Oroxylum indicum extract serving as skin oil control active matter as well as preparation method and application of oroxylum indicum extract

Abstract

The invention relates to an oroxylum indicum extract serving as a skin oil control active matter as well as a preparation method and application of the oroxylum indicum extract. Wherein the oroxylum indicum extract serving as the skin oil control active matter at least comprises the following components in percentage by mass: 25%-35% of oroxylum indicum A and 20%-35% of oroxylum indicum B. The oroxylum indicum extract serving as the skin oil control active matter is natural and mild, can effectively inhibit skin oil secretion, can inhibit inflammation and can reduce lipid peroxidation products, so that the prepared cosmetics have excellent oil control and soothing effects, and are safe, green, natural and mild.

Description

Technical Field

[0001] The invention relates to the technical field of cosmetics, and in particular to an Oroxylum butterfly extract as a skin oil-control active substance, and a preparation method and application thereof. Background Art

[0002] Oily skin is caused by excessive secretion of sebaceous glands and dysfunction of sebaceous glands. The sebaceous glands of people with oily skin tend to secrete too much oil, which makes the face shiny and prone to corresponding facial skin diseases, such as skin sensitivity, allergies, acne, seborrheic dermatitis, etc.

[0003] At present, there are mainly two types of active ingredients for oil control in traditional cosmetics: the first type: oil-absorbing powders, such as silica, starch, PMMA, etc., which can quickly fill pores and absorb excess oil to improve oily skin. The effect is fast, but long-term use may cause pores to become clogged, and can only control oil temporarily, not treating the root cause. The second type: organic acid ingredients, such as salicylic acid, which can achieve the effect of exfoliation, and also have strong oil-control activity, but they are irritating and cannot be ignored. Long-term use may lead to excessive removal of the stratum corneum, causing redness, desquamation and other problems, and cause the stratum corneum to become thinner. Summary of the invention

[0004] Based on this, it is necessary to provide an Oroxylum butterfly extract as a skin oil control active substance and its preparation method and application to address the above problems. The Oroxylum butterfly extract as a skin oil control active substance is natural and mild, can effectively inhibit skin oil secretion, and can also inhibit inflammation and reduce the production of lipid peroxidation products, so that the prepared cosmetics not only have excellent oil control and soothing effects, but are also safe, green, natural and mild.

[0005] An oroxylum butterfly extract as a skin oil-control active ingredient comprises at least the following components in percentage by mass: 25%-35% oroxylin A and 20%-35% oroxylin B.

[0006] The method for preparing the Oroxylum indica extract as a skin oil-control active ingredient comprises the following steps:

[0007] A. Using ethanol to heat and reflux extract the Oroxylum butterfly powder, and then filtering to obtain the Oroxylum butterfly extract;

[0008] B. Concentrating the volume of the Oroxylum indica extract to 8 to 12 times the mass of the Oroxylum indica powder, obtaining a supernatant by centrifugation, and filtering the supernatant to obtain an Oroxylum indica concentrate;

[0009] C. enriching the Oroxylum indica concentrate by a macroporous adsorption resin column, and then introducing an eluent to elute, to obtain an eluent, wherein the flow rate of the Oroxylum indica concentrate is 2BV / h-4BV / h, and the flow rate of the eluent is 1BV / h-3BV / h;

[0010] D. Concentrating the volume of the eluate to 1 to 1.5 times the mass of the Oroxylum indica powder, and then spray drying the eluate to obtain the Oroxylum indica extract as a skin oil-control active ingredient.

[0011] In one of the embodiments, 50%-80% by mass ethanol is used to perform two heating reflux extractions on the Oroxylum butterfly powder, wherein the temperature of each reflux extraction is 70°C-90°C, the extraction time is 1h-3h, the solid-liquid ratio is 1:10-1:30, and the mixture is filtered through a 100-300 mesh filter, and finally the filtrate is combined to obtain the Oroxylum butterfly extract.

[0012] In one embodiment, the mass fraction of ethanol in the Oroxylum indica concentrate is 5%-30%, and the solid content of the Oroxylum indica concentrate is 2.0%-3.0%;

[0013] And / or, in the step of obtaining the supernatant by centrifugation, the centrifugal speed is 8000×g-10000×g, and the centrifugal time is 10 min-20 min;

[0014] And / or, in the step of filtering the supernatant, the pore size of the filter membrane is 1 μm-5 μm, and the filter membrane is selected from any one of a mixed cellulose ester membrane, a polyethersulfone membrane, and a nylon membrane.

[0015] In one of the embodiments, in the step of introducing the eluent for elution, the macroporous adsorption resin column is first cleaned with deionized water to remove impurities, the flow rate of deionized water is 2BV / h-4BV / h, and the flow rate of deionized water is 8BV-10BV; then, an ethanol solution with a mass fraction of 50%-80% is used for analysis, and the flow rate of the ethanol solution is 4BV-8BV to obtain an eluent.

[0016] In one embodiment, the volume of the eluent is concentrated to 1-1.5 times the mass of the Oroxylum indica powder to obtain a concentrated solution, the solid content of the concentrated solution is 7%-15%, and the mass fraction of ethanol in the concentrated solution is 2%-15%.

[0017] In one of the embodiments, the packing diameter-to-height ratio of the macroporous adsorption resin in the macroporous adsorption resin column is 1:4-1:8, and the macroporous adsorption resin skeleton is styrene-divinylbenzene and / or divinylbenzene.

[0018] In one embodiment, the macroporous adsorption resin is selected from LX-T83.

[0019] Application of Oroxylum butterfly extract as skin oil-control active ingredient in oil-control functional cosmetics.

[0020] In one embodiment, the mass fraction of the Oroxylum indica extract as a skin oil-control active ingredient in the oil-control functional cosmetic is 0.001%-0.2%.

[0021] The Oroxylum butterfly extract in the present invention, as an efficient skin oil control active ingredient, contains a specific ratio of Oroxylum butterfly glycoside A and Oroxylum butterfly glycoside B. This unique ratio gives the Oroxylum butterfly extract the ability to inhibit the activity of key factors such as FAS, SCD, SREBP-1C, PLIN2, etc., thereby effectively controlling the secretion of skin oil at multiple levels and achieving a significant oil control effect. In addition, excessive oil secretion may cause a series of inflammatory problems. The Oroxylum butterfly extract can effectively alleviate and improve the state of sebum oxidation by inhibiting the activity of the inflammatory mediator PGE2 and significantly reducing the generation of lipid peroxidation products. The Oroxylum butterfly extract as a skin oil control active ingredient is natural and non-irritating. Therefore, the Oroxylum butterfly extract in the present invention, as a skin oil control active ingredient, is not only natural and mild, but also can effectively control the secretion of skin oil. At the same time, it can also inhibit inflammatory reactions and reduce the production of lipid peroxidation products, so that the cosmetics prepared based on this ingredient not only have excellent oil control and soothing effects, but also ensure the safety and mildness of the product. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments recorded in the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0023] Figure 1 It is a staining fluorescence comparison diagram of any three locations of the model control group, positive control group and sample group Example 1 samples in Experimental Example 1 of the present invention under a fluorescence microscope, wherein A represents the model control group, B represents the positive control group, and C represents the sample group Example 1 samples. DETAILED DESCRIPTION

[0024] For ease of understanding of the present invention, the present invention will be described in more detail below. However, it should be understood that the present invention can be implemented in many different forms and is not limited to the embodiments or examples described herein. On the contrary, the purpose of providing these embodiments or examples is to make the understanding of the disclosure of the present invention more thorough and comprehensive.

