriching motherwort plant extract and a skin care application thereof. The blood-enriching motherwort plant extract is prepared by adding water into angelica sinensis, astragalus membranaceus and motherwort and carrying out secondary heating reflux extraction and alcohol precipitation purification, active and effective components such as leonurine, calycosin-7-glucoside, ferulic acid and arteolide can be detected, and the blood-enriching motherwort plant extract is high in extraction rate, high and stable in component content and suitable for industrial production. The obtained blood-enriching motherwort plant extract is easy to dissolve in water, can be well and uniformly mixed with a collagen extracting solution, and is high in stability, simple in preparation process and more suitable for industrial mass production. The blood-enriching motherwort plant extract is compounded with a collagen extracting solution to prepare a mask, and compared with a common mask, the mask has moisturizing and repairing effects, remarkably improves the skin cuticle moisture content of a user, remarkably reduces the TEWL value and the TEWL / Corn value of skin transepidermal moisture loss of the user, effectively inhibits tyrosinase activity and has whitening and freckle removing effects.

Description

Technical Field

[0001] The invention relates to the technical field of plant processing, and in particular to a plant extract of a blood-replenishing and motherwort prescription and its skin care application. Background Art

[0002] Medicinal plants contain a large number of beneficial active ingredients. Angelica, Astragalus and Leonurus japonicus are all medicinal plants. The prescription of nourishing blood and benefiting motherwort prepared with donkey-hide gelatin and tangerine peel has a significant improvement effect on postpartum anemia. Angelica has the effects of nourishing blood and activating blood circulation, regulating menstruation and relieving pain, and moistening the intestines and relieving constipation. It contains ingredients such as ligustilide, angelica ketone and ferulic acid. Astragalus has the effects of strengthening the spleen and replenishing the middle, raising yang and lifting the sunken, benefiting the body and strengthening the exterior, diuresis, and toxin-removing and muscle-building. It contains ingredients such as calycosin, astragaloside IV and astragalus polysaccharide. Leonurus japonicus has the effects of activating blood circulation and regulating menstruation, diuresis and swelling, and contains leonurine, stachydrine, diterpenoids and the like. The extraction process of medicinal materials has a vital impact on the efficacy of the medicine. The exploration of the extraction process of the prescription of nourishing blood and benefiting motherwort is one of the important means to improve its quality.

[0003] In addition, the application of active ingredients from medicinal plants in skin care products has also attracted more and more attention. As people pay more attention to natural, green, healthy and safe skin care products, the development of new plant-derived active ingredients has become one of the hot topics in skin care product research and development. Skin care products containing plant-derived active ingredients have the advantages of good efficacy and few side effects, and have more advantages than synthetic skin care products.

[0004] In the prior art, patent application CN1282572A discloses a series of cosmetics for treating facial chloasma, wherein the cosmetics of claims 5 to 7 are made of umbilical plaques made from more than a dozen Chinese medicinal plants including Leonurus japonicus, and used in combination with external freckle essence, freckle cream, freckle superconducting liquid, washable facial mask, and freckle cream, claiming to have the effects of treating facial chloasma, removing freckles, whitening, and nourishing the skin; wherein the umbilical plaque is used to regulate the body as a whole to improve the efficacy. However, the technical product is complex and cumbersome to use; the Chinese medicinal ingredients are complex, the preparation method is rough, and it is difficult to predict the effect of the use of the umbilical plaque. Moreover, the extraction process of Chinese medicinal plants is crucial to the water solubility, stability, and active ingredients of the product, affecting the quality and efficacy of skin care products, which limits the efficacy of plant-derived active ingredients in skin care and is difficult to promote to the public. Summary of the invention

[0005] The purpose of the present invention is to overcome the above-mentioned deficiencies of the prior art and provide a plant extract of Buxue Yimu Fang and its skin care application.

[0006] The first object of the present invention is to provide a method for preparing the plant extract of Buxue Yimu Fang.

[0007] The second object of the present invention is to provide the plant extract of Buxue Yimu Fang prepared by the method.

[0008] The third object of the present invention is to provide the use of the plant extract of the Buxue Yimu Recipe in preparing skin care products.

[0009] The fourth object of the present invention is to provide a skin care product.

[0010] In order to achieve the above object, the present invention is implemented by the following scheme:

[0011] A method for preparing a plant extract of Buxue Yimu Fang comprises the following steps:

[0012] S1: Take three medicinal materials, namely, Angelica sinensis, Astragalus membranaceus and Leonurus japonicus, soak them in water 8 to 10 times the weight of the medicinal materials, heat and reflux for extraction for 1.5 to 2 hours, filter and collect the filtrate;

[0013] S2: Add 6 to 8 times the weight of the medicinal material again, heat and reflux to extract for 1h to 1.5h, filter to obtain a filtrate;

[0014] S3: combining the filtrates of step S1 and S2 to obtain a combined filtrate; subjecting the combined filtrate to alcohol precipitation purification, solid-liquid separation, and collecting the purified filtrate to obtain the plant extract of Buxue Yimu Fang.

[0015] The obtained compound solution sample obtained after compounding the obtained plant extract of the blood-enriching and motherwort prescription with the collagen extract was easily soluble in water without precipitation, and the process was still stable after the amplified extraction. In the comparative example, angelica was extracted with alcohol alone, astragalus and motherwort were combined with water extraction, and then the obtained plant extract of the blood-enriching and motherwort prescription was mixed to produce a precipitate. The compound solution sample obtained after compounding the plant extract of the blood-enriching and motherwort prescription with the collagen extract in the comparative example was not easily soluble in water, and the process was unstable.

[0016] At the same time, the composite solution sample prepared by the present invention contains active ingredients such as leonurine, calycosin isoflavone glucoside, ferulic acid and artemisinin, and has a high extraction rate and high ingredient content.

[0017] In addition, after the composite solution sample prepared by the present invention is prepared into a facial mask, it has significant moisturizing and repairing effects, can significantly increase the moisture content of the user's skin stratum corneum, and significantly reduce the user's skin transepidermal water loss TEWL value and TEWL / Corn value. It effectively inhibits tyrosinase activity and has whitening and freckle removal effects. The above effects are better than those of the comparative example, indicating that the preparation method of the plant extract of the blood-enriching and mother-benefiting prescription of the present invention is more suitable for large-scale industrial production, and has significant effects in moisturizing and repairing and whitening and freckle removal.

[0018] Preferably, in step S1, water 8 times the weight of the sample is added for immersion.

[0019] Preferably, in step S1, the extraction is carried out under heating reflux for 2 h, and in step S2, the extraction is carried out under heating reflux for 1 h.

[0020] The heating reflux temperature is 70-90°C.

[0021] Furthermore, the immersion time is 30 to 60 minutes.

[0022] Furthermore, the immersion time is 30 minutes.

[0023] Preferably, in step S2, water in an amount of 6 times the weight of the medicinal material is added and heated under reflux for extraction.

[0024] Preferably, in step S3, during the alcohol precipitation purification, ethanol is added to the combined filtrate to an ethanol concentration of 75%.

[0025] Preferably, in step S3, the purified filtrate is concentrated by vacuum rotation to a weight equal to that of the three medicinal materials in step S1, so as to obtain the plant extract of Buxue Yimu Recipe, the density of which is 1.10-1.20 g / cm 3 .

