WO2019137387A1 - 具有美白亮肤功效的外用植物提取物、化妆品及其制备方法 - Google Patents

具有美白亮肤功效的外用植物提取物、化妆品及其制备方法 Download PDF

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WO2019137387A1
WO2019137387A1 PCT/CN2019/070952 CN2019070952W WO2019137387A1 WO 2019137387 A1 WO2019137387 A1 WO 2019137387A1 CN 2019070952 W CN2019070952 W CN 2019070952W WO 2019137387 A1 WO2019137387 A1 WO 2019137387A1
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extraction
solvent
whitening
plant extract
lightening effect
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PCT/CN2019/070952
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English (en)
French (fr)
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董银卯
孟宏
刘宇红
曲召辉
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北京东方淼森生物科技有限公司
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/92—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
    • A61K8/922—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00—Preparations for care of the skin
    • A61Q19/02—Preparations for care of the skin for chemically bleaching or whitening the skin
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00—Preparations for care of the skin
    • A61Q19/08—Anti-ageing preparations
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/52—Stabilizers
    • A61K2800/522—Antioxidants; Radical scavengers
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/59—Mixtures
    • A61K2800/592—Mixtures of compounds complementing their respective functions
    • A61K2800/5922—At least two compounds being classified in the same subclass of A61K8/18
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/805—Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95

Definitions

  • the present invention relates to a topical plant extract, in particular to a topical plant extract having whitening and skin lightening effect and a cosmetic prepared from the plant extract.
  • Whitening products have always been the mainstream beauty skin care products. Most whitening agents cut off the downstream pathway of melanin synthesis by selectively inhibiting tyrosinase activity to achieve a whitening effect. However, existing whitening agents, such as hydroquinone, have certain cytotoxicity, and local overdose can cause melanocyte death, which is manifested by white spots on the skin. How to obtain a natural safe and efficient plant whitening product is a hot spot for researchers in the field.
  • Plant extracts have many advantages as cosmetic additives, such as natural, low irritation and excellent efficacy of plant extracts. Therefore, plant extracts are increasingly used as cosmetic additives in cosmetics.
  • the functional ingredients in plant raw materials include oil-soluble components such as fatty acids, sterols, lignans, esters, polyenes, pyrrole derivatives, ketones, anthracenes, etc., in addition to sugars, amino acids, Non-oil soluble substances such as proteins.
  • the main reasons for the application of plant extracts in the field of cosmetics are (1) the extraction efficiency is too low. Due to the characteristics of plant materials, the extraction efficiency is too low, resulting in an increase in extraction costs. Therefore, many companies prefer low-cost synthetic chemical materials. Replace natural plant materials to increase economic efficiency.
  • the flower soaking oil has a long history of application. Ancient Egyptians and ancient Greeks have learned to absorb the smell of petals and herbs with oils and used them as medicines or cosmetics. Soaking oil is commonly used as a solvent for vegetable oil. The ratio of raw material to oil is about 1:3 (v/v). Soaking at room temperature requires repeated feeding for 2 to 3 times. The soaking time takes 1 to 3 months. Soaking oil has good compatibility when used in cosmetic oil dosage form, but this method has low extraction efficiency and long extraction time is not conducive to industrial production.
  • Solvent extraction is a common method for producing plant extracts, generally using ethanol, acetone, chloroform or the like as a solvent, and has the characteristics of simple equipment and high extraction rate.
  • the extract prepared by the method has high requirements on cosmetic dosage forms, and is not suitable for being added to all dosage forms, especially in oil-based cosmetics, so that the plant extracts may precipitate after being added into the pure oil cosmetic. It seriously affects the quality of the product and restricts its application in pure oil-based cosmetics.
  • Supercritical extraction is a new technology that has emerged in recent years.
  • supercritical fluid When supercritical fluid is extracted, it is generally supercritical CO 2 , which has the advantages of non-toxic and harmless, high extraction rate and high purity of extract.
  • the equipment is complicated, the input cost is high, and the extraction cost is high, which limits the industrial mass production.
  • the extract obtained by supercritical extraction generally has poor compatibility with oil and fat, which affects its application in oil-based cosmetics.
  • a second object of the present invention is to provide a method for preparing a plant extract having high extraction efficiency and stable extract properties.
  • a third object of the present invention is to provide a cosmetic prepared from the above plant extract.
  • composition selected by the invention utilizes the principle of "Jun, Chen, Zuo, Zhi" to combine eight plants, and combines the improvement of the preparation method to obtain an efficient plant whitening extraction. Things.
  • a topical plant extract having whitening and skin lightening effect wherein the plant extract is prepared from the following raw materials by weight ratio by the following method:
  • the solvent used in the present invention is a mixture of one or more of ethanol, chloroform and acetone.
  • the ratio of material to liquid and extraction temperature have a crucial influence on extraction efficiency and extraction cost.
  • the selection of the physicochemical properties of extraction solvent 1 and its more matching ratio of material to liquid and extraction parameters can not only improve the extraction efficiency, but also enhance the solvent with the next step.
  • the synergy of the two extractions In the present invention, the plant material is more fully contacted with the solvent than the solvent, and the active ingredient in the plant material is more easily extracted, the extraction efficiency is higher, the solvent and the plant material are not wasted, and the extraction cost is more economical.
  • the first extraction liquid to liquid ratio range is from 1:10 to 50 m/m, the extraction effect is better in this range, and the synergy with solvent two is stronger.
  • the extraction temperature and time of the present invention are preferably 0.5 to 2 hours under the condition of 40 to 90 °C.
  • the extraction temperature and time directly affect the properties of the extract. Inappropriate extraction temperature and time may cause oxidative degeneration of plant raw materials, loss of volatile components and changes in the properties of heat-sensitive components during the extraction process.
  • the solubility and material exchange rate are the best, and the extract is excellent and stable.
  • condition parameter of the above step (2) is more suitable for the following step (3), and the synergistic effect can be produced with the step (3).
  • the solvent used in the present invention is a mixture of one or more of the following raw materials, respectively: white oil, kinematic viscosity (40 ° C) ⁇ 30 cSt, white oil 3 #, 5 #, 7 #, 10 #, is recommended.
  • Vegetable oil is recommended to be a mixture of one or more of soybean oil, sunflower seed oil, sesame oil, macadamia nut oil, sweet almond oil, olive oil, grape seed oil, oat oil, and tea oil.
  • the combination of solvent 2 and solvent 1 is particularly important for the technical effect of the present invention.
  • the inventors have verified by experiments that the two solvents are not completely mutually soluble, and the mutual solubility can ensure better extraction efficiency, but the stability is not good when added to cosmetics. Adverse conditions such as precipitation and precipitation occur.
  • the two solvents are also not completely miscible, and the two solvents are not mutually soluble, which does not play a synergistic effect, the extraction efficiency is very low and the stability of the extract is poor. Therefore, the solvent- and solvent-based two-part solution technology is the best.
  • the inventor controls the temperature and time of the second extraction within the above-mentioned conditional parameters, which can not only improve simultaneously.
  • the extraction effect of the mutual extraction of the solvent one and the solvent part can also effectively avoid the problems that the extraction efficiency tends to slowly increase the extraction cost.
  • the extraction temperature should not be too high, and the control should be optimal below 90 °C, and the temperature should not be too low. Below 40 °C, the solubility of the functional ingredient in the solvent 2 and the compatibility of the solvent one with the solvent two are affected. In turn, the extraction efficiency is affected.
  • the choice of solvent one and solvent two is particularly important.
  • the synergistic effect of the two needs to improve the extraction efficiency of plant raw materials, and in order to adapt to industrial production, the extraction process needs to be short, and the quality of the extract needs to be high, that is, the stability of addition.
  • the extraction cost also needs to be lower. Therefore, the inventors of the present invention have experimentally verified that if the solvent of the present invention is more polar than solvent one, the extraction efficiency and the stability of the extract are both poor.