[0025] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as those generally understood by those skilled in the art of the present invention. The terms used herein in the specification of the present invention are only for the purpose of describing specific implementation methods or embodiments, and are not intended to limit the present invention. The optional scope of the term "and / or" used herein includes any one of two or more related listed items, and also includes any and all combinations of related listed items, and the combinations include any two related listed items, any more related listed items, or all related listed items.

[0026] The applicant has found through research that the oroxylum butterfly is the dried mature seeds of the oroxylum butterfly plant of the Bignoniaceae family. It looks like paper and is also called "thousand-layer paper". It is often used for lung heat cough, throat paralysis, hoarseness, liver and stomach pain, and has been included in the "Chinese Pharmacopoeia". The chemical composition of the oroxylum butterfly plant is complex, containing flavonoids, parahydroxyphenylethanol, cyclohexanol and volatile oils. Flavonoids are the main active ingredients of the oroxylum butterfly plant. The special pharmacological activity exhibited by the oroxylum butterfly extract has whitening, acne removal, anti-ultraviolet, after-sun repair and liver cancer cell inhibition effects, but the use of oroxylum butterfly extract as an oil-control active ingredient in oil-control and soothing cosmetics has not been reported so far.

[0027] To this end, the Oroxylum indica extract provided by the present invention as a skin oil-control active ingredient comprises at least the following components in percentage by mass: 25%-35% of Oroxylin A and 20%-35% of Oroxylin B.

[0028] The Oroxylum butterfly extract provided by the present invention as a skin oil control active ingredient contains a specific ratio of Oroxylum butterfly glycoside A and Oroxylum butterfly glycoside B. This unique ratio gives the Oroxylum butterfly extract the ability to inhibit the activity of key factors such as FAS, SCD, SREBP-1C, PLIN2, etc., thereby effectively controlling the secretion of skin oil at multiple levels and achieving a significant oil control effect. In addition, excessive oil secretion may cause a series of inflammatory problems. The Oroxylum butterfly extract can effectively alleviate and improve the state of sebum oxidation by inhibiting the activity of the inflammatory mediator PGE2 and significantly reducing the generation of lipid peroxidation products. The Oroxylum butterfly extract as a skin oil control active ingredient is natural and non-irritating. Therefore, the Oroxylum butterfly extract in the present invention is not only natural and mild as a skin oil control active ingredient, but also can effectively control the secretion of skin oil. At the same time, it can also inhibit inflammatory reactions and reduce the generation of lipid peroxidation products, so that the cosmetics prepared based on this ingredient not only have excellent oil control and soothing effects, but also ensure the safety and mildness of the product.

[0029] Therefore, the Oroxylum butterfly extract of the present invention, which is a skin oil-control active ingredient, is natural and mild, can effectively inhibit skin oil secretion, and can also inhibit inflammation and reduce the production of lipid peroxidation products, so that the prepared cosmetics not only have excellent oil-control and soothing effects, but are also safe, green, natural and mild.

[0030] It is understandable that the Oroxylum indica extract used as the skin oil-control active ingredient in the present invention may contain other auxiliary components, such as chrysin, baicalin, etc., in addition to the effective active ingredients of Oroxylin A and Oroxylin B.

[0031] At the same time, the present invention also provides a method for preparing the above-mentioned Oroxylum indica extract as a skin oil-control active ingredient, comprising the following steps:

[0032] A. Using ethanol to heat and reflux extract the Oroxylum butterfly powder, and then filtering to obtain the Oroxylum butterfly extract;

[0033] B. Concentrating the volume of the Oroxylum indica extract to 8 to 12 times the mass of the Oroxylum indica powder, obtaining a supernatant by centrifugation, and filtering the supernatant to obtain an Oroxylum indica concentrate;

[0034] C. enriching the Oroxylum indica concentrate by a macroporous adsorption resin column, and then introducing an eluent to elute, to obtain an eluent, wherein the flow rate of the Oroxylum indica concentrate is 2BV / h-4BV / h, and the flow rate of the eluent is 1BV / h-3BV / h;

[0035] D. Concentrating the volume of the eluate to 1 to 1.5 times the mass of the Oroxylum indica powder, and then spray drying the eluate to obtain the Oroxylum indica extract as a skin oil-control active ingredient.

[0036] In step A, the number of times of heating and refluxing extraction of the Oroxylum butterfly powder with ethanol can be once, twice, or three times, and in the present invention, twice is preferred.

[0037] Specifically, 50%-80% ethanol by mass is used to heat and reflux extract the Oroxylum butterfly powder twice, wherein the temperature of each reflux extraction is 70°C-90°C, the extraction time is 1h-3h, the solid-liquid ratio is 1:10-1:30, and a 100-300 mesh filter is used for filtration, and finally the filtrate is combined to obtain the Oroxylum butterfly extract. In this way, the effective active ingredients in the Oroxylum butterfly powder can be fully extracted.

[0038] In one embodiment, the method for preparing the Oroxylum butterfly powder comprises the following steps: placing the Oroxylum butterfly raw material in an oven and drying it to a constant weight, and using a high-speed grinder to crush the Oroxylum butterfly for later use.

[0039] It should be noted that the origins of the Oroxylum indica raw materials used in the present invention include but are not limited to Yunnan, China, Guangxi, China, Vietnam, Myanmar and the like.

[0040] In step B, the mass fraction of ethanol in the Oroxylum butterfly concentrate is 5%-30%, and the solid content of the Oroxylum butterfly concentrate is 2.0%-3.0%. It can be understood that in this step, by controlling the mass fraction of ethanol and the solid content in the Oroxylum butterfly concentrate, the smoothness of the Oroxylum butterfly concentrate on the column in the subsequent step S3 can be effectively guaranteed, the efficiency of enrichment can be improved, and the loss of the effective oil-controlling active ingredients in the Oroxylum butterfly can be minimized, thereby facilitating the improvement of the yield of the effective oil-controlling active ingredients in the Oroxylum butterfly extract.

[0041] Optionally, in the step of obtaining the supernatant by centrifugation, the centrifugal speed is 8000×g-10000×g, and the centrifugal time is 10 min-20 min. Such a setting is conducive to further removing impurities and improving the purity of the effective oil-controlling active ingredients.

[0042] Optionally, in the step of filtering the supernatant, the pore size of the filter membrane is 1 μm-5 μm, and the filter membrane is selected from any one of a mixed cellulose ester membrane, a polyethersulfone membrane, and a nylon membrane. This arrangement can further remove impurities, which is beneficial to regulating the solid content of the Oroxylum indica concentrate.

[0043] In step C, the packing diameter-to-height ratio of the macroporous adsorption resin in the macroporous adsorption resin column is 1:4-1:8. Such a setting can help improve the separation efficiency of the macroporous adsorption resin column for the effective active ingredients in Oroxylum butterfly.

[0044] Optionally, the macroporous adsorption resin skeleton is styrene-divinylbenzene and / or divinylbenzene, preferably styrene-divinylbenzene. Further, the macroporous adsorption resin is selected from any one of LX-T83, D-101, AB-8, YKDH-2, HPD100, preferably LX-T83. Such a setting has high separation selectivity and adsorption for the effective active ingredients in the oroxylum butterfly extract, especially oroxylum butterfly glycoside A and oroxylum butterfly glycoside B, which is beneficial to improve the yield of the effective active ingredients in the oroxylum butterfly extract, especially the use of LX-T83 resin can obtain oroxylum butterfly glycoside A and oroxylum butterfly glycoside B with a higher mass concentration.

