A kind of kudzu vine extract with oil control and acne removal effect and its preparation method and application
Through the synergistic method of reverse micelle solvent and flash extraction, the Gexian rice extract rich in polysaccharides, proteins, VB1 and VB2 was extracted, solving the problems of long extraction time, high energy consumption and single efficacy in the prior art, and achieving the effect of oil control and acne removal.
Patent Information
- Application Number
- CN202411482237.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-23
- Publication Date
- 2025-03-04
- Estimated Expiration
- 2044-10-23
AI Technical Summary
In the prior art, the extract of Gexian rice is long and has high energy consumption. The extract is single and is only used for moisturizing and hydrating, and lacks the effect of controlling oil and removing acne.
The method of synergistic interaction between reverse micelle solvent and flash extraction is used to damage the structure of reverse micelle group by adjusting the ionic strength and pH value, and extracting the leucoria extract rich in polysaccharides, proteins, VB1 and VB2.
It significantly improves the extraction rate of active substances of Gexian rice, shortens the extraction time, reduces energy consumption, and realizes the effect of oil control and acne removal, and is suitable for the preparation of oil control and acne removal skin care products.
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Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of natural product extraction and preparation, and particularly relates to a kudzu vine extract with oil-controlling and acne-removing effects, and a preparation method and application thereof. Background Art
[0002] The nutritional content of kudzu vine is rich, and the edible and medicinal use of kudzu vine has a long history, but its application in the field of beauty and skin care has not attracted people's attention, especially the extraction of nutritional components of kudzu vine and its application in the preparation of cosmetics, only a few relevant literature reports. The Chinese patent application with publication number CN101822630A proposes a method for preparing a kudzu extract, wherein the dry algae of kudzu are taken, sieved after crushing, swollen for several hours in advance, boiled and extracted several times with water, filtered and collected the filtrate, the filtrate is concentrated under reduced pressure, concentrated and precipitated with alcohol, centrifuged to obtain a precipitate, and the precipitate is dried to form kudzu polysaccharide, which can be used for preparing moisturizing and hydrating cosmetics; the Chinese patent application with publication number CN104873576A proposes an antibacterial composition containing kudzu extract, wherein the kudzu extract used is prepared according to the following method: fresh kudzu is taken, crushed, irradiated with microwave power, boiled with water, filtered while hot, water is added to the filter residue to continue decocting, the extraction is repeated three times, the filtrate is combined, and fine filtration is performed to obtain a kudzu extract. The kudzu extract obtained by these prior arts is a kudzu polysaccharide dry matter or a kudzu polysaccharide extract, the extraction time is too long, the energy consumption is high, the material is single, and it is only used for moisturizing and hydrating in cosmetics, and the effect is single. Summary of the invention
[0003] In order to overcome the shortcomings and deficiencies in the above-mentioned prior art, shorten the extraction time, improve the extraction efficiency and reduce energy consumption, the primary purpose of the present invention is to provide a method for preparing a Pueraria lobata extract rich in polysaccharides, proteins, VB1, VB2 and other substances with oil-controlling and acne-removing effects.
[0004] Another object of the present invention is to provide a kudzu vine extract prepared by the above preparation method and having the effect of controlling oil and removing acne.
[0005] Another object of the present invention is to provide an application of the above-mentioned Pueraria lobata extract having the effect of controlling oil and removing acne.
[0006] The purpose of the present invention is achieved through the following technical solutions:
[0007] A method for preparing a kudzu vine extract having oil-controlling and acne-removing effects comprises the following steps:
[0008] (1) drying fresh kudzu vine root, and grinding the kudzu vine root through an 80-mesh sieve to obtain kudzu vine root powder;
[0009] (2) Pour sodium dodecyl sulfate powder into an isooctane-n-octanol mixture to fully dissolve it to obtain a sodium dodecyl sulfate / isooctane-n-octanol solution, wherein the volume ratio of isooctane to n-octanol in the isooctane-n-octanol mixture is 4:1; then add KCl-phosphate buffer solution with a concentration of 0.20-0.30 mol / L, and stir until the solution becomes clear and transparent to obtain an SDS reverse micelle solvent;
[0010] (3) mixing the kudzu vine powder obtained in step (1) with the SDS reverse micelle solvent obtained in step (2) at a solid-liquid ratio of 1 g:50-100 mL, and then placing the mixture in a flash extractor for flash extraction to obtain a kudzu vine crude extract;
[0011] (4) adding an equal volume of KCl-phosphate buffer having a pH of 9.0 and a concentration of 0.50-2.00 mol / L to the crude extract of the radix puerariae obtained in step (3); shaking the mixture at room temperature, transferring the centrifuged solution into a separatory funnel after centrifugation, and recovering the upper organic solvent after standing and stratifying; concentrating the lower aqueous phase to 1 / 3-1 / 2 of its volume, and then adding hexylene glycol and p-hydroxyacetophenone to obtain a radix puerariae extract; the mass percentage concentrations of hexylene glycol and p-hydroxyacetophenone in the radix puerariae extract are 2% and 0.5%, respectively.