  • the solvent one and the solvent two can be partially miscible under certain conditions, which can enhance the solubility of the active ingredient in the solvent two, so that some of the original is insoluble in the oil. Or a substance having poor solubility in fats and oils can be well dissolved in the solvent 2.
  • the combination of the two can meet all the conditions required for the extraction of the above-mentioned cosmetic plant raw materials, greatly improve the extraction efficiency of the plant active ingredients, and the obtained extract has stable properties and is excellent in compatibility with other raw materials of cosmetics.
  • the present invention may select one of the above-mentioned various solvents for single solvent extraction, or may perform multi-solvent compound extraction according to the actual extracted plant material characteristics, and the ratio between the solvents may be based on the experience or actual experience of those skilled in the art. It needs to be compounded in any proportion, and there is no specific limit. Because of the nature of the solvent two, water has a great influence on the stability of the solvent 2. Therefore, the solvent is preferably a water-free system, and ethanol is exemplified, preferably anhydrous ethanol.
  • the solvent 2 of the invention selects an extraction solvent which is weaker than the solvent, mild and non-irritating, and has good compatibility with the functional ingredients in the plant material.
  • Solvent 2 may be selected from one of the above-mentioned solvents to carry out single solvent extraction, or may be subjected to multi-solvent compound extraction according to the characteristics of the actually extracted plant material.
  • the ratio between the solvents may be based on the experience or actual experience of those skilled in the art. It needs to be compounded in any proportion, and there is no specific limit.
  • the second extraction liquid in the above step (3) preferably has a range of 1:10 to 50 m/m.
  • solvent removal a solvent-removable method known to those skilled in the art can be applied thereto.
  • the preferred method recommended in the present invention is: concentrated at 40-80 ° C under reduced pressure to a solvent, completely removed, and the reduced pressure range is generally Control from 0.01Mpa to minus 0.15Mpa.
  • the solvent may have some irritation to the skin. Removing the solvent can make the product performance milder, safe and has no toxic side effects.
  • the solvent can also be removed by membrane concentration, ultrafiltration, reverse osmosis, pervaporation or the like.
  • Fine filtration to clarification the purpose of this step is to make the final extract more stable and clarified, and the fine filtration process uses a filter plate having a pore size of 0.2 to 10 ⁇ m for filtration.
  • a coarse filtration step can also be added between the step (3) and the step (4).
  • the condition is a coarse filtration of 60 to 100 mesh, and the raw material slag is filtered off.
  • the cooling step can be added before the coarse filtration, and the slurry is cooled to 40 ° C or below and the coarse filtration is optimal.
  • the plant material can also be pretreated before the first extraction.
  • the purpose of the pretreatment is to make the extraction solvent more easily penetrate the cell wall and further improve the extraction efficiency.
  • the pretreatment step is not essential, and the high extraction rate of the present invention mainly depends on the combination of the solvent one and the solvent two and the process steps and parameters used for the solvent one, and the pretreatment can be based on the extraction rate achieved by the present invention.
  • the extraction time is further shortened, but the pretreatment step may not be used for the plant material which is not convenient for pretreatment.
  • the steps of the pretreatment recommended by the inventors are as follows, and other steps known to those skilled in the art that can achieve the purpose of pretreatment can also be applied thereto.
  • (1) coarse pulverization the raw material is pulverized to 20 to 60 mesh; the pulverizing step can be carried out by using a pulverizing device known in the art, such as a cutting machine, a wall breaking machine, a pulverizer, etc., and the pulverizing step can be completed in one step or in steps. It is completed step by step from coarse to fine.
  • a pulverizing device known in the art, such as a cutting machine, a wall breaking machine, a pulverizer, etc.
  • the high temperature described here is generally at least equal to or higher than 100 ° C, and the case is preferably controlled at 100 to 130 ° C.
  • the high pressure refers to 0.1Mpa or more, and the control is best in the range of 0.1 ⁇ 0.2Mpa.
  • the processing time should not be too long, and the control should be within 30 minutes.
  • the main components of the plant cell wall are cellulose and pectin.
  • the invention adopts high temperature and high pressure pretreatment raw materials, which utilizes water vapor to destroy the hydrogen bond between the polysaccharide molecules, so that the cell wall structure is loose, which is more favorable for the solvent to penetrate through the cell wall in the subsequent extraction process. To make the extraction efficiency better.
  • drying and drying are to remove excess water vapor after high temperature and high pressure, which is more conducive to the progress of the later extraction process and the stability of the extract. In this case, it is better to dry at 50 to 80 ° C for 1 to 2 hours. Other drying means known to those skilled in the art can also be applied thereto.
  • the above plant extract is used in the preparation of a cosmetic having a whitening and lightening effect.
  • a cosmetic having a whitening and lightening effect wherein the cosmetic is made of the above-mentioned plant extracts and excipients commonly used in the field of cosmetics.
  • a cosmetic having a whitening and lightening effect wherein the cosmetic is made of the following raw materials by weight ratio:
  • a method for preparing the above cosmetic product characterized in that the steps of the preparation method are as follows:
  • the above method can prepare an oil-based cosmetic, and other dosage forms such as an emulsion, a cream, a toner, a facial mask or a facial cleanser can be prepared by using the plant extract and the conventional methods and accessories in the field of skin care products.
  • the recommended method of use of the preparation of the invention is as follows: applying the method to the surface of the human skin by a smear method, and gently massage until absorbed.
  • the invention utilizes the combination of peony, perilla, linseed, buckwheat, lotus seed, medlar, milk thistle and licorice and gives the best compatibility amount, and the synergistic effect between the components is combined with the invention.
  • the new method of effectively extracting cosmetic plant raw materials by different polar solvents can greatly improve the skin whitening effect.
  • the method of the invention optimizes the extraction step and the extraction condition parameters according to the optimization of the extraction solvent and the selection of the specific solvent, so that the extraction efficiency of the plant raw material is greatly increased, and the plant extraction efficiency is evaluated mainly by the antioxidant and anti-inflammatory effects of the plant material.
  • the main effects of the plant extract added by cosmetics are also the above two types.
  • the extract obtained by the method of the present invention can be seen by the efficacy test that the extracts obtained by the prior art are far superior to the extracts obtained by the prior art.
  • the extraction method of the present invention effectively shortens the extraction time, the extraction efficiency is high, the equipment used is conventional and low, and the preparation cost of the plant extract is effectively reduced, and the present invention is very suitable for large-scale industrial production.
  • the plant extract obtained in this case is more stable, and has better compatibility with various cosmetic formulations, especially in the addition of oil-based cosmetics, which effectively improves the precipitation and precipitation of the prior art extracts.
  • the defects that affect the quality and efficacy of the product make the cosmetics easier to store and transport, the product quality is better, and the effect is better when used.
  • Figure 1 is a graph showing the extraction efficiency of samples 1 to 24 by DPPH clearance rate
  • Figure 3 is a graph showing the extraction effect of samples 31 to 36 by DPPH clearance rate
  • Figure 4 is a graph showing the DPPH clearance rate evaluation of the group screening experiment
  • Fig. 5 is a graph showing the evaluation of melanin synthesis inhibition rate in the panel screening test.
  • each solvent used in the solvent of the present embodiment is an anhydrous solvent.
  • the following examples are not to be construed as limiting the scope of the invention in any way.
  • Peony 3g perilla 5g, linseed 10g, buckwheat 1g, lotus seed 5g, wolfberry 10g, milk thistle 8g, licorice 1g;
  • the filter plate has a pore size of 10 ⁇ m and is finely filtered until the filtrate is clarified.
  • Peony 10g perilla seed 1g, linseed 5g, buckwheat 6g, lotus seed 1g, wolfberry 4g, silymarin 5g, licorice 6g;
  • the filter plate has a pore size of 1 ⁇ m and is finely filtered until the filtrate is clarified.
  • the filter plate has a pore size of 0.2 ⁇ m, and is finely filtered until the filtrate is clarified.