[0045] In one embodiment, before the macroporous adsorption resin is filled in the column, the macroporous adsorption resin is also pretreated, and the pretreatment steps include: soaking the macroporous adsorption resin in 95% ethanol by mass for 24 hours, washing with pure water until there is no alcohol taste; then adding 4% sodium hydroxide to soak for 4 hours, and washing with pure water until neutral; then adding 4% hydrochloric acid to soak for 4 hours, and finally washing with pure water until neutral.

[0046] In one embodiment, the eluent is an ethanol solution.

[0047] Optionally, in the step of introducing the eluent for elution, the macroporous adsorption resin column is first cleaned with deionized water to remove impurities, the flow rate of deionized water is 2BV / h-4BV / h, and the flow rate of deionized water is 8BV-10BV; then, an ethanol solution with a mass fraction of 50%-80% is used for analysis, and the flow rate of the ethanol solution is 4BV-8BV to obtain an eluent. This arrangement can effectively remove the residual liquid and some water-soluble impurities in the column, and improve the purity of the Oroxylum indica extract.

[0048] In step D, a concentrated solution is also obtained, wherein the solid content of the concentrated solution is 7%-15%, and the mass fraction of ethanol in the concentrated solution is 2%-15%.

[0049] In one embodiment, the spray drying temperature is 135°C-145°C.

[0050] It can be understood that in the preparation method of the Oroxylum butterfly extract as a skin oil control active substance of the present invention, an ethanol reflux extraction method is adopted to avoid the use of high-risk organic reagents such as methanol and ethyl acetate, and the process is safer. At the same time, by controlling the flow rate of the Oroxylum butterfly concentrate and the flow rate of the eluent during the enrichment and elution process, under this synergistic effect, a high-yield Oroxylum butterfly extract is obtained, especially the content of Oroxylum butterfly glycoside A and Oroxylum butterfly glycoside B as the main oil control effective active ingredients in the Oroxylum butterfly extract. Specifically, in the Oroxylum butterfly extract as a skin oil control active substance, the mass fraction of Oroxylum butterfly glycoside A reaches 25%-35%, and the mass fraction of Oroxylum butterfly glycoside B reaches 20%-35%, which can significantly improve the oil control and soothing effect of the Oroxylum butterfly extract, so that the prepared cosmetics have both excellent oil control and soothing effects. Moreover, the preparation method has a simple process, low cost, and is conducive to large-scale production.

[0051] In addition, the present invention also provides a use of the Oroxylum butterfly extract as a skin oil-control active substance in oil-control functional cosmetics. The oil-control functional cosmetics have excellent oil-control and soothing effects and are safe, green, natural and mild.

[0052] Specifically, the Oroxylum butterfly extract is used as an active substance for inhibiting oil and lipid secretion in oil-controlling cosmetics.

[0053] Optionally, the mass fraction of the Oroxylum butterfly extract as a skin oil control active substance in the oil control functional cosmetic is 0.001%-0.2%. Specifically, the mass fraction of the Oroxylum butterfly extract as a skin oil control active substance in the oil control functional cosmetic includes but is not limited to 0.001%, 0.005%, 0.008%, 0.01%, 0.05%, 0.08%, 0.2%. Such an arrangement can further improve the oil control and soothing effect of the cosmetic.

[0054] In one embodiment, the dosage form of the oil-controlling functional cosmetic includes but is not limited to water, lotion, essence or cream.

[0055] Hereinafter, the Oroxylum butterfly extract as a skin oil control active ingredient and its preparation method and application will be further described through the following specific examples. However, those skilled in the art will understand that the following examples are only used to illustrate the present invention and should not be regarded as limiting the scope of the present invention. If no specific conditions are specified in the examples, the conventional conditions or the conditions recommended by the manufacturer are followed. The reagents or instruments used without indicating the manufacturer are all conventional products that can be obtained commercially.

[0056] It should be noted that in the present invention, high performance liquid chromatography is used to detect the contents of effective active oroxylin A and oroxylin B in the oroxylin extract as skin oil-control active ingredients.

[0057] Study on Optimization of Macroporous Adsorption Resin

[0058] Soak each type of macroporous adsorption resin in 95% ethanol for 24 hours, and wash with pure water until there is no alcohol smell; add 4% sodium hydroxide and soak for 4 hours, and wash with pure water until the pH is neutral; add 4% hydrochloric acid and soak for 4 hours, and rinse with pure water until the pH is neutral, and set aside.

[0059] Weigh 200g of Yunnan Oroxylum butterfly powder and add it to a 60% ethanol solution by mass, heat it to 85°C for the first extraction, wherein the extraction time is 1h and the solid-liquid ratio is 1:20, to obtain a first extract; pass the first extract through a 300-mesh filter to obtain a first filtrate and a first filter residue; then add the first filter residue obtained above to a 60% ethanol solution by mass, and heat it to 85°C for a second extraction, wherein the second extraction time is 1h and the second solid-liquid ratio is 1:10, to obtain a second extract, then pass the second extract through a 300-mesh filter to obtain a second filtrate, then filter the first filtrate and the second filtrate respectively, and combine the filtrates to obtain the Oroxylum butterfly extract.

[0060] The volume of 5.1 L of Oroxylum indica extract was vacuum dried and concentrated to 8 times the mass of Oroxylum indica powder (v / w), that is, concentrated to a volume of 1.6 L, and then centrifuged to discard the precipitate and collect the supernatant, wherein the centrifugal speed was 10000×g and the centrifugal time was 20 min. The supernatant was passed through a mixed cellulose ester membrane (MCE membrane) with an average pore size of 5 μm, and the filtrate was collected to obtain the Oroxylum indica concentrate, which is liquid 1.

[0061] The pretreated macroporous adsorption resin was filtered until no water dripped, 1.0 g of each was accurately weighed and placed in a 50 mL centrifuge tube with a stopper, and 25 mL of Oroxylum confusum concentrate was added respectively. The tubes were placed in a shaker and shaken at 25 °C and 180 rpm / min for 24 h to allow the macroporous adsorption resin to reach a saturated adsorption state. After the adsorption of the macroporous adsorption resin was completed, the resin was allowed to stand for solid-liquid separation, the supernatant was taken, and then filtered with a filter membrane with an average pore size of 0.22 μm, and the filtrate was collected as liquid 2.

[0062] Take the saturated macroporous adsorption resin, put it into a stoppered centrifuge tube, add 10mL of 60% ethanol solution by mass, place it in a shaker, and shake it at 25°C and 180rpm / min for 12h to completely desorb the macroporous adsorption resin; after desorption is completed, let it stand for solid-liquid separation, take the supernatant and filter it with a filter membrane with an average pore size of 0.22μm, and collect the desorption filtrate of each type of macroporous adsorption resin, which is liquid 3.

[0063] The contents of oroxylin A and oroxylin B in liquid 1, liquid 2 and liquid 3 were detected by HPLC. The static adsorption capacity, static desorption capacity and resolution of each type of macroporous adsorption resin were calculated according to the results. The calculation results are shown in Table 1, where the calculation formula is as follows:

[0064] Static adsorption capacity (mg / g) = V 液体1 ×(C 液体1 -C 液体2 ) / m 大孔吸附树脂 , where V 液体1 represents the volume of liquid 1, C 液体1 represents the concentration of oroxylin A or oroxylin B in liquid 1, C 液体2 represents the concentration of oroxylin A or oroxylin B in liquid 2, m 大孔吸附树脂 Represents the quality of macroporous adsorption resin.