[0026] Furthermore, the combined filtrate of step S3 is firstly concentrated by vacuum rotation to obtain an extract, and then purified by alcohol precipitation.

[0027] Furthermore, the vacuum rotation temperature may be 50-70°C.

[0028] Furthermore, the vacuum rotation temperature is 50°C.

[0029] In addition, the weight ratio of Angelica sinensis, Astragalus membranaceus and Leonurus japonicus can be 1.8-2.2:1.8-2.2:2.8-3.2.

[0030] Furthermore, the weight ratio of Angelica sinensis, Astragalus membranaceus and Leonurus japonicus is 2:2:3.

[0031] The invention also provides a plant extract of the Buxue Yimu prescription prepared by the method.

[0032] The present invention also requests to protect the application of the plant extract of the Buxue Yimu Recipe in preparing skin care products.

[0033] The invention provides a skin care product, which contains the plant extract of the blood-enriching and motherwort prescription.

[0034] Furthermore, the skin care product also contains collagen extract.

[0035] The collagen extract is prepared by a conventional collagen preparation method and can be purchased on the market.

[0036] Furthermore, the collagen extract is obtained by extracting and concentrating animal skin through conventional alcohol, and the animal skin can be conventional animal skin for preparing collagen extract, such as pig skin and donkey skin.

[0037] Among them, the plant extract of the Buxue Yimu recipe is compounded with the collagen extract to become the Buxue Yimu collagen plant extract, which is used as the Buxue Yimu recipe skin conditioner.

[0038] In the skin care product, the weight ratio of the Chinese angelica, astragalus and motherwort herbs used to prepare the plant extract of the blood-enriching and motherwort prescription to the collagen extract can be 25.8-26.2: 25.8-26.2: 38.8-39.2: 7.8-8.2.

[0039] Furthermore, in the blood-enriching and motherwort collagen plant extract, the weight ratio of angelica sinensis, astragalus and motherwort herbs used to prepare the blood-enriching and motherwort prescription plant extract to the collagen extract is 26:26:39:8.

[0040] Furthermore, the skin care product contains water, moisturizer, thickener, chelating agent, blood-boosting and mother-benefiting skin conditioning agent, other skin conditioning agents and pH regulator.

[0041] The moisturizing agent contains one or more of glycerin, xylitol compound moisturizing agent, inositol, betaine, erythritol, sodium hyaluronate, 4D hyaluronic acid, jojoba wax PEG-120 ester, glyceryl acrylate / acrylic acid copolymer compound moisturizing agent, methyl glucitol polyether-20, diethoxyethyl succinate, 1,3-butylene glycol, ethylhexylglycerol, 1,2-hexanediol and hydroxyethyl urea;

[0042] The xylitol compound moisturizer contains one or more of xylitol glucoside, dehydrated xylitol and xylitol; the glycerol acrylate / acrylic acid copolymer compound moisturizer contains glycerol acrylate / acrylic acid copolymer and one or more of glycerol, water and 1,2-hexanediol;

[0043] The thickener contains one or more of acrylic acid (ester) / C10-30 alkyl acrylate cross-linked polymer, polyacrylamide and hydroxyethyl cellulose compound thickener; the hydroxyethyl cellulose compound thickener contains hydroxyethyl cellulose and further contains one or more of disodium hydrogen phosphate, sodium dihydrogen phosphate and polysorbate-60;

[0044] The other skin conditioning agent contains one or more of kava root extract, peony root extract and centella asiatica extract;

[0045] The chelating agent contains caprylhydroxamic acid;

[0046] The pH adjuster contains L-arginine.

[0047] Furthermore, the weight ratio of moisturizer, thickener, chelating agent, Buxue Yimu Fang skin conditioning agent, other skin conditioning agents, pH regulator and water in the skin care product is 243.78-278.22: 1.5-2.1: 0.4-0.6: 1-8: 5-8: 0.8-1.2: 701.88-747.52.

[0048] Furthermore, the weight ratio of the moisturizer, thickener, chelating agent, Buxue Yimu Fang skin conditioning agent, other skin conditioning agents, pH regulator and water in the skin care product is 261:1.8:0.5:5:6.5:1:724.2.

[0049] Among them, the weight ratio of glycerol, xylitol composite moisturizer, inositol, betaine, erythritol, sodium hyaluronate, 4D hyaluronic acid, jojoba wax PEG-120 esters, glyceryl acrylate / acrylic acid copolymer composite moisturizer, methyl glucitol polyether-20, diethoxyethyl succinate, 1,3-butylene glycol, ethylhexylglycerol, 1,2-hexanediol and hydroxyethyl urea in the moisturizer is 58-62:4-6:19-21:19-21:28-32:0.3-0.5:0.08-0.12:4-6:9-11:48-52:14-16:28-32:0.4-0.6:4-6:8-12.

[0050] The weight ratio of xylitol glucoside, dehydrated xylitol and xylitol in the xylitol composite moisturizer is 2.5:1.75:0.75.

[0051] The weight ratio of glycerin, water, glycerin acrylate / acrylic acid copolymer and 1,2-hexanediol in the glycerin acrylate / acrylic acid copolymer composite moisturizer is 6.25:3.6:0.1:0.05.

[0052] Furthermore, the weight ratio of glycerol, xylitol composite moisturizer, inositol, betaine, erythritol, sodium hyaluronate, 4D hyaluronic acid, jojoba wax PEG-120 esters, glyceryl acrylate / acrylic acid copolymer composite moisturizer, methyl glucitol polyether-20, diethoxyethyl succinate, 1,3-butylene glycol, ethylhexylglycerol, 1,2-hexanediol and hydroxyethyl urea in the moisturizer is 60:5:20:20:30:0.4:0.1:5:10:50:15:30:0.5:5:10.

[0053] The weight ratio of the composite thickener of acrylic acid (ester) / C10-30 alkyl acrylate cross-linked polymer, polyacrylamide and hydroxyethyl cellulose in the thickener is 0.6-0.8:0.1-0.3:0.8-1.

[0054] Furthermore, the weight ratio of the composite thickener of acrylic acid (ester) / C10-30 alkyl acrylate cross-linked polymer, polyacrylamide and hydroxyethyl cellulose in the thickener is 0.7:0.2:0.9.

[0055] The weight ratio of hydroxyethyl cellulose, disodium hydrogen phosphate, sodium dihydrogen phosphate and polysorbate-60 in the hydroxyethyl cellulose composite thickener is 89.01:0.45:0.09:0.45.

[0056] The weight ratio of the kava root extract, the peony root extract and the Centella asiatica extract in the other skin conditioners is 1.3-1.8:2.3-2.8:2.3-2.8.

[0057] Furthermore, the weight ratio of the Kava Piper melongena root extract, the Paeonia lactiflora root extract and the Centella asiatica extract in the other skin conditioner is 1.5:2.5:2.5.

[0058] Furthermore, the skin care product is a facial mask liquid, and the specific preparation method is as follows:

[0059] S1: Mix the water, glycerin as a moisturizer, xylitol compound moisturizer, inositol, betaine, erythritol, acrylic acid (ester) / C10-30 alkyl acrylate cross-linked polymer, sodium hyaluronate, 4D hyaluronic acid, polyacrylamide, hydroxyethyl cellulose compound thickener, jojoba wax PEG-120 esters, glyceryl acrylate / acrylic acid copolymer compound moisturizer, methyl glucitol polyether-20 and diethoxyethyl succinate, stir and heat to 80-90°C, stop heating, keep warm and continue stirring, homogenize for 5-8 minutes to ensure that the materials are evenly dispersed, stop homogenizing, and continue stirring. After the materials are evenly dispersed and dissolved completely, cool down to 45°C while stirring to obtain phase A dissolved material.