  • the filter plate has a pore size of 0.2 ⁇ m, and is finely filtered until the filtrate is clarified.
  • Peony 7g perilla seed 7g, linseed 3g, buckwheat 3g, lotus seed 4g, wolfberry 4g, milk thistle 6g, licorice 6g;
  • the filter plate has a pore size of 10 ⁇ m and is finely filtered until the filtrate is clarified.
  • Peony 6g perilla seed 6g, linseed 6g, buckwheat 6g, lotus seed 9g, hazelnut 2g, silymarin 2g, licorice 1g;
  • the filter plate has a pore size of 6 ⁇ m, and is finely filtered until the filtrate is clarified.
  • Peony 3g perilla seed 7g, linseed 3g, buckwheat 9g, lotus seed 9g, medlar 3g, silymarin 7g, licorice 10g;
  • the filter plate has a pore size of 2 ⁇ m and is finely filtered until the filtrate is clarified.
  • Second extraction adding soybean oil according to a ratio of material to liquid of 1:25 m/m, stirring and extracting at 65 ° C for 1 h;
  • the filter plate has a pore size of 4 ⁇ m, and is finely filtered until the filtrate is clarified.
  • Second extraction adding sesame oil according to a ratio of material to liquid of 1:100 m/m, stirring and extracting at 65 ° C for 2 h;
  • the filter plate has a pore size of 8 ⁇ m and is finely filtered until the filtrate is clarified.
  • Peony 7g perilla 5g, linseed 7g, buckwheat 5g, lotus seed 7g, hazelnut 5g, silymarin 7g, licorice 5g;
  • the first extraction adding a mixed solvent of chloroform and acetone according to a ratio of material to liquid of 1:40 m/m (combined with a mass ratio of 1:1), mixing, and extracting at 90 ° C for 1 h;
  • Second extraction adding octanoic acid/capric triglyceride and hydrogenated polydecene (17cSt) compound according to a ratio of material to liquid of 1:40 m/m (the two are compounded according to a mass ratio of 1:1). Stirring at 80 ° C for 1 h;
  • the first extraction adding a mixed solvent of ethanol and acetone according to a ratio of material to liquid of 1:45 m/m (combined according to 1:1), mixing, and extracting at 80 ° C for 1 h;
  • Second extraction adding olive oil and macadamia nut oil compound according to the ratio of material to liquid 1:40 m/m (the two are compounded according to the mass ratio of 1:1), and stirring and extracting at 60 ° C for 1.5 h;
  • Peony 3g perilla 5g, linseed 3g, buckwheat 4g, lotus seed 2g, wolfberry 8g, milk thistle 8g, licorice 3g;
  • the first extraction adding a mixed solvent of chloroform and ethanol according to a ratio of material to liquid of 1:20 m/m (combined with a mass ratio of 1:1), mixing, and extracting at 80 ° C for 2 h;
  • Second extraction a mixed solvent of white oil (16 cSt) and hydrogenated polyisobutylene (11 cSt) was added according to a ratio of material to liquid of 1:60 m/m (the two were compounded according to a mass ratio of 1:1), at 70 ° C. Stirring extraction for 1.5h;
  • Peony 10g perilla 3g, linseed 3g, buckwheat 5g, lotus seed 5g, medlar 7g, silymarin 7g, licorice 7g;
  • Second extraction adding grape seed oil and oat oil mixed solvent according to the ratio of material to liquid 1:50 m/m (the two are compounded according to the mass ratio of 1:1), and stirring and extracting at 50 ° C for 1.5 h;
  • Peony 7g perilla seed 10g, linseed 6g, buckwheat 2g, lotus seed 4g, wolfberry 6g, silymarin 2g, licorice 10g;
  • Second extraction adding sweet almond oil according to the ratio of material to liquid 1:20 m/m, stirring and extracting at 45 ° C for 1 h;
  • Example 16 oil-based cosmetic having whitening and skin-lightening effect
  • Example 17 oil-based cosmetic having whitening and skin-lightening effect
  • Example 18 Oil-based cosmetic having whitening and skin-lightening effect
  • the combination of the solvent one and the solvent two of the invention, combined with the optimized extraction process and extraction parameters of the invention, can synergistically enhance the effect, so that the extraction rate is higher, the extract property is more excellent and stable, and the extraction cost is lower, suitable Industrial application.
  • Solvent one is commonly used in plant extraction, with good compatibility with various active ingredients, high extraction rate and representative solvent; considering the experimentally confirmed solvent polarity should be greater than solvent 2 extraction, the final determination It is ethanol, acetone and chloroform. The inventor believes that the above technical effects have reached the requirements of the present case, so that it is no longer necessary to perform further solvent-one screening, which is also to reduce the workload when the solvent is selected.
  • Solvent 2 selects a solvent having a polarity lower than that of solvent one, and preferably a grease.
  • Vegetable oil The properties of each vegetable oil are similar, so only one of them is representative, and the three solvents of solvent one are combined and extracted, which have good effects;
  • White oil Select two kinds of white oils within the range of defined viscosity and outside the range (generally the values near the critical value, such as 26 and 32), respectively, and extract them with three solvents of solvent one, within the viscosity range. The effect of white oil is good, and the effect outside the range is not good;
  • Isostearyl isostearate compounded with three solvents of solvent one, which have good effects;
  • Silicone oil is a silicon chain, which has a poor dissolution effect on the active components of the carbon chain, and is compounded with a solvent, and the extraction effect is not good.
  • the above is the experimental idea of the solvent screening section, that is, the samples 1 to 24 of the solvent selection section.
  • the materials and preparation methods of the samples 1 to 24 were the same except that the extraction solvent was different.
  • the specific preparation method is as follows:
  • This part is the screening of solvent two, the solvent is fixed to ethanol, chloroform, acetone.
  • DPPH scavenging free radical experiment the composition of plant extract is complicated, and it is difficult to analyze and quantify the active ingredient of the extract. Therefore, those skilled in the art can evaluate the efficiency of extracting active ingredients by detecting the activity of antioxidant activity, and the extraction efficiency is good.
  • the extract prepared by the process has more excellent antioxidant activity.
  • Antioxidant activity is generally evaluated by DPPH free radical scavenging experiments.
  • DPPH (2,2-biphenyl-1-picrylhydrazyl) is a stable organic nitrogen radical which is widely used in the study of antioxidant capacity in vitro. Based on DPPH, there is a characteristic absorption peak at around 515 nm.
  • the antioxidant provides a hydrogen atom to reduce the single electron on the DPPH to reduce the color, and the degree of radical removal is evaluated according to the amount of decrease in absorbance.
  • Samples 1 to 3 are vegetable oils (the vegetable oils are similar in nature, only sunflower seed oil is taken as an example), and the mixture is extracted with the solvent, and the vegetable oil is compounded with ethanol, acetone and chloroform, and has good extraction effects.
  • Samples 4 to 6 were obtained by combining octanoic acid/capric triglyceride with ethanol, acetone and chloroform, respectively.
  • Samples 7 to 9 are isostearyl isostearate and ethanol, acetone and chloroform, respectively, and have good extraction effects.
  • Samples 10 to 12 are white oil (26 cSt, which meets the requirements of the present invention for kinematic viscosity ⁇ 30 cSt), and are extracted with ethanol, acetone and chloroform, respectively, and have good extraction effects.
  • Samples 13 to 15 are white oil (32 cSt, which does not meet the requirements of the present invention for kinematic viscosity ⁇ 30 cSt), and are extracted with ethanol, acetone and chloroform, respectively, and the extraction effects are poor.
  • Samples 10 to 15 are white oils with kinematic viscosity ⁇ 30 cSt, compared with white oil with kinematic viscosity > 30 cSt. The reason for selecting kinematic viscosity ⁇ 30 cSt white oil is explained by the difference in extraction effect.