[0012] The polysaccharide content of the kudzu vine extract in step (4) is ≥3.00 mg / mL, the protein content is ≥0.10 mg / mL, VB1 is ≥0.01 mg / mL, and VB2 is ≥0.002 mg / mL.
[0013] The concentration of sodium dodecyl sulfate in the sodium dodecyl sulfate / isooctane-n-octanol solution in step (2) is 0.06-0.10 g / mL; the amount of KCl-phosphate buffer added is calculated based on the water content in the reaction system being controlled at 20-30 wt % after the addition of KCl-phosphate buffer.
[0014] More preferably, the concentration of sodium dodecyl sulfate in the sodium dodecyl sulfate / isooctane-n-octanol solution is 0.08 g / mL; the amount of KCl-phosphate buffer added is calculated based on the water content in the reaction system being controlled at 30 wt % after the addition of KCl-phosphate buffer.
[0015] The concentration of the KCl-phosphate buffer in step (2) is 0.25 mol / L.
[0016] The material-liquid ratio in step (3) is preferably 1 g:67 mL.
[0017] The voltage of the flash extraction in step (3) is 40-80 V, preferably 50-70 V; the time of the flash extraction is 0.5-3 min, preferably 1-2 min.
[0018] The concentration of the KCl-phosphate buffer in step (4) is preferably 1.14 mol / L.
[0019] The shaking time in step (4) is 30 minutes; the centrifugation is carried out in a centrifuge at a speed of 4000 r / min for 10 minutes.
[0020] A kudzu vine extract with oil-controlling and acne-removing effects prepared by the above preparation method.
[0021] The application of the above-mentioned kudzu vine extract with oil-controlling and acne-removing effects in the preparation of oil-controlling and acne-removing skin care products.
[0022] The kudzu vine extract is the only active ingredient in the oil-controlling and acne-removing skin care product.
[0023] The principle of the present invention is:
[0024] Reverse micelles refer to aggregates containing a water molecule core formed by surfactants dissolved in organic solvents, which are nano-sized and present as dispersed phases, and are also called reverse micelles or reverse micelles. In reverse micelles, the dual effects of surfactants and organic solvents place water inside the aggregates and organic solvents outside the aggregates. The present invention uses reverse micelle solvents to extract active ingredients from kudzu vine. During the pre-extraction process, the surfactant layer formed by the surfactant, the organic phase and the aqueous phase attracts the adjacent protein molecules due to electrostatic effects, and then the reverse micelle groups complete the encapsulation of the protein molecules (protecting the proteins from denaturation or fracture degradation due to the violent reaction process), and begin to break away from the attraction of the two interfaces and disperse into the organic phase, and the pre-extraction process is completed; in the present invention, other active ingredients such as polysaccharides are always in the aqueous phase, and the final required phase is also the aqueous phase; the present invention then destroys the reverse micelle group structure by adjusting the main influencing factors such as ionic strength and pH value, so that the target protein molecules are separated from the reverse micelle organic phase solution and enter the aqueous phase, and finally obtain an aqueous phase rich in active ingredients, and the post-extraction process is completed.
[0025] Flash extraction relies on high-speed mechanical shear force and ultra-dynamic molecular percolation technology to break the material into fine particles within a few seconds at room temperature and in the presence of solvents, promoting the contact and collision between the reverse micelle solution and the solid powder, so that the effective ingredients quickly reach a balance inside and outside the tissue. At the same time, the spatial structure of the protein develops in a direction that is more conducive to entering the reverse micelle group, thereby improving the protein extraction rate, retaining the effective ingredients to the maximum extent, and not being damaged by heat. The amount of solvent used is small, the extraction time is short, and the efficiency is high.