[0060] S2: Mix 1,3-butanediol, ethylhexylglycerol, caprylhydroxamic acid and 1,2-hexanediol, heat in a water bath to 60-65° C., and stir until dissolved into a transparent liquid to obtain a phase B dissolved material; add the phase B dissolved material to the phase A dissolved material, stir until uniform, and obtain a mixed dissolved material of phases A and B.

[0061] S3: Mix the Buxue Yimu Fang skin conditioning agent and other skin conditioning agents with the mixed dissolved materials of phases A and B, homogenize and stir until the materials are uniform, and then cool to 40° C. to obtain the mixed dissolved materials of phases A, B and C.

[0062] S4: dissolving arginine with water to obtain a phase D material solution, then adding the phase D material solution to the mixed dissolved materials of phases A, B and C, stirring until uniform, adjusting the pH value to 5.5-6.5, and obtaining a mixed dissolved material of phases A, B, C and D.

[0063] S5: Mix hydroxyethyl urea, A, B, C and D to dissolve the materials evenly, adjust the temperature to 38°C, and separate the solid and liquid to obtain the mask liquid.

[0064] The above-mentioned facial mask liquid can be processed into a sheet-shaped facial mask by conventional methods for use.

[0065] Compared with the prior art, the present invention has the following beneficial effects:

[0066] The present invention adds water to angelica, astragalus and motherwort for secondary heating and reflux extraction, and prepares the blood-enriching motherwort plant extract after alcohol precipitation and purification. The blood-enriching motherwort plant extract can detect active and effective ingredients such as leonurine, calycosin isoflavone glucoside, ferulic acid and artemisinin, and has high extraction rate, high component content and stability. The obtained blood-enriching motherwort plant extract is easily soluble in water, can be well mixed with collagen extract, has strong stability, simple configuration process, and is more suitable for industrial large-scale production. The blood-enriching motherwort plant extract is compounded with collagen extract and then prepared into a facial mask. Compared with an ordinary facial mask, it has significant moisturizing and repairing effects, can significantly improve the moisture content of the user's skin stratum corneum, and significantly reduce the user's skin transepidermal water loss TEWL value and TEWL / Corn value. It effectively inhibits tyrosinase activity and has whitening and freckle removal effects. BRIEF DESCRIPTION OF THE DRAWINGS

[0067] Figure 1 This is the liquid chromatogram of the pilot process.

[0068] Figure 2 This is the liquid chromatogram of the compound solution of the small-scale scale-up process.

[0069] Figure 3 This is the liquid chromatogram of the pilot process compound solution.

[0070] Figure 4 The moisture content of the stratum corneum in different areas of the skin at different time points. * indicates a significant difference compared with before use, p<0.050.

[0071] Figure 5 The moisture content of the stratum corneum in different areas of the skin at different time points. * indicates a significant difference compared with the control, p<0.050.

[0072] Figure 6 The TEWL values ​​of different skin areas at different time points. * indicates a significant difference compared with before use, p<0.050.

[0073] Figure 7 The TEWL values ​​of different skin regions at different time points. * indicates a significant difference compared with the control, p<0.050.

[0074] Figure 8 TEWL / Corn values ​​of different regions at different time points. * indicates significant difference compared with before use, p<0.050.

[0075] Fig. 9 TEWL / Corn values ​​of different regions at different time points. * indicates significant difference compared with the control, p<0.050. DETAILED DESCRIPTION

[0076] The present invention is further described in detail below in conjunction with the accompanying drawings and specific examples of the specification. The examples are only used to explain the present invention and are not used to limit the scope of the present invention. The test methods used in the following examples are conventional methods unless otherwise specified; the materials and reagents used are reagents and materials that can be obtained from commercial channels unless otherwise specified.

[0077] Experimental instruments: electronic balance PL402-L, electronic balance JS0128043, vacuum constant temperature dryer YB-Z, Tianjin Pharmacopoeia Standard Instrument Factory; ultrasonic cleaner KQ-400VSM, Agilent 1260 (DAD diode array detector); chromatographic column OD-3 250×4.6mm, 5μm; OVP-60 oil-free vacuum pump, digital display constant temperature water bath HH-8; UV observation box 5; rotary evaporator EYELA N-1100; electronic temperature control electric heating jacket 98-1-BN; vacuum drying oven.

[0078] Experimental reagents: methanol (chromatographic grade, Tianjin Saifu Century Technology Development Co., Ltd.), Watsons distilled water, glacial acetic acid and dichloromethane (produced by Hunan Huihong Reagent Co., Ltd.); analytical grade ethyl acetate (Tianjin Komiou Chemical Reagent Co., Ltd.).

[0079] The collagen extract used in the embodiment of the present invention was purchased from Quzhou Zhanhong Biotechnology Co., Ltd., batch number: 20220512, with a clear liquid appearance, colorless to slightly yellow, transparent, relative density (D 20 / 4) of 1.005-1.030, refractive index (N 20 / D) of 1.3350-1.3600, solid content of 3.2%-3.8%, pH of 4.0-6.5, and total bacterial count (cfu / g) <100. The pig skin is crushed and vacuumed at below 60°C, extracted and concentrated by alcohol, sterilized to obtain the collagen extract, and frozen and stored for later use.

[0080] Example 1: Combined extraction process of angelica, astragalus and motherwort

[0081] 1. Experimental Methods

[0082] 1. Preparation process

[0083] Implementation 1:

[0084] Extraction: Cut the three herbs of Angelica sinensis, Astragalus membranaceus and Leonurus japonicus into 1-2cm pieces and crush and sieve (all pass through the No. 1 sieve 10 mesh, but mixed with powder that can pass through the No. 3 sieve 50 mesh and not more than 20%) to obtain the coarse powder of the herbs. Weigh 30g of Angelica sinensis, 30g of Astragalus membranaceus and 45g of coarse powder of Leonurus japonicus respectively, and boil and extract twice in a round-bottom flask. Add 10 times the weight of the herbs in water for the first time, soak for 30min, start timing after boiling, heat (70-90℃) and reflux for 2h, filter, and collect the first filtrate. Add 8 times the weight of the herbs in water for the second time, heat and reflux for 1h, filter, and collect the second filtrate; combine the filtrates obtained from the two times, and concentrate to the weight of the herbs by vacuum rotation at 50℃ (vacuum degree -0.09mpa), to obtain the concentrated solution (extract extract), and measure the density with a density meter.

[0085] Purification: Take the extracted extract, dilute it with 5 times the amount of water to obtain a diluted extract, and perform alcohol precipitation. Slowly add 95% ethanol to the diluted extract, and stir it evenly with a glass rod to achieve an ethanol concentration of 75%. After leaving it at room temperature for 24 hours, vacuum filter it to obtain a purified filtrate, and concentrate the purified filtrate to the weight of the medicinal materials by rotating it in a vacuum at 50°C (vacuum degree -0.09 MPa) to obtain a purified extract (i.e., purified concentrate) extracted from angelica, astragalus and motherwort, and measure the density with a density meter.