[0065] Static analytical quantity (mg / g) = (V 液体3 ×C 液体3 ) / m 大孔吸附树脂 , where V 液体3 represents the volume of liquid 3, C 液体3 represents the concentration of oroxylin A or oroxylin B in liquid 3, m 大孔吸附树脂 Represents the quality of macroporous adsorption resin.

[0066] Resolution rate (%) = static resolution amount / static adsorption amount × 100%;

[0067] Component yield (%) = (V 液体3 ×C 液体3 ) / (V 液体1 ×C 液体1)×100%.

[0068] Table 1 Static adsorption effect test

[0069]

[0070] It can be seen from the data in Table 1 that the static saturated adsorption capacity and desorption rate of various types of macroporous adsorption resins are somewhat different. Considering the adsorption capacity, desorption rate and component yield of each resin on the oroxylum concentrate, the adsorption capacity and component yield of LX-T83 macroporous adsorption resin are relatively high, especially the component yield of oroxylum glycoside B is significantly higher than that of other resins. Therefore, this experiment finally determined that LX-T83 resin is the preferred resin, which can simultaneously ensure the component yields of oroxylum glycoside A and oroxylum glycoside B.

[0071] Example 1

[0072] Weigh 200g of Yunnan Oroxylum butterfly powder and add it to a 60% ethanol solution by mass, heat it to 85°C for the first extraction, wherein the extraction time is 1h and the solid-liquid ratio is 1:20, to obtain a first extract; pass the first extract through a 300-mesh filter to obtain a first filtrate and a first filter residue; then add the first filter residue obtained above to a 60% ethanol solution by mass, and heat it to 85°C for a second extraction, wherein the second extraction time is 1h and the second solid-liquid ratio is 1:10, to obtain a second extract, then pass the second extract through a 300-mesh filter to obtain a second filtrate, then filter the first filtrate and the second filtrate respectively, and combine the filtrates to obtain the Oroxylum butterfly extract.

[0073] The volume of 5.2 L of Oroxylum indica extract is vacuum dried and concentrated to 10 times the mass of Oroxylum indica powder (v / w), that is, concentrated to a volume of 2 L, and then centrifuged to discard the precipitate and collect the supernatant, wherein the centrifugal speed is 10000×g, the centrifugal time is 20 min, the supernatant is passed through a mixed cellulose ester membrane (MCE membrane) with an average pore size of 5 μm, and the filtrate is collected to obtain Oroxylum indica concentrate, wherein the mass fraction of ethanol in the Oroxylum indica concentrate is 20%, and the solid content of the Oroxylum indica concentrate is 2.4%.

[0074] The Oroxylum indica concentrate obtained above was dynamically adsorbed using 200 mL of LX-T83 resin column to obtain Oroxylum indica concentrate, wherein the column diameter-to-height ratio of the LX-T83 resin was 1:5, and the adsorption flow rate was 4 BV / h. After the adsorption was completed, 10 BV of deionized water was passed through the LX-T83 resin column at a flow rate of 4 BV / h to clean the LX-T83 resin column bed to remove some water-soluble impurities, and then 5 BV of 60% ethanol was passed through the LX-T83 resin column at a flow rate of 2 BV / h to collect the eluate.

[0075] The volume of 1L of the eluate is vacuum concentrated to 1 times the mass of the Oroxylum butterfly powder (v / w), that is, the volume is concentrated to about 200mL, to obtain a concentrated solution, wherein the solid content of the concentrated solution is 15%, and the mass fraction of ethanol in the concentrated solution is 15%. The concentrated solution is then spray-dried at an inlet temperature of 145°C to obtain a light yellow powder, that is, the Oroxylum butterfly extract as a skin oil-control active ingredient, wherein in the Oroxylum butterfly extract as a skin oil-control active ingredient, the mass fraction of oroxylin A is 28.88%, and the mass fraction of oroxylin B is 24.19%.

[0076] Example 2

[0077] Weigh 200g of Oroxylum indica powder produced in Guangxi and add it to a 50% ethanol solution by mass, heat it to 75°C for the first extraction, wherein the extraction time is 3h and the solid-liquid ratio is 1:30, to obtain a first extract; pass the first extract through a 100-mesh filter to obtain a first filtrate and a first filter residue; then add the first filter residue obtained above to a 50% ethanol solution by mass, and heat it to 75°C for a second extraction, wherein the second extraction time is 1.5h and the second solid-liquid ratio is 1:10, to obtain a second extract, then pass the second extract through a 100-mesh filter to obtain a second filtrate, then filter the first filtrate and the second filtrate respectively, and combine the filtrates to obtain the Oroxylum indica extract.

[0078] The volume of 7.2L of Oroxylum indica extract is vacuum dried and concentrated to 8 times the mass of Oroxylum indica powder (v / w), that is, concentrated to a volume of 1.6L, and then centrifuged to discard the precipitate and collect the supernatant, wherein the centrifugal speed is 10000×g, the centrifugal time is 20min, the supernatant is passed through a mixed cellulose ester membrane (MCE membrane) with an average pore size of 5μm, and the filtrate is collected to obtain Oroxylum indica concentrate, wherein the mass fraction of ethanol in the Oroxylum indica concentrate is 20%, and the solid content of the Oroxylum indica concentrate is 2.0%.

[0079] The Oroxylum indica concentrate obtained above was dynamically adsorbed using 200 mL of LX-T83 resin column to obtain Oroxylum indica concentrate, wherein the column diameter-to-height ratio of the LX-T83 resin was 1:6, and the adsorption flow rate was 2 BV / h. After the adsorption was completed, 8 BV of deionized water was used to pass through the LX-T83 resin column in a forward direction at a flow rate of 2 BV / h to clean the LX-T83 resin column bed to remove some water-soluble impurities, and then 6 BV of 60% ethanol was used to pass through the LX-T83 resin column in a forward direction at a flow rate of 3 BV / h to collect the eluate.

[0080] The volume of 1.2L of the eluate is vacuum concentrated to 1.5 times the mass of the Oroxylum butterfly powder (v / w), that is, the volume is concentrated to about 300mL, to obtain a concentrated solution, wherein the solid content of the concentrated solution is 7%, and the mass fraction of ethanol in the concentrated solution is 15%. The concentrated solution is then spray-dried at an inlet temperature of 145°C to obtain a light yellow powder, that is, the Oroxylum butterfly extract as a skin oil-control active ingredient, wherein in the Oroxylum butterfly extract as a skin oil-control active ingredient, the mass fraction of oroxylin A is 26.98%, and the mass fraction of oroxylin B is 24.82%.

[0081] Example 3

[0082] Weigh 200g of Oroxylum indica powder produced in Vietnam and add it to a 70% ethanol solution by mass, heat it to 90°C for the first extraction, wherein the extraction time is 1.5h and the solid-liquid ratio is 1:20, to obtain a first extract; pass the first extract through a 200-mesh filter to obtain a first filtrate and a first filter residue; then add the first filter residue obtained above to a 60% ethanol solution by mass, and heat it to 85°C for a second extraction, wherein the second extraction time is 1.5h and the second solid-liquid ratio is 1:10, to obtain a second extract, then pass the second extract through a 200-mesh filter to obtain a second filtrate, then filter the first filtrate and the second filtrate respectively, and combine the filtrates to obtain the Oroxylum indica extract.