[0026] Compared with the prior art, the present invention has the following advantages and effects:
[0027] (1) The method of the present invention adopts the synergistic effect of reverse micelle solvent and flash extraction, which significantly improves the extraction rate of active substances in kudzu vine, deeply extracts the active ingredients in kudzu vine, and makes the obtained kudzu vine extract have good oil control and acne removal effects, and is very suitable for preparing oil control and acne removal products.
[0028] (2) The method of the present invention shortens the extraction time, improves the extraction efficiency, reduces the energy consumption, and realizes the recycling of the reverse micelle solvent.
[0029] (3) The production process is simple and can effectively reduce production costs. The reverse micelle technology realizes the simultaneous and efficient extraction of polysaccharides and proteins from Pueraria lobata. Part of the solvent can be recycled, which can effectively reduce production costs. DETAILED DESCRIPTION
[0030] The present invention is further described below with reference to specific embodiments, but they should not be construed as limiting the present invention.
[0031] Example 1
[0032] A kudzu vine extract with oil-controlling and acne-removing effects is prepared by the following method:
[0033] S1. After drying fresh kudzu vine, crush it with a pulverizer and pass it through an 80-mesh sieve to obtain kudzu vine powder; weigh 18.76g of sodium dodecyl sulfate (SDS) powder, pour the SDS powder into 234.5mL of a prepared isooctane-n-octanol mixed solution (the volume ratio of isooctane to n-octanol is 4:1) to fully dissolve it, and obtain a sodium dodecyl sulfate / isooctane-n-octanol solution with a concentration of 0.07g / mL of sodium dodecyl sulfate; add 100.5mL of a KCl-phosphate buffer with a concentration of 0.25mol / L, stir until the solution becomes clear and transparent, and obtain an SDS reverse micelle solvent; mix 5g of kudzu vine powder and SDS reverse micelle solvent at a solid-liquid ratio of 1g:67mL, and then place it in a flash extractor, set the voltage to 60V, and flash extract for 2min to obtain a kudzu vine crude extract;
[0034] S2. Add an equal volume of KCl-phosphate buffer with a pH of 9.0 and a concentration of 1.14 mol / L to the crude extract of the radix puerariae obtained in step S1, transfer the mixture into a centrifuge after shaking at room temperature for 30 min, centrifuge at 4000 r / min for 10 min, transfer the centrifuge into a separating funnel, recover the upper organic solvent after standing and stratifying, collect the lower aqueous phase extract and concentrate it to 165 g, add hexylene glycol and p-hydroxyacetophenone so that the proportions of the two in the final radix puerariae extract are 2 wt% hexylene glycol and 0.5 wt% p-hydroxyacetophenone, respectively, to obtain a radix puerariae extract.
[0035] Example 2
[0036] A kudzu vine extract with oil-controlling and acne-removing effects is prepared by the following method:
[0037] S1. After drying fresh kudzu vine, crush it with a pulverizer, pass it through an 80-mesh sieve, and obtain kudzu vine powder; weigh 16g of sodium dodecyl sulfate (SDS) powder, pour the SDS powder into a prepared 200mL isooctane-n-octanol mixed solution (the volume ratio of isooctane to n-octanol is 4:1) to fully dissolve it, and obtain a sodium dodecyl sulfate / isooctane-n-octanol solution with a concentration of 0.07g / mL of sodium dodecyl sulfate; add 50mL of KCl-phosphate buffer with a concentration of 0.20mol / L, stir until the solution becomes clear and transparent, and obtain SDS reverse micelle solvent; mix 5g of kudzu vine powder and SDS reverse micelle solvent at a solid-liquid ratio of 1g:50mL, and then place it in a flash extractor, set the voltage to 60V, and flash extract for 2min to obtain a kudzu vine crude extract;
[0038] S2. Add an equal volume of KCl-phosphate buffer with a pH of 9.0 and a concentration of 1.14 mol / L to the crude extract of the radix puerariae obtained in step S1, transfer the mixture into a centrifuge after shaking at room temperature for 30 min, centrifuge at 4000 r / min for 10 min, transfer the centrifuge into a separating funnel, recover the upper organic solvent after standing and stratifying, collect the lower aqueous phase extract and concentrate it to 165 g, add hexylene glycol and p-hydroxyacetophenone so that the proportions of the two in the final radix puerariae extract are 2 wt% hexylene glycol and 0.5 wt% p-hydroxyacetophenone, respectively, to obtain a radix puerariae extract.