[0086] Collecting the paste: drying the purified extract at 80°C to constant weight to obtain the combined extract of Angelica, Astragalus and Leonurus japonicus. Calculate the extraction rate of the dry paste.

[0087] Embodiment 2: add 8 times of water for the first boiling and 6 times of water for the second boiling. The other preparation methods are the same as those of Embodiment 1.

[0088] Implementation 3: During the first extraction, water with a volume concentration of 10 times the weight of the medicinal material is replaced with 60% ethanol with a volume concentration of 8 times the weight of the medicinal material, and the mixture is heated under reflux for 1 hour. Other extraction methods are the same as those in Implementation 1.

[0089] Implementation scheme 4: During the first extraction, replace 10 times the weight of the medicinal material with 8 times the weight of the medicinal material, and heat under reflux for 1 hour; during the second extraction, replace the water with 60% volume concentration ethanol, and the other extraction methods are the same as Implementation scheme 1.

[0090] The purification method of implementation schemes 3 and 4 is: combine the filtrates obtained twice, add 5% activated carbon by weight of the filtrate for decolorization, stir for 15 minutes and then filter to obtain a decolorized filtrate, and then concentrate to the weight of the medicinal material according to implementation scheme 1, purify and collect the paste.

[0091] Example 2 Small-scale scale-up process for combined extraction of angelica, astragalus and motherwort

[0092] According to the extraction and purification method of embodiment 2 of example 1, three batches of small-scale test and scale-up process were carried out, wherein the weight of the medicinal materials used in each batch was: 100 g of angelica sinensis, 100 g of astragalus and 150 g of motherwort.

[0093] The obtained Angelica sinensis, Astragalus membranaceus and Leonurus japonicus combined extracted and purified extract is stored at 2-10° C. without collecting the paste.

[0094] Example 3: Pilot-scale extraction of angelica, astragalus and motherwort

[0095] Three batches of pilot processes were carried out according to the extraction and purification method of Example 2. The weight of the medicinal materials used in each batch was: 600 g of Angelica sinensis, 600 g of Astragalus membranaceus and 900 g of Leonuri, and an extract of Angelica sinensis, Astragalus membranaceus and Leonuri was obtained.

[0096] Comparative Example 1 Extracting Angelica sinensis alone

[0097] The effects of the morphology of the medicinal materials (angelica powder and angelica fragments), different concentrations of ethanol as extraction solvents, and three extraction methods (percolation, ultrasonic extraction, and heating reflux extraction) on the extraction rate of angelica were studied.

[0098] 1. Comparative Example 1 Scheme 1:

[0099] Extraction: Crush and sieve the angelica sinensis (all of it can pass through the No. 2 sieve 24 mesh, but it is mixed with powder that can pass through the No. 4 sieve 65 mesh and not more than 40%) to obtain angelica sinensis coarse powder. Weigh 100g of angelica sinensis coarse powder, soak it in 600g of 70% ethanol by volume for 48 hours, and then slowly percolate to keep the ethanol liquid level not lower than the angelica sinensis medicinal surface to obtain the percolate solution. The percolate solution is vacuum-rotated and evaporated at 60℃ to the weight of the medicinal material to obtain the angelica sinensis extract, and the density is tested with a density meter.

[0100] Purification: Add 5 times the amount of water to the angelica extract to dilute it to obtain a diluted extract, add 5% activated carbon by weight of the diluted extract for decolorization, filter after decolorization, and obtain the angelica decolorized filtrate.

[0101] Collecting the paste: After the decolorized filtrate of Angelica sinensis is heated in a 90°C water bath and evaporated to dryness, it is dried at 80°C to constant weight to obtain the Angelica sinensis extract dry paste, and the extraction rate of the dry paste is calculated.

[0102] 2. Comparative Example 1 Scheme 2:

[0103] Extraction: Weigh 50g of Angelica sinensis coarse powder, soak it in 300g of 60% ethanol by volume for 1h, ultrasonicate it for 30min, filter it, and collect the filtrate. Evaporate the filtrate to the weight of the medicinal material at 60℃ in vacuum rotary evaporation to obtain the Angelica sinensis extract, and test the density with a density meter.

[0104] Purification and collection of cream: Same as in Example 1, Scheme 1.

[0105] 3. Comparative Example 1 Scheme 3:

[0106] The volume concentration of ethanol in the immersion extraction was set to 95%, the vacuum rotary evaporation temperature was set to 40° C., and other extraction, purification and cream collection methods were the same as those in Scheme 2 of Comparative Example 1.

[0107] 4. Comparative Example 1 Scheme 4:

[0108] After setting up ethanol immersion, the ultrasonic treatment for 30 min was replaced by heating under reflux for 1 h. Other extraction, purification and cream collection methods were the same as those in Scheme 2 of Comparative Example 1.

[0109] 5. Comparative Example 1 Scheme 5:

[0110] After ethanol immersion, the ultrasonic treatment for 30 min was replaced by heating under reflux for 1 h. Other extraction, purification and cream collection methods were the same as those in Scheme 3 of Comparative Example 1.

[0111] 6. Comparative Example 1 Scheme 6:

[0112] The angelica was cleaned, dried, cut into 1-2 cm segments, and then extracted. Other extraction, purification, and paste collection methods were the same as those in Scheme 2 of Comparative Example 1.

[0113] 7. Comparative Example 1 Scheme 7:

[0114] The angelica form used is the same as that in Scheme 6 of Comparative Example 1, and other extraction methods, purification, and paste collection methods are the same as those in Scheme 3 of Comparative Example 1.

[0115] 8. Comparative Example 1 Scheme 8:

[0116] The angelica form used is the same as that in Scheme 6 of Comparative Example 1, and other extraction, purification and paste collection methods are the same as those in Scheme 4 of Comparative Example 1.

[0117] 9. Comparative Example 1 Scheme 9:

[0118] The angelica form used is the same as that in Scheme 6 of Comparative Example 1, and other extraction, purification and paste collection methods are the same as those in Scheme 5 of Comparative Example 1.

[0119] In the actual extraction process, if the weight of angelica sinensis changes, the weight ratio of ethanol to angelica sinensis remains unchanged, and other process parameters are the same.

[0120] Comparative Example 2 Combined Extraction of Astragalus and Leonurus

[0121] 1. Comparative Example 2 Scheme 1:

[0122] Extraction: Cut the two medicinal materials of Astragalus and Leonurus into 1-2cm segments and crush them with a mortar. Weigh 40g of Astragalus and 60g of Leonurus respectively, boil and extract twice in a round-bottom flask. For the first time, add 8 times the weight of the medicinal materials in water, soak for 30 minutes, start timing after boiling, heat (70-90℃) and reflux for 2 hours, filter, and collect the first filtrate; for the second time, add 6 times the weight of the filter residue in water, heat and reflux for 1 hour, filter, and collect the second filtrate; combine the filtrates obtained from the two times, and concentrate to the weight of the medicinal materials at 50℃ vacuum rotation (vacuum degree -0.09mpa), so as to obtain the Astragalus and Leonurus concentrated solution (extract extract), and use a density meter to test the density.

[0123] Purification and collection of paste: As in Example 1, the Astragalus and Leonurus herba are combined to extract a dry paste, and the extraction rate of the dry paste is calculated.

[0124] 2. Comparative Example 2 Scheme 2:

[0125] The first extraction was carried out with 10 times of water, and the second extraction was carried out with 8 times of water. The other methods were the same as those in Scheme 1 of Comparative Example 2.