[0083] The volume of 5.4 L of Oroxylum indica extract is vacuum dried and concentrated to 11 times the mass of Oroxylum indica powder (v / w), that is, concentrated to a volume of 2.2 L, and then centrifuged to discard the precipitate and collect the supernatant, wherein the centrifugal speed is 10000×g, the centrifugal time is 20 min, the supernatant is passed through a mixed cellulose ester membrane (MCE membrane) with an average pore size of 5 μm, and the filtrate is collected to obtain Oroxylum indica concentrate, wherein the mass fraction of ethanol in the Oroxylum indica concentrate is 20%, and the solid content of the Oroxylum indica concentrate is 2.4%.

[0084] The Oroxylum indica concentrate obtained above was dynamically adsorbed using 200 mL of LX-T83 resin column to obtain Oroxylum indica concentrate, wherein the column diameter-to-height ratio of the LX-T83 resin was 1:8, and the adsorption flow rate was 4 BV / h. After the adsorption was completed, 10 BV of deionized water was passed through the LX-T83 resin column at a flow rate of 2 BV / h to clean the LX-T83 resin column bed to remove some water-soluble impurities, and then 8 BV of 60% ethanol was passed through the LX-T83 resin column at a flow rate of 3 BV / h to collect the eluate.

[0085] The volume of 1.6L of the eluate is vacuum concentrated to 1.5 times the mass of the Oroxylum butterfly powder (v / w), that is, the volume is concentrated to about 300mL, to obtain a concentrated solution, wherein the solid content of the concentrated solution is 7%, and the mass fraction of ethanol in the concentrated solution is 15%. The concentrated solution is then spray-dried at an inlet temperature of 145°C to obtain a light yellow powder, that is, the Oroxylum butterfly extract as a skin oil-control active ingredient, wherein in the Oroxylum butterfly extract as a skin oil-control active ingredient, the mass fraction of oroxylin A is 27.19%, and the mass fraction of oroxylin B is 24.52%.

[0086] Example 4

[0087] Weigh 200g of Oroxylum indica powder from Myanmar and add it to an ethanol solution with a mass fraction of 80%, heat it to 70°C for the first extraction, wherein the extraction time is 2h and the solid-liquid ratio is 1:20, to obtain a first extract; pass the first extract through a 200-mesh filter to obtain a first filtrate and a first filter residue; then add the first filter residue obtained above to an ethanol solution with a mass fraction of 80%, and heat it to 70°C for a second extraction, wherein the second extraction time is 2h and the secondary solid-liquid ratio is 1:10, to obtain a second extract, then pass the second extract through a 200-mesh filter to obtain a second filtrate, then filter the first filtrate and the second filtrate respectively, and combine the filtrates to obtain the Oroxylum indica extract.

[0088] The volume of 5.3 L of Oroxylum indica extract is vacuum dried and concentrated to 12 times the mass of Oroxylum indica powder (v / w), that is, concentrated to a volume of 2.4 L, and then centrifuged to discard the precipitate and collect the supernatant, wherein the centrifugal speed is 10000×g, the centrifugal time is 20 min, the supernatant is passed through a mixed cellulose ester membrane (MCE membrane) with an average pore size of 5 μm, and the filtrate is collected to obtain Oroxylum indica concentrate, wherein the mass fraction of ethanol in the Oroxylum indica concentrate is 20%, and the solid content of the Oroxylum indica concentrate is 2.4%.

[0089] The obtained Oroxylum indica concentrate was dynamically adsorbed using 200 mL of LX-T83 resin column to obtain Oroxylum indica concentrate, wherein the column diameter-to-height ratio of LX-T83 resin was 1:5, and the adsorption flow rate was 4 BV / h. After the adsorption was completed, 10 BV of deionized water was passed through the LX-T83 resin column at a flow rate of 2 BV / h to clean the LX-T83 resin column bed to remove some water-soluble impurities, and then 8 BV of 60% ethanol was passed through the LX-T83 resin column at a flow rate of 3 BV / h to collect the eluate.

[0090] The volume of 1.6L of the eluate is vacuum concentrated to 1 times the mass of the Oroxylum butterfly powder (v / w), that is, the volume is concentrated to about 200mL, to obtain a concentrated solution, wherein the solid content of the concentrated solution is 10%, and the mass fraction of ethanol in the concentrated solution is 15%. The concentrated solution is then spray-dried at an inlet temperature of 145°C to obtain a light yellow powder, that is, the Oroxylum butterfly extract as a skin oil-control active ingredient, wherein in the Oroxylum butterfly extract as a skin oil-control active ingredient, the mass fraction of oroxylin A is 26.75%, and the mass fraction of oroxylin B is 24.67%.

[0091] The Oroxylum butterfly extract as a skin oil control active ingredient prepared in Example 1 was used as an experimental sample for efficacy testing, as follows:

[0092] Experimental Example 1

[0093] In vitro oil control efficacy test

[0094] Experimental methods:

[0095] (1) Cytotoxicity of samples to human sebaceous gland cells (SZ95) was tested by MTT method

[0096] Experimental steps: Cell inoculation: Inoculate cells in a 96-well plate (5×10 3 / well), and cultured at 37°C, 5% CO2 for 24 hours. Grouped administration: the sample group was replaced with the culture medium containing the sample at the corresponding concentration, the normal control group was replaced with fresh culture medium, and the blank control group was replaced with blank culture medium. Three biological replicates were set up and incubated at 37°C, 5% CO2 for 24 hours; after the incubation, MTT solution was added to each well, and after continuing to culture for 4 hours, the culture medium was removed, DMSO solution was added, and the mixture was shaken and mixed. The absorbance value (OD) at 490nm was measured. 490 ), and the test results are shown in Table 2-1, where cell viability (%) = (OD 490样本组 -OD 490空白对照组 ) / (OD 490正常对照组 -OD 490空白对照组 )×100%.

[0097] (2) Lipid accumulation inhibition effect

[0098] Experimental steps: Cell inoculation: Human sebaceous gland cells (SZ95) were cultured at 1×10 5The cells / well were inoculated in a 12-well plate and cultured in an incubator (37°C, 5% CO2) for 24 h. A normal control group (0% sample), a model control group (0.0188 μM dihydrotestosterone (DHT) + 0% sample), a sample group (0.0188 μM DHT + 0.005% sample), and a positive control group (0.0188 μM dihydrotestosterone (DHT) + 50 μg / mL tetrandrine) were set up, and three biological replicates were set up.

[0099] Dihydrotestosterone (DHT) modeling + administration: After the cells adhered to the wall, according to the above grouping, the normal control group and the model control group were replaced with fresh culture medium, and the sample group was replaced with fresh culture medium containing samples, and treated with DHT to induce lipid synthesis. Then they were placed in a 37°C, 5% CO2 incubator for another 24 hours;

[0100] Sampling and detection: After incubation for 24 hours, discard the culture medium, wash twice with PBS, and fix with 4% paraformaldehyde at room temperature for 10 minutes. After fixation, stain with Nile red dye (100μg / mL) and incubate in a 37°C incubator for 10 minutes, remove the dye, and then wash three times with PBS. Observe the staining under a fluorescence microscope. Cells with strong orange-red fluorescence are lipid-rich positive cells. Nile red staining detects the lipid content in the cytoplasm of human sebaceous gland cells (SZ95).

[0101] The calculation formula is as follows: Inhibition rate (%) = (model control group - sample group) / model control group × 100%, and the calculation results are shown in Table 2-2, where C1-C5 in Table 2-1 represent sample concentrations (w / v%) in the culture medium of 0.00234%, 0.00469%, 0.00938%, 0.0188%, and 0.0376%, respectively. According to the cytotoxicity results, 0.005% was subsequently selected as the sample addition concentration for the oil secretion inhibition experiment.