  • Samples 16 to 18 are hydrogenated polydecene (30 cSt, which meets the requirements of the present invention for kinematic viscosity ⁇ 30 cSt), which are extracted with ethanol, acetone and chloroform, respectively, and have good extraction effects.
  • Samples 19 to 21 are hydrogenated polydecene (46 cSt, which does not meet the requirements of the present invention for kinematic viscosity ⁇ 30 cSt), and are extracted with ethanol, acetone, and chloroform, respectively, and the extraction effects are poor.
  • Samples 16 to 21 are similar to white oil. They are hydrogenated polydecene with kinematic viscosity ⁇ 30 cSt, which is compared with the kinematic viscosity > 30 cSt. The difference in extraction effect indicates the reason for selecting kinematic viscosity ⁇ 30 cSt hydrogenated polydecene. . Further, since hydrogenated polydecene and hydrogenated polyisobutylene are both polymers, only hydrogenated polydecene will be described as an example.
  • Samples 22 to 24 are polydimethylsiloxane (silicone oil, PMX200, 6cSt) and are extracted with ethanol, acetone and chloroform respectively. Since silicone oil is a silicon chain structure, the solubility of the active components of the carbon chain is poor. The extraction effect is very poor, showing that the DPPH clearance rate is extremely low; due to poor compatibility, the stability is not good, which is characterized by turbidity of the sample or analysis of the activity (precipitation).
  • the preferred solvent 2 of the present invention includes vegetable oil (samples 1 to 3), caprylic/capric triglyceride (samples 4 to 6), isostearyl isostearate (samples 7 to 9), White oil with oil viscosity (40 ° C) ⁇ 30 cSt (samples 10 to 12) and hydrogenated polyisobutylene with kinematic viscosity (40 ° C) ⁇ 30 cSt (the same as olefin polymer with hydrogenated polydecene, only hydrogenated polydecene)
  • hydrogenated polydecenes having a kinematic viscosity (40 ° C) ⁇ 30 cSt (samples 16 to 18).
  • the solvent 2 of the present invention as a comparative counterexample includes white oil (samples 13 to 15) having a kinematic viscosity (40 ° C) > 30 cSt, hydrogenated polydecene having a kinematic viscosity (40 ° C) > 30 cSt (samples 19 to 21), and 6 cSt poly 2 Methyl siloxane PMX200 (samples 22-24).
  • Silicone oil polydimethylsiloxane
  • the second extraction temperature selection experiment the second step is the solvent-solvent two synergistic extraction, so this step extraction is very important, and the second extraction temperature directly affects the mutual solubility and extraction efficiency of the two solvents.
  • the solvent is ethanol, for example, and the solvent is octanoic acid triglyceride.
  • This part is the screening of the process parameters extracted in the second step.
  • the DPPH and stability of the product are compared under the six conditions of 30 ° C, 40 ° C, 60 ° C, 75 ° C, 90 ° C and 95 ° C.
  • the extraction effect (DPPH) and stability are good at 40 ⁇ 90°C, the extraction effect at 30°C is poor, and the extraction effect at 95°C is poor.
  • the extraction temperature is recommended to be in the range of 40 ° C to 90 ° C, and the optimum extraction temperature is 60 ° C.
  • the second step is the solvent-solvent two synergistic extraction, the extraction of this step is very important, the second step of extracting the liquid solution directly affects the mutual solubility of solvent one and solvent two, with the extraction Extraction efficiency
  • the solvent is ethanol, for example, and the solvent is octanoic acid triglyceride.
  • the composition selected by the invention is guided by the theory of "the qi and bloodliness" of the traditional Chinese medicine, and according to the principle of "jun, minister, sage, and ambassador", the medicinal herbs and the medicinal herbs are used to promote blood circulation.
  • the adjuvant nourishes and nourishes the medicine, so that the medicine can clear away heat and detoxify, and achieve the effect of whitening and brightening the skin.
  • the extraction efficiency of the active ingredient is significantly increased, thereby obtaining an efficient plant extract.
  • the preparation method of each sample in the experiment is the same, the total mass of the raw material medicine is 10 g, and the composition and compatibility relationship of each sample group are different, as shown in Table 8.
  • the specific preparation method steps are as follows:
  • Second extraction adding octanoic acid triglyceride according to a ratio of material to liquid of 1:25 m/m, and extracting at 60 ° C for 1 h;
  • samples 1 to 10 were evaluated by DPPH clearance.
  • the experimental method is shown in the DPPH free radical scavenging experiment.
  • the results are shown in Figure 4.
  • the results showed that the DPPH clearance rate of the sample and the dosage of sample 5 (the case group) was the highest, and the effect was the best.
  • Samples 1 to 4 lacking the raw materials of the prescription and 6 to 10 groups of DPPH were not removed within the ratio of the prescription. The rate is significantly lower than sample 5.
  • Mouse melanoma cells (B16) have high melanin expression and are commonly used in the study of melanin synthesis.
  • B16 cells were cultured in RPMI-1640 complete medium (containing fetal bovine serum containing 10% by volume) under the conditions of 37 ° C, 5% CO 2 (volume fraction of CO 2 in the air in the incubator).
  • the cultured passage 3 B16 cells were seeded in 6-well plates, and after 24 hours, the fresh medium to which samples 1-10 were added was exchanged. The blank was replaced with RPMI-1640 complete medium instead of the sample solution. After continuing to incubate for 72 h, the supernatant was discarded. 1 mL of a mass concentration of 2.5 g/L trypsin digest was added to each well and digested at room temperature for 5 min. The digestion was stopped by adding 4 mL of RPMI-1640 complete medium and pipetted into a single cell suspension.
  • the inhibition rate of the sample for melanin synthesis was calculated according to the following formula:
  • composition of the plant extract is complicated, and it is difficult to analyze and quantify the active ingredient of the extract. Therefore, those skilled in the art can evaluate the efficiency of extracting the active ingredient by detecting the antioxidant activity, and the extract prepared by the process with good extraction efficiency will be Have more excellent effects.
  • Antioxidant activity is generally evaluated by DPPH free radical scavenging experiments.
  • DPPH 2,2-biphenyl-1-picrylhydrazyl
  • DPPH 2,2-biphenyl-1-picrylhydrazyl
  • the antioxidant provides a hydrogen atom to reduce the single electron on the DPPH to reduce the color, and the degree of radical removal is evaluated according to the amount of decrease in absorbance.
  • Sample preparation for the efficacy test of the present invention is as follows
  • Sample 1 (prepared oil extraction of the prior art): 5 g of peony, 5 g of perilla, 3 g of linseed, 3 g of buckwheat, 3 g of lotus seed, 3 g of medlar, 3 g of silymarin, 3 g of licorice, coarsely pulverized to 40 mesh , mixing; 0.2MPa, 110 ° C, treatment 30min; 60 ° C drying 2h; according to the ratio of material to liquid 1:25m / m adding octanoic acid / citric acid triglyceride, stirring at 80 ° C for 1h; according to the ratio of material to liquid 1 Addition of caprylic/capric triglyceride at 25 (m/m), stirring and extracting at 60 ° C for 1 h; cooling to below 40 ° C, 60 mesh coarse filtration, filter plate pore size 0.5 ⁇ m, fine filtration until the filtrate is clarified, to obtain sample 1.
  • Sample 2 (prior art ethanol extraction): take 5g of peony, 5g of perilla, 3g of linseed, 3g of buckwheat, 3g of lotus seed, 3g of medlar, 3g of milk thistle, 3g of licorice, coarsely pulverized to 40 mesh , Mixing; 0.2MPa, 110 ° C, treatment for 30 min; drying at 60 ° C for 2 h; adding ethanol according to the ratio of material to liquid 1:25 m / m, mixing, extracting at 80 ° C for 1 h; according to the ratio of material to liquid 1:25 (m / m) adding ethanol, stirring and extracting at 60 ° C for 1 h; cooling to below 40 ° C, 60 mesh coarse filtration; 60 ° C concentrated under reduced pressure, cooling to below 40 ° C, filter plate pore size 0.5 ⁇ m, fine filtration to clear the filtrate, then sample 2 .