[0126] Comparative Example 3: Extraction of Angelica sinensis, Astragalus membranaceus and Leonurus japonicus separately

[0127] 150g of Leonurus japonicus, 100g of Angelica sinensis and 100g of Astragalus membranaceus were extracted and purified respectively in the same manner as in Example 2 to obtain Leonurus japonicus purified extract, Angelica sinensis purified extract and Astragalus membranaceus purified extract.

[0128] Example 4 Preparation of a composite solution by compounding with collagen extract

[0129] The composite solution sample was prepared according to the weight ratio of Leonurus japonicus medicinal material: Astragalus medicinal material: Angelica sinensis medicinal material: collagen extract of 39:26:26:8.

[0130] 1. Preparation of compound solution samples of Example 1 and Comparative Examples 1 and 2

[0131] When preparing the composite solution samples 1 and 2, as shown in Table 1, the combined extract of Astragalus and Motherwort and the dry extract of Angelica sinensis were dissolved in an appropriate amount of water to obtain an aqueous solution of Motherwort, Astragalus and Angelica sinensis with a total weight of 35 g. The above-mentioned aqueous solution of Motherwort, Astragalus and Angelica sinensis was mixed with 3.08 g of collagen extract to prepare a composite aqueous solution, and then filtered with neutral qualitative filter paper (pore size of 30-50 μm) to obtain composite solution samples 1 and 2.

[0132] When preparing the composite solution samples 3 and 4, as shown in Table 1, the combined extract of Angelica sinensis, Astragalus and Motherwort was dissolved in an appropriate amount of water to obtain a motherwort, Astragalus and Angelica sinensis aqueous solution with a total weight of 35 g. The above-mentioned motherwort, Astragalus and Angelica sinensis aqueous solution was mixed with 3.08 g of collagen extract to prepare a composite aqueous solution, and then filtered with neutral qualitative filter paper (pore size of 30-50 μm) to obtain composite solution samples 3 and 4.

[0133] Table 1 Compound solution sample configuration

[0134]

[0135]

[0136] 2. Preparation of compound solution samples for small-scale scale-up process, separate extraction of each medicinal material, and sample preparation of compound solution for pilot process

[0137] 1) Preparation of small-scale scale-up compound solution sample: The purified extract of batch 1 of the small-scale scale-up process of Example 2 was centrifuged at a speed of 12000 rpm for 5 min, the supernatant was taken, and collagen extract was added. The configuration ratio is shown in Table 2 to obtain a composite stock solution.

[0138] Table 2 Small scale test and scale-up process compounding experiment

[0139]

[0140] 2) Preparation of compound solution samples from each medicinal material

[0141] The purified extract of Leonurus japonicus, the purified extract of Angelica sinensis and the purified extract of Astragalus membranaceus from Batch 1 of Comparative Example 3 were centrifuged at 12000 rpm for 5 min, the supernatant was taken, mixed according to the proportions in Table 3, and the collagen extract was added to obtain a composite stock solution.

[0142] Table 3 Experiments on extracting and compounding each herbal medicine separately

[0143]

[0144] 3) Preparation of pilot process compound solution samples

[0145] The purified extract of pilot process batch 1 was taken and compounded solution samples were prepared according to the compounding method in the above-mentioned small-scale test process. The compounding ratios are shown in Table 4.

[0146] Table 4 Pilot process compounding experiment

[0147]

[0148] 3. Preparation of compound solution samples of commercially available extracts of Leonurus japonicus, Astragalus membranaceus and Angelica sinensis

[0149] The motherwort extract, astragalus extract and angelica extract of Company A, and the motherwort extract, astragalus extract and angelica extract of Company B were respectively used to prepare compound solution samples according to the method for preparing compound solution samples by extracting each medicinal material separately.

[0150] Example 5 Calculation of extraction rate and appearance evaluation

[0151] 1. Experimental Methods

[0152] According to the weight of the dry paste obtained, the theoretical amount of paste from the raw medicinal materials is calculated and the extraction rate is calculated. The dry paste extraction rate = dry paste amount / herbal material amount*100%.

[0153] The density of the concentrated solution of each solution was tested using a density / specific gravity tester.

[0154] 2. Experimental Results

[0155] 1. For Example 1

[0156] (1) The concentrated solutions of Schemes 1 and 2 of Example 1 are brown; the concentrated solution of Scheme 3 after the first alcohol extraction is dark green with a large amount of residue, and the concentrated solution of Scheme 4 after the first water extraction is dark green with a large amount of residue. The dark green color is the pigment of Leonurus japonicus. The dry pastes obtained in each scheme are brown-yellow and easily soluble in water.

[0157] (2) According to Table 5, the extraction rate is analyzed: the extraction rate of Scheme 2 of Example 1 is 32.80%, and the extraction rate of Scheme 1 is 26.70%; the extraction rate in Scheme 2 is higher than the extraction rate in Scheme 1.

[0158] The extraction rate of scheme 4 is 29.66%, which is not much different from the extraction rate of scheme 1. The extraction rate of scheme 3 is 32.29%, which is not much different from the extraction rate of scheme 2, with no significant difference. However, the color of the alcohol extraction filtrate is dark green, and activated carbon decolorization is required, and the purification process is complicated. Therefore, the extraction process of schemes 3 and 4 of embodiment 1 is not considered.

[0159] (3) In schemes 1 and 2 of Example 1, during the first extraction, the texture of the motherwort was fluffy, and 10 times the amount of water was more sufficient for soaking. Both 10 times the amount of water and 8 times the amount of water were sufficient for soaking the medicinal material for extraction, but 10 times the amount of water required a long concentration time and high energy consumption; during the second extraction, 6 times the amount of water was sufficient for soaking.

[0160] Table 5: Combined extraction rate of angelica, astragalus and motherwort (final product is dry paste)

[0161]

[0162] 2. For Example 2

[0163] As shown in Table 6, the extract obtained by combining angelica, astragalus and motherwort with water was brown in color, and the density of the extract was controlled at 1.10-1.11 g / cm 3 At the same time, the comparison of the data in Table 5 and Table 6 also shows that the process is stable after the small test is enlarged.

[0164] Table 6 Extraction results of the small-scale scale-up process of combined extraction of Angelica sinensis, Astragalus membranaceus and Leonurus japonicus

[0165]

[0166] 3. For Example 3

[0167] The pilot process results are shown in Table 7. The extract obtained by combining angelica, astragalus and motherwort with water is brown. The density of the extract is controlled at 1.13-1.14 g / cm 3 At the same time, the comparison with the data in Table 5 and Table 7 also shows that the process is still relatively stable after pilot scale-up.

[0168] Table 7 Extraction results of pilot process of combined extraction of Angelica sinensis, Astragalus membranaceus and Leonurus japonicus

[0169]

[0170] 4. For Example 4

[0171] 1) Preparation of compound solution samples of Example 1 and Comparative Examples 1 and 2

[0172] (1) The combined extract of Astragalus and Leonurus is easily soluble in water, and the color is a brownish yellow transparent solution; the collagen extract is light yellow; the alcohol extract of Angelica sinensis is insoluble in water, and after dissolving in water, it is a light yellow turbid solution; when samples 1 and 2 are prepared, the Leonurus, Astragalus and Angelica sinensis aqueous solution produces a precipitate, the upper solution is yellow in color, and the solution is a transparent brownish yellow solution after microporous membrane filtration; the combined extract of Angelica sinensis, Astragalus and Leonurus is easily soluble in water, and the color is brownish yellow, and the solution is a transparent brownish yellow solution after microporous membrane filtration; the color of the Leonurus, Astragalus and Angelica sinensis aqueous solution is dark green, and the solution is a transparent yellow-green solution after microporous membrane filtration. Therefore, sample 3 is easily soluble in water, has a brownish yellow color, has a simple preparation process, and is more suitable for industrial production.