[0039] Example 3
[0040] A kudzu vine extract with oil-controlling and acne-removing effects is prepared by the following method:
[0041] S1. After drying fresh kudzu vine root, crush it with a pulverizer, pass it through an 80-mesh sieve, and obtain kudzu vine root powder; weigh 10.5g of sodium dodecyl sulfate (SDS) powder, pour the SDS powder into the prepared 175mL isooctane-n-octanol mixed solution (the volume ratio of isooctane to n-octanol is 4:1) to fully dissolve it, and obtain a sodium dodecyl sulfate / isooctane-n-octanol solution with a concentration of 0.06g / mL of sodium dodecyl sulfate; add 75mL of KCl-phosphate buffer with a concentration of 0.25mol / L, stir until the solution becomes clear and transparent, and obtain SDS reverse micelle solvent; mix 5g of kudzu vine root powder and SDS reverse micelle solvent at a solid-liquid ratio of 1g:50mL, and then place it in a flash extractor, set the voltage to 70V, and flash extract for 2min to obtain a kudzu vine root crude extract;
[0042] S2. Add an equal volume of KCl-phosphate buffer with a pH of 9.0 and a concentration of 1.14 mol / L to the crude extract of the radix puerariae obtained in step S1, transfer the mixture into a centrifuge after shaking at room temperature for 30 min, centrifuge at 4000 r / min for 10 min, transfer the centrifuge into a separating funnel, recover the upper organic solvent after standing and stratifying, collect the lower aqueous phase extract and concentrate it to 165 g, add hexylene glycol and p-hydroxyacetophenone so that the proportions of the two in the final radix puerariae extract are 2 wt% hexylene glycol and 0.5 wt% p-hydroxyacetophenone, respectively, to obtain a radix puerariae extract.
[0043] Example 4
[0044] A kudzu vine extract with oil-controlling and acne-removing effects is prepared by the following method:
[0045] S1. After drying fresh kudzu vine root, crush it with a pulverizer, pass it through an 80-mesh sieve, and obtain kudzu vine root powder; weigh 25.2g of sodium dodecyl sulfate (SDS) powder, pour the SDS powder into the prepared 350mL isooctane-n-octanol mixed solution (the volume ratio of isooctane to n-octanol is 4:1) to fully dissolve it, and obtain a sodium dodecyl sulfate / isooctane-n-octanol solution with a concentration of 0.07g / mL of sodium dodecyl sulfate; add 150mL of KCl-phosphate buffer with a concentration of 0.25mol / L, stir until the solution becomes clear and transparent, and obtain SDS reverse micelle solvent; mix 5g of kudzu vine root powder and SDS reverse micelle solvent at a solid-liquid ratio of 1g:100mL, and then place it in a flash extractor, set the voltage to 58V, and flash extract for 1min to obtain a kudzu vine root crude extract;
[0046] S2. Add an equal volume of KCl-phosphate buffer with a pH of 9.0 and a concentration of 1.14 mol / L to the crude extract of the radix puerariae obtained in step S1, transfer the mixture into a centrifuge after shaking at room temperature for 30 min, centrifuge at 4000 r / min for 10 min, transfer the centrifuge into a separating funnel, recover the upper organic solvent after standing and stratifying, collect the lower aqueous phase extract and concentrate it to 165 g, add hexylene glycol and p-hydroxyacetophenone so that the proportions of the two in the final radix puerariae extract are 2 wt% hexylene glycol and 0.5 wt% p-hydroxyacetophenone, respectively, to obtain a radix puerariae extract.
[0047] Comparative Example 1
[0048] The other steps are the same as those in Example 1, except that the mass concentration of the sodium dodecyl sulfate / isooctane-n-octanol solution obtained in S1 is different.
[0049] That is, S1 of this comparative example is specifically as follows:
[0050] S1. After drying fresh kudzu vine root, crush it with a pulverizer, pass it through an 80-mesh sieve, and obtain kudzu vine root powder; weigh 9.38g of sodium dodecyl sulfate (SDS) powder, pour the SDS powder into 234.5mL of the prepared isooctane-n-octanol mixed solution (the volume ratio of isooctane to n-octanol is 4:1) to fully dissolve it, and obtain a sodium dodecyl sulfate / isooctane-n-octanol solution with a concentration of 0.04g / mL of sodium dodecyl sulfate; add 100.5mL of KCl-phosphate buffer with a concentration of 0.25mol / L, stir until the solution becomes clear and transparent, and obtain SDS reverse micelle solvent; mix 5g of kudzu vine root powder and SDS reverse micelle solvent at a solid-liquid ratio of 1g:67mL, and then place it in a flash extractor, set the voltage to 60V, and flash extract for 2min to obtain a kudzu vine root crude extract.