  • Sample 3 (two extractions with solvent polarity less than solvent 2): take 5g of peony, 5g of perilla, 3g of linseed, 3g of buckwheat, 3g of lotus seed, 3g of medlar, 3g of silibin, 3g of licorice, coarsely pulverized to 40 mesh, mixed; 0.2MPa, 110 ° C, treatment for 30min; 60 ° C drying for 2h; ratio of material to liquid 1:25 (m / m), adding cyclohexane, stirring at 80 ° C for 1h; Adding butanediol to the ratio of material to liquid 1:25 (m/m), stirring and extracting at 60 ° C for 1 h; cooling to 40 ° C or less, 60 mesh coarse filtration; concentration at 60 ° C under reduced pressure to remove cyclohexane; cooling to below 40 ° C, The filter plate had a pore size of 0.5 ⁇ m and was finely filtered to obtain Sample 3.
  • A is the OD value of the sample solution mixed with the DPPH solution
  • B is the OD value of the mixed ethanol and DPPH solution
  • C is the OD value of the mixed ethanol and the sample solution.
  • Sample 1 was directly extracted with oil. Due to the large molecular weight of the oil, it was difficult to pass through the cell wall and cell membrane, and the intracellular active ingredient was extracted, and the viscosity was high, which was not conducive to the substance transfer during the extraction process, so the DPPH clearance rate was low.
  • Sample 2 is extracted with ethanol. Ethanol is an excellent solvent. At the same time as the oil-soluble active ingredient is extracted, a large amount of water-soluble polysaccharide is also dissolved. When concentrated, the viscous substance such as polysaccharide is partially dissolved in oil to form a precipitate. The loss of active ingredients is caused, so the DPPH clearance rate is low.
  • Sample 3 was extracted by two-step double solvent, but solvent 1 (ratio to solvent 2) was weaker, solvent 2 (ratio to solvent 1) was more polar, and solvent 1 had weaker interaction with cell membrane, which was not conducive to the two solvents.
  • solvent 1 ratio to solvent 2
  • solvent 1 had weaker interaction with cell membrane, which was not conducive to the two solvents.
  • solvent 1 had weaker interaction with cell membrane, which was not conducive to the two solvents.
  • solvent 1 ratio to solvent 2
  • solvent 1 had weaker interaction with cell membrane, which was not conducive to the two solvents.
  • Sample 4 was an extract prepared in Example 10 of the present invention, and the sample material 4 had the same ratio of material to liquid ratio as samples 1, 2 and 3, but the DPPH clearance rate was significantly higher than that of samples 1, 2 and 3, and was far superior. The sum of the effects of samples 1 and 2.
  • Turbidity is an optical property that is caused by the scattering of light caused by tiny particles in a liquid. The higher the turbidity, the larger the amount of scattered light. In this experiment, HI93414 high-precision data turbidity measuring instrument was used to detect sample turbidity. The lower the measured value, the lower the turbidity and the better the clarity, which proves that the product is stable.
  • the sample 1 itself is extracted by oil and fat, so the turbidity is excellent in the oil-type cosmetic auxiliary material; the sample 2 is an alcohol-soluble extract, and the compatibility with the oil and fat is poor, so the turbidity is high.
  • the extraction solvent of the sample 3 reverses the polarity of the solvent of the present invention, so that the solvent of the final product is relatively polar, and the compatibility with the oil is poor, so the turbidity is high.
  • Sample 4 was extracted with solvent one and solvent two, and the extraction process was optimized, so that the compatibility of the active ingredient with the commonly used auxiliary oil of cosmetics was good, so the turbidity was lower, and even better than the extract obtained by oil extraction.
  • Sample 1 grey extraction
  • Sample 2 ethanol extraction
  • 30-day stability test showed that there was a large amount of precipitation, indicating that the sample stability deteriorated.
  • Sample 3 in the case where the solvent was less polar than the solvent 2) 30-day stability test showed that the appearance of the sample had a large amount of precipitation, indicating that the sample stability was deteriorated.
  • Sample 4 Example 10) 30-day stability test showed that the appearance was clear and transparent, and the odor was normal, indicating that the stability of the prepared extract in this case was better than that of samples 1, 2 and 3.
  • the extraction efficiency of the present invention is much higher than that of direct extraction of oil (sample 1) and ethanol extraction (sample 2).
  • the extraction efficiency of the present invention is far superior to that of Sample 1 and Sample 2. If you want to achieve the same extraction efficiency as the case, the raw material needs to be increased to twice the current amount. At the same time as the increase of raw materials, the extraction solvent also needs to be multiplied.
  • the prior art ethanol extraction has been at least doubled than the organic solvent in this case. If the raw material is increased to twice the amount, the organic solvent is at least three times more than the present case. Therefore, the present invention is less expensive than the existing extraction process, requires less raw materials and extraction solvents, and is less expensive to prepare, store, and transport.
  • this case greatly reduces the amount of organic solvents, effectively avoids the cost of organic solvent recovery and emissions, and more importantly, greatly reduces the risk of environmental pollution.
  • this case has the advantages of cost saving, material reduction, energy consumption reduction and environmental protection compared with the prior art, and is very suitable for the industrialized large-scale production of energy saving and emission reduction.
  • Examples 10, 16, 17, 18, respectively were prepared from the samples 10, 16, 17, 18, respectively, and the blank group was added with an equal amount of caprylic/capric triglyceride.
  • Examples 16, 17, and 18 are oil-based products which can be used alone or as additives as in the present experiment, and the specific use method does not affect the final effect.
  • test site was the inner side of the curved arm, and there were 2 patients falling off between the groups. There was no obvious systemic adverse reaction or skin irritation above grade 3 in the test population. The effective volunteers in this test. The number is 30.
  • the skin melanin tester (Mexameter MX18) was used to assess changes in skin melanin content before and after use of the present invention.
  • the test method is based on the principle of spectral absorption, and the amount of melanin in the skin is determined by measuring the amount of reflection of a specific wavelength of light on human skin.
  • the skin melanin content MI value characterizes the melanin index, and the larger the MI value, the higher the skin melanin content. The measurement results are shown in the table below.
  • Example 16 180 175 169 168
  • Example 17 179 176 170
  • Example 18 181 176 168 168
  • the skin melanin content is lower than that before use, indicating that the external skin care preparation prepared by the invention can effectively reduce the skin melanin content.
  • the inventors made the same comparison with other embodiments of the present invention and obtained the same conclusion.
  • L* value is white balance, and the larger the L* value, the more the color is white.
  • ITA° value is the individual type angle of the skin. The larger the ITA° value, the brighter the skin.
  • the sample was the same as 1.
  • the skin melanin content was reduced.