[0173] 2) Preparation of compound solution samples for small-scale scale-up process, separate extraction of each medicinal material, and sample preparation of compound solution for pilot process

[0174] (1) Example 2 Small-scale scale-up process The color of the composite solution sample prepared from the purified extract of batch 1 was brown-yellow and had no precipitation.

[0175] (2) The color of the composite solution sample prepared from the purified extract of Leonurus japonicus, purified extract of Angelica sinensis and purified extract of Astragalus membranaceus in Batch 1 of Comparative Example 3 was brown-yellow with precipitation.

[0176] (3) The color of the composite solution sample of the purified extract configured in the pilot process batch 1 of Example 3 was brown-yellow and had no precipitation.

[0177] 3) Preparation of commercially available mixed solution samples of Leonurus japonicus extract, Astragalus membranaceus extract and Angelica sinensis extract

[0178] Comparative Example 3: The color of the composite solution sample prepared from commercially available Leonurus japonicus extract, Astragalus membranaceus extract and Angelica sinensis extract was brown-yellow with precipitation.

[0179] 4. For Comparative Example 1:

[0180] (1) The dry pastes of Comparative Example 1 Schemes 1 to 6 are all yellow oily pastes.

[0181] (2) From the perspective of Schemes 1 to 3 of Comparative Example 1, it takes 60 hours to extract Angelica sinensis by percolation, which is time-consuming and inefficient. (3) According to the analysis of extraction rate in Table 8: the extraction rate in Scheme 4 of Comparative Example 1 is 49.6%, which is greater than the extraction rate of Scheme 2 of Comparative Example 1, which is 35.8%; the extraction rate of Scheme 5 of Comparative Example 1 is 22.8%, which is greater than the extraction rate of Scheme 3 of Comparative Example 1, which is 4.5%; the extraction rate of Scheme 8 of Comparative Example 1 is 34.3%, which is greater than the extraction rate of Scheme 6 of Comparative Example 1, which is 30.8%; the extraction rate of Scheme 9 of Comparative Example 1 is 18.48%, which is greater than the extraction rate of Scheme 7 of Comparative Example 1, which is 4.1%. Therefore, under the premise of the same ethanol concentration and medicinal material form, the extraction rate of heating reflux is greater than the ultrasonic extraction rate.

[0182] (4) Ethanol concentration: As shown in Table 8, under the same medicinal material morphology and extraction process conditions, the extraction rate of 60% ethanol by volume is greater than that of 95% ethanol by volume. The extraction rate of 60% ethanol by volume concentration of Angelicae Sinensis fragments by hot reflux is 34.3%, and the extraction rate of 95% ethanol by volume concentration of Angelicae Sinensis fragments by hot reflux is 18.48%. The extraction rate of Angelicae Sinensis by 60% ethanol by volume concentration is twice that of 95% ethanol by volume concentration. The dry paste obtained by each extraction is golden yellow, not completely soluble in water, and becomes turbid when dissolved in water.

[0183] In addition, the angelica residue extracted with 60% ethanol by volume is very soft and easily becomes gelatinous. It needs to be re-dissolved and then precipitated with alcohol during purification (Comparative Example 1 Scheme 4). The filtrate of Scheme 8 of Comparative Example 1 is the darkest and has the most sediment. The residue is relatively soft and difficult to purify. Therefore, when extracted with 60% ethanol by volume, the angelica should be in the form of fragments. The residue extracted with 95% ethanol by volume is relatively hard, and the filtrate is yellow and transparent. However, in industrial production, under heating and reflux conditions, the ethanol concentration is high and the safety factor is low (Comparative Example 1 Schemes 5 and 9).

[0184] (5) Medicinal material form: Under the same extraction process and extraction solvent conditions, the extraction rate of Angelica sinensis coarse powder is greater than that of Angelica sinensis fragments. However, since Angelica sinensis coarse powder produces more residues during the extraction process, and considering the above factors to determine the ethanol concentration, Angelica sinensis fragments are more suitable than coarse powder, and 60% volume concentration of ethanol is more suitable than 95% volume concentration of ethanol as the extraction solvent.

[0185] Table 8 Extraction rate of Angelica sinensis extracted separately (final product is dry paste)

[0186]

[0187] 6. For Comparative Example 2:

[0188] (1) Comparative Example 2 The dry pastes of each solution are all brown-yellow and easily soluble in water.

[0189] (2) As shown in Table 9, the extraction rate of Scheme 1 of Comparative Example 2 is 21.9%, and the extraction rate of Scheme 2 of Comparative Example 2 is 19.8%; the properties of the extracts of Scheme 1 of Comparative Example 2 and Scheme 2 of Comparative Example 2 are both brown-yellow and easily soluble in water.

[0190] Table 9 Extraction rate of combined extraction of Astragalus and Leonurus japonicus (final product is dry paste)

[0191]

[0192] Example 6 Liquid chromatography detection content

[0193] 1. Experimental Methods

[0194] (1) Preparation of liquid chromatography solutions

[0195] Preparation of reference solution: Accurately weigh ligustilide, ferulic acid, calycosin glucoside and leonurine, and add methanol to prepare a 5 μg / mL reference solution.

[0196] Preparation of test solution: Take 1 mL of the test sample (if testing purified extract, weigh 0.4 g), place it in a 10 mL volumetric flask, add appropriate amount of 60% methanol solution (containing 0.1% glacial acetic acid), ultrasonically treat for 30 min (power 300 W, frequency 25 kHz), cool, and dilute to the volumetric flask mark with 60% methanol solution (containing 0.1% glacial acetic acid).

[0197] (2) Liquid chromatography conditions

[0198] The liquid chromatography conditions are shown in Table 10.

[0199] Table 10 Liquid chromatography detection conditions

[0200]

[0201] 2. Experimental Results

[0202] 1. For Example 1:

[0203] As pointed out in Example 5, the purification process of Schemes 3 and 4 in Example 1 is complicated, so the extraction process is not considered, and liquid chromatography is no longer performed on it. As shown in Table 11, Scheme 2 in Example 1 has higher content of characteristic components of leonurine, calycosin glucoside, ferulic acid and artemisinin than Scheme 1, and the extraction and concentration time of Scheme 1 in Example 1 is long and the energy consumption is high. Scheme 2 in Example 1 is selected to extract Angelica sinensis, Astragalus and Leonurus japonicus together.

[0204] Table 11 Component detection results of Example 1 Schemes 1 and 2

[0205]

[0206] 2. For Example 2:

[0207] Taking ferulic acid as a representative of the characteristic components, its content in the three batches of purified extracts obtained in Example 2 was detected. The results are shown in Table 12. There is no obvious difference in the content of ferulic acid between different batches, indicating that the small-scale scale-up process of the present invention is stable in production.