[0051] Comparative Example 2
[0052] The other steps are the same as those in Example 1, except that the material-liquid ratio of S1 is different.
[0053] That is, S1 of this comparative example is specifically as follows:
[0054] S1. After drying fresh kudzu vine root, crush it with a pulverizer, pass it through an 80-mesh sieve, and obtain kudzu vine root powder; weigh 18.76g of sodium dodecyl sulfate (SDS) powder, pour the SDS powder into 234.5mL of the prepared isooctane-n-octanol mixed solution (the volume ratio of isooctane to n-octanol is 4:1) to fully dissolve it, and obtain a sodium dodecyl sulfate / isooctane-n-octanol solution with a concentration of 0.07g / mL of sodium dodecyl sulfate; add 100.5mL of KCl-phosphate buffer with a concentration of 0.25mol / L, stir until the solution becomes clear and transparent, and obtain SDS reverse micelle solvent; mix 5g of kudzu vine root powder and SDS reverse micelle solvent at a solid-liquid ratio of 1g:30mL, and then place it in a flash extractor, set the voltage to 60V, and flash extract for 2min to obtain a kudzu vine root crude extract.
[0055] Comparative Example 3
[0056] The other steps are the same as those in Example 1, except that the extraction voltage and extraction time of S1 are different.
[0057] That is, S1 of this comparative example is specifically as follows:
[0058] S1. After drying fresh kudzu vine root, crush it with a pulverizer, pass it through an 80-mesh sieve, and obtain kudzu vine root powder; weigh 18.76g of sodium dodecyl sulfate (SDS) powder, pour the SDS powder into 234.5mL of the prepared isooctane-n-octanol mixed solution (the volume ratio of isooctane to n-octanol is 4:1) to fully dissolve it, and obtain a sodium dodecyl sulfate / isooctane-n-octanol solution with a concentration of 0.07g / mL of sodium dodecyl sulfate; add 100.5mL of KCl-phosphate buffer with a concentration of 0.25mol / L, stir until the solution becomes clear and transparent, and obtain SDS reverse micelle solvent; mix 5g of kudzu vine root powder and SDS reverse micelle solvent at a solid-liquid ratio of 1g:67mL, and then place it in a flash extractor, set the voltage to 150V, and flash extract for 0.5min to obtain a kudzu vine root crude extract.
[0059] Comparative Example 4
[0060] The other steps are the same as those in Example 1, except that the concentration of S2 KCl-phosphate buffer is different.
[0061] That is, S2 of this comparative example is specifically as follows:
[0062] S2. Add an equal volume of KCl-phosphate buffer with a pH of 9.0 and a concentration of 2.50 mol / L to the crude extract of the radix puerariae obtained in step S1, transfer the mixture into a centrifuge after oscillation at room temperature for 30 min, centrifuge at 4000 r / min for 10 min, transfer the centrifuge into a separatory funnel, recover the upper organic solvent after standing and stratifying, collect the lower aqueous phase extract and concentrate it to 165 g, add hexylene glycol and p-hydroxyacetophenone so that the proportions of the two in the final radix puerariae extract are 2 wt% hexylene glycol and 0.5 wt% p-hydroxyacetophenone, respectively, to obtain a radix puerariae extract.
[0063] Comparative Example 5
[0064] The other steps are the same as those in Example 1, except that the extraction method of S1 adopts ultrasonic-assisted extraction.
[0065] That is, S1 of this comparative example is specifically as follows:
[0066] S1. After drying fresh kudzu vine, crush it with a grinder and pass it through an 80-mesh sieve to obtain kudzu vine powder; weigh 14g of sodium dodecyl sulfate (SDS) powder, pour the SDS powder into 234.5mL of the prepared isooctane-n-octanol mixed solution (the volume ratio of isooctane to n-octanol is 4:1) to fully dissolve it, and obtain a sodium dodecyl sulfate / isooctane-n-octanol solution; add 100.5mL of 0.25mol / L KCl-phosphate buffer, stir until the solution becomes clear and transparent, and obtain an SDS reverse micelle solvent; mix 5g of kudzu vine powder and SDS reverse micelle solvent at a solid-liquid ratio of 1g:67mL, and perform ultrasonic-assisted extraction with an ultrasonic power of 225W and an ultrasonic time of 40min.