[0102] Table 2-1 Cytotoxicity of samples from Example 1 to SZ95

[0103]

[0104] Table 2-2 Results of oil accumulation inhibition rate

[0105]

[0106] At the same time, the applicant also obtained the staining fluorescence comparison images of any three locations of the model control group, positive control group and sample group Example 1 samples under a fluorescence microscope, such as Figure 1 As shown, from Figure 1 It can be seen that the fluorescence intensity in the sample of Example 1 of the present invention is the weakest, indicating that the Oroxylum butterfly extract as a skin oil-control active ingredient in the present invention can significantly inhibit skin oil secretion.

[0107] Sebaceous glands are the source and target tissue of androgens. Dehydroepiandrosterone is produced in sebaceous glands and converted into the most active testosterone and 5α-dihydrotestosterone through a series of enzyme catalysis. They can stimulate the proliferation and differentiation of sebaceous gland cells and stimulate the synthesis of lipids. Combined with the data in Table 2, it can be seen that compared with the model control group, the oil secretion inhibition rate of the positive control group is 31%, and the oil secretion inhibition rate of the sample in Example 1 at a concentration of 0.005% reaches 24%. Therefore, this experiment established a model of excessive lipid secretion of human sebaceous gland cells (SZ95) induced by dihydrotestosterone (DHT). Based on the results of Nile red staining, it can be seen that compared with the model control group, the sample in Example 1 of the sample group can significantly inhibit oil accumulation at a concentration of 0.005%, reflecting the oil control effect.

[0108] Experimental Example 2

[0109] 5α-reductase inhibition assay

[0110] Experimental method: The experimental setting groups are shown in Table 3-1, where 1 mL of PBS solution was added to the blank control group, 1 mL of sample working solution was added to the sample group, 1 mL of finasteride working solution was added to the positive control group, and 1 mL of 5% ethanol was added to the enzyme tube.

[0111] Add 1 mL of enzyme solution, 1 mL of NADPH solution and 1 mL of testosterone solution into a test tube, set up 3 parallel tubes, shake gently, take 200 μL with a pipette and add it to a 96-well ELISA plate, put it into the ELISA reader for detection, and measure the absorbance at 340 nm as the first measurement value A0.

[0112] After incubation at 37°C for 30 minutes, the sample was placed in an ELISA reader and the absorbance at 340 nm was measured as the second measurement value A. 30 , and detected the 5α-reductase inhibition rate. The test results are shown in Table 3-2.

[0113] Where, 5α-reductase inhibition rate (%) = (1-(A 样品0 -A 样品30 ) / (A 酶0 -A 酶30 ))×100%, where A 样品0 The absorbance value of the first sample group (0min) is measured, A 样品30 The absorbance value of the second sample group (30min) is measured, A 酶0 A is the average absorbance of the first (0min) enzyme tube measurement. 酶30 It is the average value of absorbance measured in the enzyme tube for the second time (30min).

[0114] Table 3-1 Experimental group information

[0115]

[0116] Table 3-2 5α-reductase test results

[0117]

[0118]

[0119] Combined with Table 3-2, it can be seen that compared with the blank control group, the 5α-reductase inhibition rate of the positive control group is 41.69%, and the reductase inhibition rates of the sample in Example 1 at concentrations of 0.001%, 0.005%, and 0.01% are 12.03%, 17.02%, and 20.76%, respectively. 5α-reductase plays an important role in the regulation of sebum secretion. The enzyme is mainly responsible for converting testosterone in the body into more active dihydrotestosterone, which can accelerate the proliferation of sebaceous gland cells and sebum synthesis, thereby causing oily skin. Therefore, this experiment detected the enzyme inhibition rate of the sample at a given concentration and observed that: compared with the blank control, the sample in Example 1 showed significant inhibition of 5α-reductase activity in the concentration range of 0.001%-0.01%, and showed concentration dependence. This result reflects the oil control effect of the sample in Example 1.

[0120] Experimental Example 3

[0121] Inhibitory effects of lipid synthesis regulators

[0122] (1) The MTT method was used to detect the cytotoxicity of the samples to human sebaceous gland cells (SZ95). The experimental content was the same as that of Experimental Example 1.

[0123] (2) Expression of genes related to lipid synthesis regulation (PPARγ, FAS, SCD, SREBP-1c, IGF-1R, PLIN2)

[0124] Experimental steps: Cell inoculation: Human sebaceous gland cells (SZ95) were plated at 3×10 5 Each well was inoculated in a 6-well plate and cultured in an incubator (37°C, 5% CO2) for 24 h. A normal control group (0% sample), a model control group (0.0188 μM DHT+0% sample), and a sample group (0.0188 μM DHT+0.005% sample) were set up respectively. Corresponding positive control groups were set up for the detected genes, including 0.0188 μM dihydrotestosterone+0.0005 mg / mL clapristone, or 0.0188 μM dihydrotestosterone+0.078 μM AKT inhibitor, and three biological replicates were set up.

[0125] Modeling + drug administration: After the cells adhered to the wall, according to the above grouping, the normal control group was replaced with fresh culture medium, the model control group was replaced with fresh culture medium containing dihydrotestosterone, the sample group was replaced with fresh culture medium containing sample and dihydrotestosterone, the positive control group 1 was replaced with fresh culture medium containing clapriston and dihydrotestosterone, and the positive control group 2 was replaced with fresh culture medium containing AKT inhibitor and dihydrotestosterone. Then it was placed in a 37°C, 5% CO2 incubator for further incubation for 24 hours.

[0126] Sampling and detection: After 24 hours of incubation, the culture medium was discarded, and the cells were washed twice with D-Hanks. The total RNA of each experimental group was extracted, and cDNA was synthesized. The gene expression of β-actin and the target gene was detected by q-PCR. β-actin was used as the internal reference for gene expression to calculate the relative RNA expression of the target gene; where the relative RNA expression = 2 ΔΔC(t) , ΔΔC(t)=ΔC(t) 模型对照组 -ΔC(t) 样本组 , ΔC(t)=C(t) 目的基因 -C(t) (β-actin) The specific test results are shown in Tables 4-1 to 4-6, wherein Table 4-1 is the detection result of SREBP-1C gene expression, Table 4-2 is the detection result of FAS gene expression, Table 4-3 is the detection result of SCD gene expression, Table 4-4 is the detection result of IGF-1R gene expression, Table 4-5 is the detection result of PPARγ gene expression, and Table 4-6 is the detection result of PLIN2 gene expression.

[0127] Table 4-1 Detection results of SREBP-1C gene expression

[0128]

[0129] Table 4-2 Detection results of FAS gene expression

[0130]

[0131]

[0132] Table 4-3 Detection results of SCD gene expression

[0133]

[0134] Table 4-4 Detection results of IGF-1R gene expression

[0135]

[0136] Table 4-5 Detection results of PPARγ gene expression

[0137]

[0138]

[0139] Table 4-6 Detection results of PLIN2 gene expression

[0140]

[0141] Note: In Tables 4-1 to 4-6, P < 0.05 indicates a significant difference, and P < 0.01 indicates an extremely significant difference.