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Abstract

一种具有美白亮肤功效的外用植物提取物，所述植物提取物由下述重量份配比的原料经下述方法制备而成：（1）按照下述重量份配比称取各原料，混匀；牡丹子1-10份、紫苏子1-10份、亚麻子1-10份、荞麦1-10份、莲子1-10份、枸杞子1-10份、水飞蓟1-10份、甘草1-10份；（2）第一次提取：按照料液比为1:10-100m/m混合原料和溶剂一，40-90℃条件下提取0.5-2h；（3）第二次提取：按照料液比为1:10-100m/m加入溶剂二，40-90℃条件下提取0.5-2h；（4）去除溶剂一；（5）精滤至澄清，即得提取物；所述溶剂一为乙醇、氯仿和丙酮中的一种或多种的混合；所述溶剂二为白油、氢化聚异丁烯、氢化聚癸烯、辛酸/癸酸甘油三酯、异硬脂酸异硬脂醇酯和植物油中的一种或多种的混合。

Description

具有美白亮肤功效的外用植物提取物、化妆品及其制备方法 技术领域
本发明涉及一种外用植物提取物，具体地说是一种具有美白亮肤功效的外用植物提取物及由该植物提取物制备得到的化妆品。
背景技术
美白产品一直是主流的美容护肤品。大部分美白剂通过选择性抑制酪氨酸酶活性，切断黑素合成下游途径，达到美白效果。但是现有美白剂，如氢醌，具有一定的细胞毒性，局部过量敷用可导致黑素细胞死亡，表现为皮肤出现白斑。如何获得一种天然安全高效的植物美白产品为本领域技术人员研究的热点。
植物提取物作为化妆品添加剂有诸多优势，如植物提取物成分天然、刺激性低和功效卓越等，因此，植物提取物作为功效添加剂在化妆品中的应用日益增多。植物原料中的功效成分有脂肪酸、甾醇、木脂素、酯类、多烯类、吡咯衍生物、酮类、醌类等油溶性成分，除此之外还会含有一些像糖类、氨基酸、蛋白质等非油溶性物质。目前植物提取物在化妆品领域应用受困的主要原因有(1)提取效率过低，由于植物原料的特性，提取效果过低造成提取成本的增加，因此很多企业优先选择低成本的合成化学原料来代替天然植物原料，以增加经济效益。(2)植物原料提取物的稳定性不佳。植物原料在添加进化妆品各剂型中，往往稳定性不好，在储存和运输过程中易出现变质、析出或沉淀的现象，不仅使产品腐坏率增加造成成本增加，还会直接影响功效，造成消费者使用感受下降。尤其是对于油剂型化妆品来说，油剂型化妆品对澄清度有极高的要求，一旦出现轻微析出和沉淀即会影响产品质量及性能。因此目前化妆品企业急需一种适用于工业生产的，提取率高、提取物稳定性好的植物提取物制备工艺。
对现有植物原料功效成分的提取方法介绍如下，目前现有制备工艺有以下几种：
1.浸泡提取
花草浸泡油具有悠久的应用历史，古埃及人和古希腊人已经学会用油脂吸收花瓣和药草的气味，作为药物或化妆品使用。浸泡油常用植物油做为溶剂，原料与油脂的比例约为1:3(v/v)，常温浸泡，需要反复投料2～3次，浸泡时间需要1～3个月。浸泡油在化妆品油剂型中使用时有较好的兼容性，但是此种方法提取效率低，提取时间较长不利于工业生产。
2.油脂直接高温提取
普济方、太平圣惠方等古籍中，记载了诸多油膏，以中药并油、脂煎焦去滓，用 于治疗皮肤疾病或美容。至今民间仍保留了许多经方、验方，将麻油烧热煎煮中药得到药油，用于缓解皮肤的各种不适症状。所以使用油脂直接高温煎煮也是传统提取方法之一，但是此种方法比较原始、提取效率低、不能有效提取植物中的活性成分，耗时长，物料浪费严重，提取效率低等严重制约了工业化生产。
3.水蒸气蒸馏法
水蒸气蒸馏法是植物精油提取常用的方法，但是此种方法只适用于提取植物中芳香类的易挥发性成分，而不挥发性成分则无法提取利用。
4.溶剂法提取
溶剂提取是生产植物提取物的常用方法，一般以乙醇、丙酮、氯仿等作为溶剂，具有设备简单，提取率高等特点。但此方法制备的提取物，对化妆品剂型要求较高，不适合添加入所有剂型，尤其是在油剂型化妆品中的溶解性较差，使得植物提取物加入纯油剂化妆品中后会有沉淀析出，严重影响产品质量，制约了其在纯油剂型化妆品中的应用。
5.超临界提取
超临界提取是近年兴起的新技术，提取溶剂时超临界流体，一般为超临界CO 2，具有无毒无害，提取率高，提取物纯度高等优点。但设备复杂、投入成本高，提取成本高，使得工业化大批量生产受限。且超临界提取得到的提取物一般与油脂的兼容性差，影响其在油剂型化妆品中的应用。
上述现有方法存在诸多缺陷，同时，受提取效率的限制，制备成本过高、有机溶剂排放造成环境污染等问题也日渐凸显。因此，本领域急需解决上述用于化妆品和护理产品添加的植物提取物制备中存在的问题。
发明内容
本发明的目的在于提出一种具有美白亮肤功效的植物提取物。
本发明的第二目的在于提出一种提取效率高，提取物性质稳定的植物提取物的制备方法。
本发明的第三目的在于提出由上述植物提取物制备得到的化妆品。
本发明的发明思路为：本发明选择的组合物利用“君、臣、佐、使”的组方原则，将八种植物进行配伍，结合对制备方法的改进，得到一种高效的植物美白提取物。
为实现本发明的目的，本发明采用如下具体技术方案：
一种具有美白亮肤功效的外用植物提取物，其中，所述植物提取物由下述重量份配比的原料经下述方法制备而成：
(1)按照下述重量份配比称取各原料，混匀；
牡丹子1～10份、紫苏子1～10份、亚麻子1～10份、荞麦1～10份、莲子1～10份、枸杞子1～10份、水飞蓟1～10份、甘草1～10份；
(2)第一次提取：按照料液比为1:10～100m/m混合原料和溶剂一，40～90℃条件下提取0.5～2h；
本发明所用溶剂一为乙醇、氯仿和丙酮中的一种或多种的混合。
料液比与提取温度对提取效率及提取成本有至关重要的影响，针对提取溶剂一的理化性质选择与其更匹配的料液比和提取参数不仅可以提高提取效率，还可以增强与下步溶剂二提取的协同性。本发明料液比范围内植物原料与溶剂一接触更充分，植物原料中的活性成分更易被提取，提取效率更高的同时不会造成溶剂及植物原料的浪费，提取成本更经济。优选的第一次提取料液比范围值为1:10～50m/m，此范围内提取效果更好，且与溶剂二协同性更强。
本发明提取温度和时间优选40～90℃条件下提取0.5～2h。提取温度和时间直接影响提取物性质，不恰当的提取温度和时间可能造成提取过程中植物原料的氧化变性、挥发性成分的损失及热敏性成分性质改变等，此范围内提取物功效成分在溶剂内的溶解性及物质交换速率均最佳，提取物功效优异且稳定。
上述步骤(2)的条件参数更适合于下述步骤(3)配合，可与步骤(3)产生协同增效的功效。
(3)第二次提取：按照料液比为1:10～100m/m加入溶剂二，40～90℃条件下提取0.5～2h；
本发明所用溶剂二为下述原料中的一种或多种的混合，分别是：白油，运动粘度(40℃)≤30cSt，推荐采用白油3#、5#、7#、10#、15#、26#；氢化聚异丁烯，运动粘度(40℃)≤30cSt，推荐采用氢化聚异丁烯Parleam 6、Parleam EX；氢化聚癸烯，运动粘度(40℃)≤30cSt，推荐采用氢化聚癸烯PAO2、PAO4、PAO6；辛酸/癸酸甘油三酯、异硬脂酸异硬脂醇酯和植物油。植物油推荐采用大豆油、向日葵籽油、芝麻油、澳洲坚果油、甜杏仁油、橄榄油、葡萄籽油、燕麦油、茶油中的一种或多种的混合。