[0067] Comparative Example 6
[0068] The other steps are the same as in Example 1, except that the extractant of S1 is different.
[0069] That is, S1 of this comparative example is specifically as follows:
[0070] S1. After drying fresh kudzu vine root, crush it with a pulverizer and pass it through an 80-mesh sieve to obtain kudzu vine root powder; weigh 5 g of kudzu vine root powder, mix it with 335 mL of water at a solid-liquid ratio of 1 g:67 mL, and then place it in a flash extractor, set the voltage to 60 V, and flash extract for 2 min to obtain a kudzu vine root crude extract.
[0071] Test Example 1 Determination of the content of oil-controlling and acne-removing ingredients in the extract of Pueraria lobata
[0072] 1. Determination of polysaccharide content in kudzu vine extract
[0073] Preparation of total sugar solution: Add 1 mL of distilled water and 2 mL of 6 mol / L hydrochloric acid solution to 1 mL of the sample solution to be tested, heat in a boiling water bath for 5 min, then cool to room temperature, add a drop of phenolphthalein indicator solution, and then add 15 wt% sodium hydroxide solution until the solution turns slightly red, transfer to a 10 mL volumetric flask, and shake to volume.
[0074] Preparation of reducing sugar solution: Place 1 mL of the sample solution to be tested in a 10 mL volumetric flask, add one drop of phenolphthalein indicator solution, then add 15 wt% sodium hydroxide solution until the solution turns slightly red, add pure water to the scale, and shake well.
[0075] 1 mL of the prepared total sugar solution and reducing sugar solution were taken and placed in different test tubes. 2 mL of DNS reagent was added to each test tube. After being fully mixed, the mixture was placed in a boiling water bath for 5 min. After being taken out, the mixture was quickly cooled to room temperature and 9 mL of distilled water was added to each test tube. The blank solution was used as a control and the absorbance of the solution was measured at 540 nm.
[0076] The content of reducing sugar and total sugar is determined, and the difference between the two is the polysaccharide content.
[0077] 2. Determination of protein content in kudzu vine extract
[0078] Preparation of Roche solution:
[0079] 1) Prepare solution A: Weigh 2 g of sodium hydroxide and 10 g of sodium carbonate, dissolve them in 400 mL of pure water, and dilute to 500 mL after they are fully dissolved to obtain solution A.
[0080] 2) Prepare solution B: weigh 0.1 g of sodium potassium tartrate and 0.05 g of copper sulfate, dissolve them in 8 mL of pure water, and dilute to 10 mL after full dissolution to obtain solution B.
[0081] 3) Mix solution A and solution B in a volume ratio of 50:1 to obtain Roche solution, and store at 4°C.
[0082] Preparation of standard solution: Bovine serum albumin (BSA) is used as the standard. Weigh 0.05 g BSA and dissolve it in 50 mL of 0.1 mol / L sodium hydroxide solution. Take 10 mL of this solution and dilute it to 50 mL with distilled water to prepare the BSA standard solution. 1 mL of BSA standard solution contains 200 μg of protein.
[0083] Add 5 mL of Roche solution to the standard solutions and sample solutions of different concentrations, shake well, and leave for 10-15 minutes. Then add 0.5 mL of 1 mol / L Folin phenol solution, shake well, and leave at room temperature in the dark for 30 minutes. Measure the absorbance of each solution at 660nm using a UV-visible spectrophotometer.
[0084] Compare the absorbance of the sample solution with the standard curve to obtain the protein content.
[0085] 3. Determination of VB1 and VB2 content in Pueraria extract
[0086] VB1: Refer to GB5009.84-2016 Determination of vitamin B1 in food; VB2: Refer to GB5009.85-2016 Determination of vitamin B2 in food.
[0087] 4. The results of testing the contents of the effective components in the extracts of Puerariae lobata obtained in Examples 1-4 and Comparative Examples 1-6 are shown in Table 1.