[0208] Table 12 Statistical results of the content of characteristic components of the small-scale scale-up process

[0209]

[0210] 3. For Example 3:

[0211] Taking ferulic acid as a representative of the characteristic components, its content in the three batches of purified extracts obtained in Example 3 was detected. The liquid chromatogram results are as follows: Figure 1 As shown, the content calculation results are shown in Table 13. There is no obvious difference in the content of ferulic acid between different batches, indicating that the pilot-scale scale-up process of the present invention is stable in production.

[0212] Table 13 Statistical results of characteristic component contents of pilot process

[0213]

[0214]

[0215] 4. For Comparative Example 1:

[0216] As pointed out in Example 5, the percolation extraction process of Scheme 1 of Comparative Example 1 is not good, and Schemes 2 to 5 of Comparative Example 1 are all extracted with Angelica sinensis coarse powder, which is easy to produce more residues during the extraction process, so the above schemes are no longer subjected to liquid chromatography detection. As shown in Table 14, under ultrasonic conditions, the content of ligustilide in the Angelica sinensis extract dry paste is greater than 50.00%, and the content of ferulic acid is less than 20.00%; under heating and reflux conditions, the content of ligustilide in the Angelica sinensis extract dry paste is greater than 40.00%, and the content of ferulic acid is greater than 20.00%. Compared with the heating and reflux extraction process, the ultrasonic extraction time is short, and it is conducive to the extraction of heat-labile components (such as ligustilide), but it cannot meet the extraction rate of ferulic acid, and it has been stated above that the extraction rate of heating and reflux is greater than the ultrasonic extraction rate. Therefore, the method of Scheme 8 of Comparative Example 1 is better.

[0217] Table 14 Component test results of each solution of Comparative Example 1

[0218]

[0219] 5. For Comparative Example 2

[0220] As shown in Table 15, the content of leonurine detected in Scheme 1 of Comparative Example 2 was 1.96%, and the content of calycosin isoflavone glucoside was 0.52%, and the content of leonurine detected in Scheme 2 of Comparative Example 2 was 1.93%, and the content of calycosin isoflavone glucoside was 0.47%. The extraction rate and representative component content of Schemes 1 and 2 of Comparative Example 2 were not much different, and the product properties were similar without obvious differences.

[0221] Table 15 Test results of components of each solution in comparative example 2

[0222]

[0223] According to the previous appearance identification, the Angelica alcohol extract is insoluble in water, and it is a light yellow turbid solution after being dissolved in water; in the process of preparing the composite solution samples 1 and 2 in Example 4, the Leonurus, Astragalus and Angelica aqueous solution produces precipitates, which are difficult to mix evenly with the collagen extract and have poor stability, which is not conducive to the subsequent development of composite solutions. Therefore, the extraction methods of Comparative Examples 1 and 2 are not selected.

[0224] 6. For Comparative Example 3

[0225] As shown in Table 16, Comparative Example 3 was compared with commercially available angelica extract, astragalus extract and motherwort extract. The results show that the content of the target component in the single medicinal material extract is much higher than that in the commercially available single medicinal material extract (Company A, Company B), and is consistent with the content of the target component in Example 2 and Example 3, indicating that the three medicinal materials can be combined for water extraction, and there is no interaction between the medicinal materials in the extraction of leonurine, ferulic acid, calycosin isoflavones and ligustilide. In the commercially available single medicinal material extract, the corresponding target component is much lower than the content in the self-extracted single medicinal material extract. At the same time, considering that the process of extracting the three medicinal materials separately is complicated, the method of Scheme 2 of Example 1 is selected to extract angelica, astragalus and motherwort together.

[0226] Table 16 Comparison of ingredients in extracts of Angelica sinensis, Astragalus membranaceus and Leonurus japonicus

[0227]

[0228] In Table 16, " / " indicates that the active ingredient was not detected because the substance to be tested does not contain the active ingredient. "0" indicates that the test was performed but no chromatographic peak was detected.

[0229] 7. For Example 4

[0230] As shown in Table 17, the compound solution samples configured in the small-scale scale-up process batch 1 of Example 2 and the compound solution samples configured in the pilot process batch 1 of Example 3 were compared and analyzed. The contents of each target component were basically the same. However, the compound solution samples configured in Example 4 of Company A's motherwort extract, astragalus extract and angelica extract and the compound solution configured in Company B's motherwort extract, astragalus extract and angelica extract were compared and analyzed. The target components were different and some components could not be detected. Figure 2 As shown in the figure, it is the chromatogram of the compound solution of the small-scale scale-up process. Figure 3 Shown is the chromatogram of the pilot process compound solution.

[0231] Table 17 Comparison of ingredients of compound stock solution

[0232]

[0233] "0" means that the test was performed but no chromatographic peak was detected.

[0234] Example 7 Preparation of the compound facial mask liquid of the Buxue Yimu Recipe

[0235] 1. Experimental Methods

[0236] 1. The formula of the compound facial mask liquid of the Buxue Yimu Recipe is shown in Table 18. The plant extract of the Buxue Yimu Recipe is the purified extract obtained according to Scheme 2 of Example 1. The method of preparing the compound stock solution by the small-scale test-amplification process according to Example 4 is used to obtain the Buxue Yimu collagen plant extract.

[0237] Table 18 Mask formula

[0238]

[0239]

[0240]

[0241]

[0242] 2. The preparation method is as follows:

[0243] (1) Cleaning, disinfection and drying equipment

[0244] (2) Add the materials of phase A in Table 18 to the emulsifier in order, first add the liquid raw materials, then add the powder raw materials (be careful not to add the powder materials to the stirring paddle), stir at 60 rpm while heating, and when the temperature rises to 80-90°C, stop heating, keep warm and continue stirring, and turn on the homogenizer, homogenize for 5-8 minutes to ensure that the materials are evenly dispersed, stop homogenizing, and continue stirring. After the materials are evenly dispersed and dissolved, cool down to 45°C while stirring to obtain the dissolved materials of phase A.

[0245] (3) Pre-mix the materials of phase B in Table 18, heat in a water bath to 60-65°C, stir until dissolved into a transparent liquid, and set aside. Add phase B to the dissolved materials of phase A in step (2), stir until uniform, and obtain a mixed dissolved material of phases A and B.

[0246] (4) The phase C material in Table 18 is mixed with the phase A and B dissolved materials in step (3), homogenized and stirred until the material is uniform, and then the cooling water is turned on to cool the material to 40° C. to obtain a mixed dissolved material of phases A, B and C.

[0247] (5) Dissolve the phase D material in Table 18 with a small amount of water to obtain a phase D material solution, then slowly and gradually add the phase D material solution to the mixed dissolved materials of phases A, B and C in step (4), stir until uniform, and adjust the pH value to 5.5-6.5 to obtain a mixed dissolved material of phases A, B, C and D.

[0248] (6) After the premix of the E phase material in Table 18 is uniform, it is added to the mixed dissolved materials of A, B, C and D phases in step (5), stirred at a medium speed of 100-150 rpm until the mixture is uniform, cooled to 38°C, and after the inspection index is qualified, filtered through 200 mesh to obtain the facial mask liquid. The facial mask liquid is divided and filled into irradiated sterilized facial mask bags, 30 mL per bag, to obtain the facial mask.

[0249] Example 8 Mask Moisturizing and Repairing Efficacy Test

[0250] 1. Mask testing method:

[0251] (1) Detection method

[0252] The subjects cleaned their faces with a facial cleanser and dried their skin with dry facial tissues, then sat in a laboratory at 21±1°C and 50±10% RH for 30 minutes.