溶剂二和溶剂一的配合对本发明技术效果尤为重要，发明人经实验验证，两溶剂之间不能完全互溶，完全互溶虽然可以保证较好的提取效率，但添加进化妆品中稳定性不好，易出现析出沉淀等不良情况。两溶剂也不能完全不互溶，两溶剂不互溶则不能起到协同增效的作用，提取效率非常低且提取物稳定性差。因此溶剂一和溶剂二部分互溶技术效果最佳，为了使两溶剂配合提取效率更高提取成本更经济，发明人将第 二次提取的温度和时间控制在上述条件参数范围内，不仅可以同时提高溶剂一和溶剂二部分互溶共同提取的提取效果，还可以有效避免提取效率趋于缓慢增加提取成本等问题。根据溶剂二特性，提取温度不宜过高，控制在90℃以下最佳，温度也不宜过低，低于40℃会影响功效成分在溶剂二内的溶解性以及溶剂一与溶剂二的相溶性，进而影响提取效率。
根据上述方法的描述，溶剂一和溶剂二的选择尤为重要，二者配合需要协同增效提高植物原料的提取效率，并且为了适应工业生产，提取过程需短，提取物品质需高即添加稳定性好，提取成本也需较低。因此，本案发明人经实验验证发现，如果本发明溶剂二极性大于溶剂一，提取效率及提取物稳定性均较差。发明人惊喜的发现如果溶剂一比溶剂二极性更强，溶剂一和溶剂二在一定条件下可部分互溶，此特点可增强活性成分在溶剂二中的溶解性，使得某些原本不溶于油脂，或者在油脂中溶解性差的物质能够很好的溶解在溶剂二中。二者配合提取，即可满足上述化妆品植物原料提取所需的所有条件，极大的提高了植物活性成分的提取效率，得到的提取物性质稳定，与化妆品其他原料兼容性极佳。
本发明可以选择上述记载的诸多溶剂中的一种进行单一溶剂提取，也可以根据实际提取的植物原料特性进行多溶剂的复配提取，溶剂之间复配比例可以根据本领域技术人员经验或者实际需要任意比例复配，无具体限定。因为溶剂二的特性，水对溶剂二的稳定性影响巨大，所以溶剂一优选无水体系，以乙醇为例，优选无水乙醇。
本发明溶剂二选择极性较溶剂一弱的提取溶剂，温和无刺激，与植物原料中的功效成分相容性好。溶剂二可以选择上述记载的诸多溶剂中的一种进行单一溶剂提取，也可以根据实际提取的植物原料特性进行多溶剂的复配提取，溶剂之间复配比例可以根据本领域技术人员经验或者实际需要任意比例复配，无具体限定。
上述步骤(3)中第二次提取料液比较佳范围值为1:10～50m/m。
(4)去除溶剂一；本领域技术人员公知的可去除溶剂的方法均可应用在此，本案推荐的较佳方法是：在40～80℃减压浓缩至溶剂一完全去除，减压范围一般控制在0.01Mpa至负0.15Mpa。溶剂一可能对皮肤有一定刺激性，去除溶剂一可以使产品性能更加温和，安全无毒副作用。溶剂一还可以采用膜浓缩、超滤、反渗透、渗透气化等方式脱除。
(5)精滤至澄清；此步骤的目的是使最终提取物更加稳定澄清，精滤过程使用的是0.2～10μm孔径的滤板进行过滤。
为了更有利于上述减压浓缩和精滤步骤的进行，并且更好的保护减压浓缩及精滤 设备，在步骤(3)和步骤(4)之间还可以增加粗滤步骤，粗滤的条件是60～100目粗滤，滤去原料渣。为了保持过滤料液的稳定，粗滤之前还可以增加冷却步骤，将料液冷却至40℃或40℃以下再进行粗滤最佳。
植物原料在第一次提取之前还可以进行预处理，预处理的目的是为了使提取溶剂更容易渗透细胞壁，进一步提高提取效率。预处理的步骤不是必须的，本发明提取率高主要取决于溶剂一和溶剂二的配合以及针对溶剂一二所使用的工艺步骤及参数，预处理可以在本发明所达到的提取率的基础上进一步缩短提取时间，但对于不便于预处理的植物原料也可以不使用预处理步骤。发明人推荐的预处理的步骤如下述，其他本领域技术人员公知的可实现预处理目的的步骤也可应用于此。
(1)粗粉碎：将原料粉碎至20～60目；粉碎步骤可利用本领域公知的粉碎设备进行，如切割机、破壁机、粉碎机等，粉碎步骤可以一次性完成，也可以分步骤由粗至细逐步完成。
(2)高温高压处理，此处所述的高温一般为至少等于或高于100℃的温度，本案控制在100～130℃为宜。高压指0.1Mpa以上，控制在0.1～0.2Mpa范围内效果最佳。处理时间不宜过长，控制在30min以内为佳。植物细胞壁的主要成分是纤维素和果胶，本发明采用高温高压预处理原料，是利用水蒸气破坏多糖分子间的氢键，使细胞壁结构松散，更有利于后续提取过程中溶剂透过细胞壁进入，使提取效率更佳。
(3)干燥，干燥的目的是去除高温高压后多余的水汽，更利于后期提取过程的进行和提取物的稳定，在本案中50～80℃干燥1～2h为佳。其他本领域技术人员公知的干燥手段也可以应用于此。
上述植物提取物在制备具有美白亮肤功效的化妆品中的应用。
一种具有美白亮肤功效的化妆品，其中，所述化妆品由上述的植物提取物及化妆品领域常用辅料制成。
一种具有美白亮肤功效的化妆品，其中，所述化妆品由下述重量份配比的原料制成：
牡丹籽油5～10、紫苏籽油5～20、上述植物提取物75～90、丁羟基甲苯0.1～0.3。
一种上述化妆品的制备方法，其特征在于，所述的制备方法步骤如下：
(1)按照上述配比称取各原料；
(2)将丁羟基甲苯加入所述植物提取物中，50～60℃下加热搅拌溶解20～40min；
(3)降温至30～40℃后加入紫苏籽油和牡丹籽油，搅拌均匀，即得。
上述方法制备得到的是油剂型化妆品，利用本发明植物提取物及护肤品领域常规方法及辅料也可以制备得到其他剂型，如乳液、膏霜、爽肤水、面膜或洗面奶等。
本发明制剂推荐使用方法为：以涂抹方法施于人体皮肤表面，轻轻按摩直至吸收。
本发明的有益结果：
本发明利用牡丹子、紫苏子、亚麻子、荞麦、莲子、枸杞子、水飞蓟和甘草配合且给出了最佳的配伍用量，各组分之间协同起效，结合本发明提出的新的不同极性双溶剂对化妆品植物原料有效提取的方法可以实现美白亮肤效果的极大提升。本发明方法根据对提取溶剂的优化配合及具体溶剂的选择，对提取步骤及提取条件参数的优化，使植物原料提取效率大幅增加，植物提取效率的评测主要通过植物原料的抗氧化和抗炎功效来评价，化妆品添加的植物提取物主要功效也是上述两种，通过本案方法提取得到的提取物通过功效实验可以看出在上述两功效方面远远优于现有技术提取得到的提取物。本案提取方法有效的缩短了提取时间，提取效率高，所用设备常规且低廉，均有效的降低了植物提取物制备成本，本案非常适合大规模工业化生产。更重要的是，本案提取得到的植物提取物成分更加稳定，与化妆品各种剂型的辅料兼容性更好，尤其是添加进油剂型化妆品中，有效的改进了现有技术提取物析出及出现沉淀等影响产品质量和功效的缺陷，使得化妆品更易储存运输，产品品质更佳，且使用时效果更佳。
附图说明
图1为样品1～24提取效果通过DPPH清除率评价图；
图2为样品25～30提取效果通过DPPH清除率评价图；
图3为样品31～36提取效果通过DPPH清除率评价图；
图4为组方筛选实验DPPH清除率评价图；
图5为组方筛选试验黑素合成抑制率评价图。
具体实施方式
为了使本领域技术人员更加详细的了解本发明所述提取方法，发明人提供如下具体实施例，所涉及到的试剂均为本领域内公知且可市售购买获得的，所述涉及到的仪器设备也是本领域的技术人员公知且能够掌握和运用的设备。为了保证溶剂二及提取物的稳定，本具体实施方式中溶剂一使用的各溶剂均为无水溶剂。以下实施例不得理解为任何意义上的对本发明权利要求的限制。