[0142] SREBP-1C is an important member of the sterol regulatory element binding protein family. It mainly selectively regulates the expression levels of fatty acid and triglyceride synthase genes. It is a key regulatory point in lipid metabolism, especially fatty acid metabolism. It regulates lipid synthesis in the body by regulating the gene expression of fat metabolism-related enzymes. Reduced SREBP-1C activity can inhibit the expression levels of key enzymes (FAS, SCD) involved in lipid synthesis, thereby controlling oil secretion; IGF-1R is a transmembrane receptor that plays a role in cell proliferation, differentiation, and transformation. It affects cell proliferation and differentiation, and these processes are also related to the function of sebaceous gland cells. The activation of IGF-1R can promote cell proliferation and growth through specific signal transduction pathways, such as MAPK and PI3K / AKT, which may indirectly increase the oil production of sebaceous cells. Therefore, downregulating the expression of IGF-1R can inhibit the excessive proliferation of sebaceous gland cells and achieve the purpose of oil control; PLIN2, as the second most abundant lipid droplet coating protein in sebaceous gland cells, is the main member regulated during cell differentiation. Experiments have reported that downregulation of PLIN2 in sebaceous gland cells significantly inhibits lipid accumulation. At the same time, PLIN2-deficient mice showed a significant reduction in sebaceous gland size, cell number, and cell proliferation; in addition, PPARγ activation can increase the expression level of the PLIN gene in adipocytes, and the expression level of PLIN determines the abundance of lipid droplets. Therefore, downregulating PPARγ can effectively inhibit the synthesis of lipid droplets.

[0143] Combining the data in Tables 4-1 to 4-6, it can be seen that based on human sebaceous gland cells (SZ95), compared with the model control group, the gene expression levels of fatty acid synthase (FAS), stearoyl-CoA desaturase (SCD), sterol regulatory element binding protein 1C (SREBP-1C), peroxisome proliferator-activated receptor (PPARγ), and lipid droplet envelope protein (PLIN2) in the sample of Example 1 at a concentration of 0.005% (w / v) were significantly downregulated, especially FAS, SCD, SREBP-1C, and PLIN2. Therefore, the oroxylin extract as a skin oil-control active ingredient in the present invention contains oroxylin A and oroxylin B in a specific mass ratio, which can better regulate the expression levels of genes related to lipid synthesis regulation and has an oil-control effect.

[0144] Experimental Example 4

[0145] Lipid peroxidation improvement effect

[0146] Experimental methods:

[0147] (1) Cytotoxicity of samples to human immortalized keratinocytes (HaCaT) was tested using the MTT method

[0148] Experimental steps: Cell inoculation: Inoculate cells in a 96-well plate (5×10 3 / well), and cultured at 37°C, 5% CO2 for 24 hours. Drug administration: The sample group was replaced with the culture medium containing the sample of the corresponding concentration, the normal control group was replaced with fresh culture medium, and the blank control group was replaced with blank culture medium. Three biological replicates were set up, and incubated at 37°C, 5% CO2 for 24 hours; after the incubation, MTT solution was added to each well, and after continuing to culture for 4 hours, the culture medium was removed, and DMSO solution was added, and the mixture was shaken and mixed. The absorbance value (OD) at 490nm was measured 490 ), and the test results are shown in Table 5-1, where cell viability (%) = (OD 490样本组 -OD 490空白对照组 ) / (OD 490正常对照组 -OD 490空白对照组 )×100%, wherein C1-C5 in Table 5-1 represent the sample concentrations (w / v%) in the culture medium of 0.00588%, 0.00117%, 0.00234%, 0.00469%, and 0.00938%, respectively.

[0149] (2) Effects of samples on the content of malondialdehyde (MDA) and lipid peroxide (LPO) in human immortalized keratinocytes (HaCaT) after lipopolysaccharide (LPS) modeling

[0150] Experimental steps: Cell seeding: Immortalized human keratinocytes (HaCaT) were cultured at 6×10 5Each well was inoculated into a 6-well plate and cultured in an incubator (37°C, 5% CO2) for 24 h. A normal control group (0% sample), a model control group (2.5 μg / mL LPS + 0% sample), a sample group (2.5 μg / mL LPS + 0.002% sample), and a positive control group (2.5 μg / mL LPS + 0.03% N-acetyl-L-cysteine) were set up, and three biological replicates were set up.

[0151] Drug administration + modeling: discard the culture medium in the 6-well plate and carry out the drug administration operation. Drug administration or LPS treatment is carried out according to the above grouping, 2mL per well. After the drug administration is completed, the 6-well plate is placed in an incubator (37°C, 5% CO2) and cultured for 24h±2h; Collect cells: After the culture is completed, collect cell samples for subsequent MDA and LPO content determination. The measurement results are shown in Tables 5-2 to 5-3, among which the malondialdehyde (MDA) test kit and lipid peroxide (LPO) test kit are from Nanjing Jiancheng Biotechnology Co., Ltd., and the detection method refers to the corresponding instructions. Table 5-2 shows the effect of the sample on the MDA content of human immortalized keratinocytes (HaCaT) after LPS modeling, and Table 5-3 shows the effect of the sample on the LPO content of human immortalized keratinocytes (HaCaT) after LPS modeling.

[0152] Table 5-1 Toxicity of samples in Example 1 to HaCaT cells

[0153]

[0154] Table 5-2 Test results of MDA content

[0155]

[0156] Table 5-3 Test results of LPO content

[0157]

[0158] It can be seen from Table 5-1 that, based on the cytotoxicity results, 0.002% was subsequently selected as the sample addition concentration for the oil secretion inhibition experiment. At the same time, it can be seen from the data in Tables 5-2 and 5-3 that, compared with the model control group, the sample in Example 1 significantly reduced the content of lipid peroxides (LPO) and malondialdehyde (MDA) in the cells at a concentration of 0.002% (w / v). Among them, lipid peroxide LPO is a peroxide formed by unsaturated fatty acids in the body under the action of free radicals. The decomposition of lipid peroxide LPO can produce MDA. The changes in the content of LPO and MDA can reflect the inhibitory effect of the sample on lipid peroxidation. Therefore, the experimental results show that the Oroxylum indica extract in Example 1 of the present invention as a skin oil control active can significantly inhibit the generation of lipid peroxidation products, improve the lipid peroxidation state, and help alleviate the irritation problem caused by lipid peroxidation on the skin surface.

[0159] Experimental Example 5

[0160] In vitro inflammatory mediator inhibition efficacy

[0161] Experimental methods:

[0162] (1) MTT method was used to detect the cytotoxicity of samples to mouse mononuclear macrophages (Raw264.7)

[0163] Experimental steps: Cell inoculation: Inoculate cells in a 96-well plate (5×10 3 / well), and cultured at 37°C, 5% CO2 for 24 hours. Drug administration: The sample group was replaced with the culture medium containing the sample of the corresponding concentration, the normal control group was replaced with fresh culture medium, and the blank control group was replaced with blank culture medium. Three biological replicates were set up, and incubated at 37°C, 5% CO2 for 24 hours; after the incubation, MTT solution was added to each well, and after continuing to culture for 4 hours, the culture medium was removed, and DMSO solution was added, and the mixture was shaken and mixed. The absorbance value (OD) at 490nm was measured 490 ), and the test results are shown in Table 6-1, where cell viability (%) = (OD 490样本组 -OD 490空白对照组 ) / (OD 490正常对照组 -OD 490空白对照组 )×100%, wherein C1-C5 in Table 6-1 represent the sample concentrations (w / v%) in the culture medium of 0.000147%, 0.000294%, 0.000588%, 0.00117%, and 0.00234%, respectively.

[0164] (2) Effects of samples on PGE2 content in Raw264.7 after LPS modeling

[0165] Experimental steps: Cell seeding: Raw264.7 was plated at 3×10 5Each well was inoculated into a 6-well plate and cultured in an incubator (37°C, 5% CO2) for 24 h. A normal control group (0% sample), a model control group (0.5 μg / mL LPS + 0% sample), a sample group (0.5 μg / mL LPS + 0.0003% / 0.001% sample), and a positive control group (0.5 μg / mL LPS + 0.01% dexamethasone) were set up, and three biological replicates were set up.