[0253] One side of the subject's cheek was randomly selected as the mask sample 1 area, and the other side was selected as the mask sample 2 area. The mask prepared in Example 7 was used in the mask sample 1 area, and the control mask was used in the mask sample 2 area. After applying for 15 to 20 minutes, the mask was removed and massaged to help absorb the mask liquid.

[0254] Laboratory technicians used the skin moisture test probe Corneometer CM825 and the skin moisture loss test probe Tewameter TM300 to respectively detect the moisture content of the skin stratum corneum and the transepidermal water loss TEWL value of the skin, and calculated the TEWL / Corn value. The detection time was 0h, 2h and 6h after using the mask.

[0255] Mask sample 1 is the mask prepared in Example 7, and mask sample 2 is the control mask sample. In the control mask, the plant extract of Buxue Yimu Fang is a compound solution prepared according to the method of sample 1 in Example 4.

[0256] (2) Subject information

[0257] Gender of subjects: female; Age of subjects: 25-41 years old; Number of subjects: 40.

[0258] Other criteria for the subjects: healthy, facial stratum corneum moisture content <60 c.u., TEWL value >15 g / h / m 2 ; Be able to cooperate well with the experimenters and maintain a regular life during the study; Be able to read and understand all the contents of the informed consent form and voluntarily sign the informed consent form; Agree not to use any cosmetics, drugs and health products that may affect the results during the trial.

[0259] 2. Experimental Results

[0260] like Figure 4 and Figure 5As shown, 2h and 6h after using the mask sample, the moisture content of the stratum corneum of the skin of the subjects in the mask sample 1 area increased by 31.24% and 24.08%, which was significantly different from before use. 2h and 6h after using the mask sample, the moisture content of the stratum corneum of the skin of the subjects in the mask sample 2 area increased by 26.63% and 13.62%, which was significantly different from before use. Moreover, compared with mask sample 1 and mask sample 2, the hydrating effect of mask sample 1 is significantly better than that of mask sample 2, especially the moisture content increase rate after 6h of use is significantly better than that of mask sample 2, indicating that mask sample 1 has a longer hydrating time.

[0261] like Figure 6 and Figure 7 As shown, 2h and 6h after using the samples, the TEWL value of the mask sample 1 area of ​​the subjects decreased by 20.72% and 19.37%, which was significantly different from before use. 2h and 6h after using the mask samples, the TEWL value of the mask sample 2 area of ​​the subjects decreased by 15.38% and 14.03%, which was significantly different from before use. Moreover, compared with mask sample 1 and mask sample 2, mask sample 1 is significantly better than mask sample 2 in preventing the loss of moisture in the stratum corneum, and mask sample 1 has a more lasting moisturizing effect.

[0262] The smaller the TEWL / Corn value, the better the skin barrier function. Figure 8 and Fig. 9 As shown, 2h and 6h after using the mask sample, the TEWL / Corn value of the mask sample 1 area of ​​the subject decreased by 42.31% and 36.54%, which was significantly different from before use. 2h and 6h after using the mask sample, the TEWL / Corn value of the mask sample 2 area of ​​the subject decreased by 36.73% and 28.57%, which was significantly different from before use. Moreover, 2h and 6h after using the samples, there was a significant difference in the TEWL / Corn values ​​of the mask sample 1 and mask sample 2 areas of the subjects, and the effect of mask sample 1 on improving the skin barrier function was significantly better than mask sample 2.

[0263] The above data show that the facial mask prepared by the present invention has the effects of hydrating, moisturizing and repairing.

[0264] Example 9 Facial Mask Whitening and Spot Removal Effect

[0265] 1. Experimental Methods

[0266] Take the facial mask liquid of Example 7 and the control facial mask liquid, and prepare them into a 0.5 mg / mL test solution with phosphate buffer. 5U / mL tyrosinase solution and 0.02 mol / L L-tyrosine solution. In the control mask solution, the plant extract of Buxue Yimu Fang is a compound solution prepared according to the method of Sample 1 in Example 4.

[0267] Take 1 mL of the test solution, 1 mL of L-tyrosine solution, 1 mL of tyrosinase solution and 2 mL of phosphate buffer solution and mix them evenly. After standing at 37°C for 15 min, measure the absorbance at 475 nm. Repeat three times and take the average value to calculate the tyrosinase inhibition rate.

[0268] Tyrosinase inhibition rate = [1-(D3-D4) / (D1-D2)] × 100%; wherein, D1 does not add the test solution; D2 does not add the test solution and tyrosinase solution; D3 adds the test solution, L-tyrosine solution and tyrosinase solution; D4 does not add the tyrosinase solution; the reaction system is supplemented to 5 mL with phosphate buffer.

[0269] 2. Experimental Results

[0270] The tyrosinase inhibition rate of the facial mask liquid of Example 7 is 85.21%, and the tyrosinase inhibition rate of the facial mask liquid of the control facial mask liquid is 69.35%. The facial mask of Example 7 of the present invention can effectively inhibit the activity of tyrosinase and has the effect of whitening and removing spots.

[0271] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention rather than to limit the protection scope of the present invention. For ordinary technicians in this field, other different forms of changes or modifications can be made based on the above descriptions and ideas. It is not necessary and impossible to list all the implementation methods here. Any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should be included in the protection scope of the claims of the present invention.

Claims

1. A method for preparing a plant extract of Buxue Yimu Fang, characterized in that: The following steps are involved: S1: Take three medicinal materials, namely, Angelica sinensis, Astragalus membranaceus and Leonurus japonicus, soak them in water 8 to 10 times the weight of the medicinal materials, heat and reflux for extraction for 1.5 to 2 hours, filter and collect the filtrate; S2: Add 6 to 8 times the weight of the medicinal material again, heat and reflux to extract for 1h to 1.5h, filter to obtain a filtrate; S3: combining the filtrates of step S1 and S2 to obtain a combined filtrate; subjecting the combined filtrate to alcohol precipitation purification, solid-liquid separation, and collecting the purified filtrate to obtain the plant extract of Buxue Yimu Fang.

2. The preparation method according to claim 1, characterized in that: In step S1, water 8 times the weight of the sample is added for immersion.

3. The preparation method according to claim 1, characterized in that: In step S1, the extraction is carried out under heating reflux for 2 h, and in step S2, the extraction is carried out under heating reflux for 1 h.

4. The preparation method according to claim 1, characterized in that: In step S2, water in an amount of 6 times the weight of the medicinal residue is added and heated to reflux for extraction.

5. The preparation method according to claim 1, characterized in that: In step S3, during the alcohol precipitation purification, ethanol is added to the combined filtrate to an ethanol concentration of 75%.

6. The preparation method according to claim 1, characterized in that: In step S3, the purified filtrate is concentrated by vacuum rotation to obtain the plant extract of Buxue Yimu Fang.

7. The plant extract of Buxue Yimu Fang prepared by the method according to any one of claims 1 to 6.

8. Use of the plant extract of Buxue Yimu Recipe according to claim 7 in preparing skin care products.

9. A skin care product, characterized in that: The skin care product contains the plant extract of the blood-replenishing and motherwort prescription as claimed in claim 7.

10. The skin care product according to claim 9, characterized in that: The skin care product also contains collagen extract.

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