[0088] Table 1 Determination results of active ingredient content (unit: mg / mL)
[0089]
[0090] As can be seen from Table 1, the contents of polysaccharides, proteins, VB1 and VB2 and other effective ingredients in the kudzu vine extracts obtained in Examples 1 to 4 are higher than those in the kudzu vine extracts obtained in Comparative Examples 1 to 6, indicating that the method of the present invention deeply extracts the effective ingredients in kudzu vine, so that the obtained kudzu vine extract has good oil-controlling and acne-removing effects, and is very suitable for preparing oil-controlling and acne-removing products.
[0091] Test Example 2: Oil control and acne removal effect of the essence containing kudzu vine extract
[0092] 1. Preparation of oil-control and anti-acne essence containing kudzu vine extract
[0093] 5wt% glycerol, 3wt% propylene glycol, 0.2wt% hydroxyethyl cellulose and 85.85wt% deionized water were heated and stirred to dissolve until there were no particles, and then kept at 85°C for 20 min, cooled to 50°C with stirring, and 2wt% of iris extract was added and stirred evenly, 0.3wt% p-hydroxyacetophenone, 0.35wt% 1,2-hexanediol, 0.03wt% phenoxyethanol and 0.27wt% ethylhexylglycerol were heated until dissolved evenly, then added to the system and stirred evenly, cooled with cold water, and finally 3wt% butylene glycol was added and stirred evenly to obtain essence solutions 1-10 (wherein, essence solutions 1-4 contained the iris extracts obtained in Examples 1-4, and essence solutions 5-10 contained the iris extracts obtained in Comparative Examples 1-6).
[0094] 2. Test of the oil control and acne removal effect of the essence
[0095] 1. Test subjects: 60 subjects with mixed or oily skin, mild or moderate acne, aged 18-35 years old, were randomly selected.
[0096] 2. Test sample: 1 to 10 of the essence solution containing the extracts of Examples 1 to 4 and Comparative Examples 1 to 6.
[0097] 3. Test area: face. Use the self-before and after control method and record the samples used by each subject.
[0098] 4. Test method: The subjects were randomly divided into 10 groups, 6 people in each group, and each group tested 1 sample. After cleaning the face, 1g of essence solution was applied to the test area and massaged for absorption, once in the morning and evening, for 30 consecutive days. The glossiness of the subject's face was measured using the Skin-Glossymeter GL200 test probe (Courage+khazaka, Germany), and the test was performed 3 times at each time and the average value was taken. The working environment temperature was 23-25℃, and the relative humidity was 45%-65%. After the subject sat quietly for 20 minutes, the skin glossiness of the test area sample was tested before use (T0), and then the test sample was used as specified. The skin glossiness of the test area was tested at 15 days and 30 days respectively.
[0099] The sensory evaluation of the subjects on the oil-control effect of the samples and the oil secretion test results were statistically analyzed, and the oil-control and acne-removing effects and irritation of the 10 groups of samples were investigated.
[0100] 3. Test results of the oil control and acne removal effect of the essence
[0101] Table 2 Oil secretion test results and sensory evaluation satisfaction of subjects
[0102]
[0103] As can be seen from Table 2, the use of the essence solution to which the extract of the iris lobata obtained in Examples 1 to 4 is added significantly reduces the oil secretion on the skin surface.
[0104] Table 3 Increased glossiness of cheeks before and after using the essence solution ∆L
[0105]
[0106] As can be seen from Table 3, all subjects can observe that acne becomes smaller and redness and swelling are reduced within 1-15 days. Among them, the essence solution prepared from the kudzu vine extract obtained in Example 1 is the best in reducing skin inflammation, increasing skin glossiness, and having the highest acne removal efficiency.
[0107] Table 4 Evaluation results of improvement of skin sensitivity symptoms of subjects
[0108]
[0109] Note: If the redness, swelling, itching, oily acne and symptoms are significantly improved, it will be recorded as markedly effective; if the redness, swelling, itching, oily acne and symptoms are not improved or even aggravated, it will be recorded as ineffective.
[0110] As can be seen from Table 4, the essence solution prepared from the extract of Puerariae lobata obtained in Example 1 is most effective in relieving skin inflammation and improving skin sensitivity, and the subjects did not experience irritation.
[0111] It can be seen from Tables 2, 3 and 4 that, compared with Comparative Examples 1-6, the essence stock solution to which the extract of Pueraria lobata obtained in Examples 1-4 is added can better improve the oiliness and acne on the face of the subjects, and there is no skin allergy, that is, the extract of Pueraria lobata obtained in Examples 1-4 has the best oil control and acne removal effect and skin friendliness.