[0166] LPS modeling + drug administration: According to the experimental groups, the modeling and drug administration groups were treated with a certain final concentration of LPS and drugs for 24h±2h; Cell supernatant collection: After the incubation, the cell culture supernatant was collected in a 1.5mL sterile centrifuge tube, and the PGE2 test kit was used. The kit was purchased from Enzo Biochemical Co., Ltd. ADI-900-001, and the test was performed according to the operating instructions of the kit. The test results are shown in Table 6-2.

[0167] Table 6-1 Cytotoxicity of samples from Example 1 to Raw264.7 cells

[0168]

[0169] Table 6-2 Test results of PGE2 content

[0170]

[0171] Combined with Table 6-1, it can be seen that according to the cytotoxicity results, 0.0003% and 0.001% were subsequently selected as sample addition concentrations for the oil secretion inhibition experiment. Combined with the data in Table 6-2, it can be seen that based on the LPS-induced Raw264.7 cell model, compared with the model control group, the Oroxylum butterfly extract in the sample of Example 1 significantly reduced the content of the inflammatory mediator PGE2 at the action concentrations of 0.0003% and 0.001%, indicating that the Oroxylum butterfly extract as a skin oil control active in Example 1 of the present invention can significantly inhibit the generation of the inflammatory mediator PGE2 and has an excellent soothing effect.

[0172] Application Example 1: Oil Control Moisturizing Lotion

[0173] The preparation method is as follows: (Note: during the preparation process, ensure that all equipment and containers are clean and dry), put all the raw materials of phase A (such as phase A01-A11 raw materials in Table 7) into the operating container, heat to 80°C, and stir until completely uniform; put all the raw materials of phase B (such as phase B01-B08 raw materials in Table 7) into the operating container, heat to 78°C, and stir until completely uniform; put phase B into phase A, mix and stir evenly, and cool to 65°C; add the pre-mixed phase C raw materials (such as phase C01-C02 raw materials in Table 7), stir until completely uniform, and cool to 38°C; add phase D raw materials (such as phase D01-D03 raw materials in Table 7) in sequence, stir until completely uniform, and obtain an oil-control moisturizing lotion.

[0174] Table 7 Oil Control Moisturizing Lotion Formula

[0175]

[0176] Application Example 2: Oil Control Moisturizing Essence

[0177] Preparation method: (Note: during the preparation process, ensure that all equipment and containers are clean and dry. Put all the raw materials of phase A (such as the raw materials of phase A01-A12 in Table 8) into the operating container, heat to 80°C, stir until completely uniform, and cool to 65°C; add the pre-mixed phase B (such as the raw materials of phase B01-B02 in Table 8), stir until completely uniform; cool to 38°C; add the raw materials of phase C (such as the raw materials of phase C01-C03 in Table 8) in sequence, stir until completely uniform, and obtain the oil-controlling moisturizing essence.

[0178] Table 8 Oil Control Moisturizing Essence Formula

[0179]

[0180] The above-mentioned embodiments only express several implementation methods of the present invention, and the descriptions thereof are relatively specific and detailed, but they cannot be understood as limiting the scope of the invention patent. It should be pointed out that, for ordinary technicians in this field, several variations and improvements can be made without departing from the concept of the present invention, and these all belong to the protection scope of the present invention. Therefore, the protection scope of the patent of the present invention shall be subject to the attached claims.

Claims

1. An Oroxylum indica extract as a skin oil control active ingredient, characterized in that: The invention at least comprises the following components in percentage by mass: 25%-35% of oroxylin A and 20%-35% of oroxylin B.

2. The method for preparing the Oroxylum indica extract as a skin oil-control active ingredient according to claim 1, characterized in that: The steps include: A. Using ethanol to heat and reflux extract the Oroxylum butterfly powder, and then filtering to obtain the Oroxylum butterfly extract; B. Concentrating the volume of the Oroxylum indica extract to 8 to 12 times the mass of the Oroxylum indica powder, obtaining a supernatant by centrifugation, and filtering the supernatant to obtain an Oroxylum indica concentrate; C. enriching the Oroxylum indica concentrate by a macroporous adsorption resin column, and then introducing an eluent to elute, to obtain an eluent, wherein the flow rate of the Oroxylum indica concentrate is 2BV / h-4BV / h, and the flow rate of the eluent is 1BV / h-3BV / h; D. Concentrating the volume of the eluate to 1 to 1.5 times the mass of the Oroxylum indica powder, and then spray drying the eluate to obtain the Oroxylum indica extract as a skin oil-control active ingredient.

3. The method for preparing the Oroxylum indica extract as a skin oil-control active ingredient according to claim 2, characterized in that: The oroxylum butterfly powder is subjected to two heating reflux extractions with 50%-80% ethanol by mass, wherein the temperature of each reflux extraction is 70°C-90°C, the extraction time is 1h-3h, the solid-liquid ratio is 1:10-1:30, and the mixture is filtered with a 100-300 mesh filter, and the filtrate is finally combined to obtain the oroxylum butterfly extract.

4. The method for preparing the Oroxylum indica extract as a skin oil-control active ingredient according to claim 2, characterized in that: The mass fraction of ethanol in the Oroxylum indica concentrated solution is 5%-30%, and the solid content of the Oroxylum indica concentrated solution is 2.0%-3.0%; And / or, in the step of obtaining the supernatant by centrifugation, the centrifugal speed is 8000×g-10000×g, and the centrifugal time is 10 min-20 min; And / or, in the step of filtering the supernatant, the pore size of the filter membrane is 1 μm-5 μm, and the filter membrane is selected from any one of a mixed cellulose ester membrane, a polyethersulfone membrane, and a nylon membrane.

5. The method for preparing the Oroxylum indica extract as a skin oil-control active ingredient according to claim 2, characterized in that: In the step of introducing the eluent for elution, the macroporous adsorption resin column is first cleaned with deionized water to remove impurities, the flow rate of deionized water is 2BV / h-4BV / h, and the flow rate of deionized water is 8BV-10BV; then, an ethanol solution with a mass fraction of 50%-80% is used for analysis, and the flow rate of the ethanol solution is 4BV-8BV to obtain an eluent.

6. The method for preparing the Oroxylum indica extract as a skin oil-control active ingredient according to claim 5, characterized in that: The volume of the eluate is concentrated to 1 to 1.5 times the mass of the Oroxylum indica powder to obtain a concentrated solution, wherein the solid content of the concentrated solution is 7% to 15%, and the mass fraction of ethanol in the concentrated solution is 2% to 15%.

7. The method for preparing the Oroxylum indica extract as a skin oil-control active ingredient according to claim 2, characterized in that: The macroporous adsorption resin in the macroporous adsorption resin column has a column diameter-to-height ratio of 1:4-1:8, and the macroporous adsorption resin skeleton is styrene-divinylbenzene and / or divinylbenzene.

8. The method for preparing the Oroxylum indica extract as a skin oil-control active ingredient according to claim 7, characterized in that: The macroporous adsorption resin is selected from LX-T83.

9. Application of Oroxylum butterfly extract as skin oil-control active ingredient in oil-control functional cosmetics.

10. The use according to claim 9, characterized in that: The mass fraction of the Oroxylum indica extract as the skin oil-control active ingredient in the oil-control functional cosmetic is 0.001%-0.2%.

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