[0112] In summary, the kudzu vine extract obtained by the present invention is mild and non-irritating, effectively reduces excessive secretion of skin oil, and relieves the effects of redness, swelling, and pain of inflammatory acne.
[0113] The above embodiments are preferred implementation modes of the present invention, but the implementation modes of the present invention are not limited to the above embodiments. Any other changes, modifications, substitutions, combinations, and simplifications that do not deviate from the spirit and principles of the present invention should be equivalent replacement methods and are included in the protection scope of the present invention.
Claims
1. A method for preparing a kudzu vine extract having oil-controlling and acne-removing effects, characterized in that The steps include: (1) drying fresh kudzu vine root, and grinding the kudzu vine root through an 80-mesh sieve to obtain kudzu vine root powder; (2) Pour sodium dodecyl sulfate powder into an isooctane-n-octanol mixture and fully dissolve it to obtain a sodium dodecyl sulfate / isooctane-n-octanol solution, wherein the volume ratio of isooctane to n-octanol in the isooctane-n-octanol mixture is 4:1, and the concentration of sodium dodecyl sulfate in the sodium dodecyl sulfate / isooctane-n-octanol solution is 0.06-0.10 g / mL; then add KCl-phosphate buffer having a concentration of 0.20-0.30 mol / L, and stir until the solution becomes clear and transparent to obtain an SDS reverse micelle solvent; the amount of the KCl-phosphate buffer added is calculated based on the water content in the reaction system being controlled at 20-30 wt % after the addition of the KCl-phosphate buffer; (3) mixing the kudzu vine powder obtained in step (1) with the SDS reverse micelle solvent obtained in step (2) at a solid-liquid ratio of 1 g: 50-100 mL, and then placing the mixture in a flash extractor for flash extraction to obtain a kudzu vine crude extract; the flash extraction voltage is 40-80 V, and the flash extraction time is 0.5-3 min; (4) adding an equal volume of KCl-phosphate buffer having a pH of 9.0 and a concentration of 1.14 mol / L to the crude extract of the radix puerariae obtained in step (3); shaking the mixture at room temperature, transferring the centrifuged solution into a separatory funnel after centrifugation, and recovering the upper organic solvent after standing and stratification; concentrating the lower aqueous phase to 1 / 3-1 / 2 of its volume, and then adding hexylene glycol and p-hydroxyacetophenone to obtain a radix puerariae extract; the mass percentages of hexylene glycol and p-hydroxyacetophenone in the radix puerariae extract are 2% and 0.5%, respectively.
2. The method for preparing the kudzu vine extract having the effect of controlling oil and removing acne according to claim 1, characterized in that: The polysaccharide content of the kudzu vine extract in step (4) is ≥3.00 mg / mL, the protein content is ≥0.10 mg / mL, VB1 is ≥0.01 mg / mL, and VB2 is ≥0.002 mg / mL.
3. The method for preparing the kudzu vine extract having the effect of controlling oil and removing acne according to claim 1, characterized in that: The concentration of sodium dodecyl sulfate in the sodium dodecyl sulfate / isooctane-n-octanol solution is 0.08 g / mL; the amount of KCl-phosphate buffer added is calculated based on the water content in the reaction system being controlled at 30 wt % after the KCl-phosphate buffer is added.
4. The method for preparing the kudzu vine extract having the effect of controlling oil and removing acne according to claim 1, characterized in that: The concentration of the KCl-phosphate buffer in step (2) is 0.25 mol / L; The shaking time in step (4) is 30 minutes; the centrifugation is carried out in a centrifuge at a speed of 4000 r / min for 10 minutes.
5. The method for preparing the kudzu vine extract having the effect of controlling oil and removing acne according to claim 1, characterized in that: The material-liquid ratio in step (3) is 1 g:67 mL.
6. The method for preparing the kudzu vine extract having the effect of controlling oil and removing acne according to claim 1, characterized in that: The voltage of the flash extraction in step (3) is 50-70V, and the time of the flash extraction is 1-2min.
7. An extract of Herba Puerariae with oil-controlling and acne-removing effects prepared by the preparation method according to any one of claims 1 to 6.
8. Use of the extract of Miscanthus puerariae with oil-controlling and acne-removing effects according to claim 7 in the preparation of oil-controlling and acne-removing skin care products.
9. The use according to claim 8, characterized in that: The kudzu vine extract is the only active ingredient in the oil-controlling and acne-removing skin care product.
Citation Information
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