本案具体实施方式中使用原料及设备购买厂家见表1和表2。
表1 本发明所用原料
Figure PCTCN2019070952-appb-000001
表2 设备来源
Figure PCTCN2019070952-appb-000002
Figure PCTCN2019070952-appb-000003
实施例1
(1)按照下述重量份配比称取各原料，混匀；
牡丹子3g、紫苏子5g、亚麻子10g、荞麦1g、莲子5g、枸杞子10g、水飞蓟8g、甘草1g；
(2)第一次提取：按照料液比为1:20m/m加入乙醇，混合，50℃条件下提取2h；
(3)第二次提取：按照料液比为1:50m/m加入向日葵籽油，50℃条件下搅拌提取1h；
(4)40℃减压浓缩至乙醇完全去除；
(5)滤板孔径10μm，精滤至滤液澄清，即得。
实施例2
(1)按照下述重量份配比称取各原料，混匀；
牡丹子10g、紫苏子1g、亚麻子5g、荞麦6g、莲子1g、枸杞子4g、水飞蓟5g、甘草6g；
(2)第一次提取：按照料液比为1:10m/m加入乙醇，混合，40℃条件下提取2h；
(3)第二次提取：按照料液比为1:40m/m加入氢化聚异丁烯(20cSt)，60℃条件下搅拌提取1h；
(4)50℃减压浓缩至乙醇完全去除；
(5)滤板孔径1μm，精滤至滤液澄清，即得。
实施例3
(1)按照下述重量份配比称取各原料，混匀；
牡丹子1g、紫苏子10g、亚麻子3g、荞麦10g、莲子6g、枸杞子1g、水飞蓟10g、甘草3g；
(2)第一次提取：按照料液比为1:100m/m加入无水乙醇，混合，90℃条件下提取0.5h；
(3)第二次提取：按照料液比为1:100m/m加入辛酸/癸酸甘油三酯，90℃条件下搅拌提取2h；
(4)80℃减压浓缩至乙醇完全去除；
(5)滤板孔径0.2μm，精滤至滤液澄清，即得。
实施例4
(1)按照下述重量份配比称取各原料；
牡丹子7g、紫苏子8g、亚麻子1g、荞麦2g、莲子10g、枸杞子1g、水飞蓟1g、甘草10g；
(2)粗粉碎：将各原料药粉碎至20目混匀；
(3)高温高压处理：0.1MPa，100℃，处理5min；
(4)干燥：50℃干燥1h；
(5)第一次提取：按照料液比为1:70m/m加入氯仿，混合，45℃条件下提取1h；
(6)第二次提取：按照料液比为1:50m/m加入白油(7cSt)，45℃条件下搅拌提取2h；
(7)40℃减压浓缩至氯仿完全去除；
(8)滤板孔径0.2μm，精滤至滤液澄清，即得。
实施例5
(1)按照下述重量份配比称取各原料；
牡丹子7g、紫苏子7g、亚麻子3g、荞麦3g、莲子4g、枸杞子4g、水飞蓟6g、甘草6g；
(1)粗粉碎：将各原料药粉碎至40目混匀；
(2)高温高压处理：0.2MPa，130℃，处理20min；
(3)干燥：60℃干燥2h；
(4)第一次提取：按照料液比为1:10m/m加入氯仿，混合，90℃条件下提取1h；
(5)第二次提取：按照料液比为1:10m/m加入辛酸/癸酸甘油三酯，80℃条件下搅拌提取1h；
(6)60℃减压浓缩至氯仿完全去除；
(7)滤板孔径10μm，精滤至滤液澄清，即得。
实施例6
(1)按照下述重量份配比称取各原料；
牡丹子6g、紫苏子6g、亚麻子6g、荞麦6g、莲子9g、枸杞子2g、水飞蓟2g、甘草1g；
(2)粗粉碎：将各原料药粉碎至60目混匀；
(3)高温高压处理：0.2MPa，110℃，处理35min；
(4)干燥：75℃干燥1.5h；
(5)第一次提取：按照料液比为1:60m/m加入氯仿，混合，90℃条件下提取2h；
(6)第二次提取：按照料液比为1:60m/m加入氢化聚癸烯(30cSt)，90℃条件下搅拌提取0.5h；
(7)80℃减压浓缩至氯仿完全去除；
(8)滤板孔径6μm，精滤至滤液澄清，即得。
实施例7
(1)按照下述重量份配比称取各原料；
牡丹子3g、紫苏子7g、亚麻子3g、荞麦9g、莲子9g、枸杞子3g、水飞蓟7g、甘草10g；
(2)粗粉碎：将各原料药粉碎至30目混匀；
(3)高温高压处理：0.1MPa，100℃，处理5min；
(4)干燥：70℃干燥1h；
(5)第一次提取：按照料液比为1:60m/m加入丙酮，混合，50℃条件下提取1h；
(6)第二次提取：按照料液比为1:10m/m加入异硬脂酸异硬脂醇酯，45℃条件下搅拌提取1h；
(7)45℃减压浓缩至丙酮完全去除；
(8)滤板孔径2μm，精滤至滤液澄清，即得。
实施例8
(1)按照下述重量份配比称取各原料；
牡丹子6g、紫苏子4g、亚麻子1g、荞麦7g、莲子3g、枸杞子8g、水飞蓟3g、甘草9g；
(2)粗粉碎：将各原料药粉碎至50目混匀；
(3)高温高压处理：0.1MPa，110℃，处理20min；
(4)干燥：60℃干燥1h；
(5)第一次提取：按照料液比为1:35m/m加入丙酮，混合，65℃条件下提取1.5h；
(6)第二次提取：按照料液比为1:25m/m加入大豆油，65℃条件下搅拌提取1h；
(7)50℃减压浓缩至丙酮完全去除；
(8)滤板孔径4μm，精滤至滤液澄清，即得。
实施例9
(1)按照下述重量份配比称取各原料，混匀；
牡丹子2g、紫苏子2g、亚麻子2g、荞麦2g、莲子2g、枸杞子2g、水飞蓟2g、甘草2g；
(2)粗粉碎：将各原料药粉碎至50目混匀；
(3)高温高压处理：0.2MPa，130℃，处理30min；
(4)干燥：65℃干燥2h；
(5)第一次提取：按照料液比为1:40m/m加入氯仿乙醇混合液(氯仿乙醇按照质量比1:1复配)，混合，65℃条件下提取2h；
(6)第二次提取：按照料液比为1:100m/m加入芝麻油，65℃条件下搅拌提取2h；
(7)55℃减压浓缩至溶剂一完全去除；
(8)滤板孔径8μm，精滤至滤液澄清，即得。
实施例10
(1)按照下述重量份配比称取各原料，混匀；
牡丹子5g、紫苏子5g、亚麻子3g、荞麦3g、莲子3g、枸杞子2g、水飞蓟2g、甘草2g
(2)粗粉碎：将各原料碎至40目，混匀；
(3)高温高压处理：0.2MPa，110℃，处理30min；
(4)干燥：60℃干燥1.5h；
(5)第一次提取：按照料液比为1:25m/m加入乙醇，混合，80℃条件下提取1h；
(6)第二次提取：按照料液比为1:25m/m加入辛酸/癸酸甘油三酯，60℃条件下搅拌提取1h；
(7)冷却至40℃以下，60目粗滤；
(8)60℃减压浓缩至溶剂一完全去除；
(9)冷却至40℃以下，滤板孔径0.5μm，精滤至滤液澄清，即得。
实施例11
(1)按照下述重量份配比称取各原料，混匀；
牡丹子7g、紫苏子5g、亚麻子7g、荞麦5g、莲子7g、枸杞子5g、水飞蓟7g、甘草5g；
(2)粗粉碎：将各原料粉碎至50目混匀；
(3)高温高压处理：0.2MPa，110℃，处理15min；
(4)干燥：75℃干燥1h；
(5)第一次提取：按照料液比为1:40m/m加入氯仿和丙酮混合溶剂(二者之间按照质量比1:1复配)，混合，90℃条件下提取1h；
(6)第二次提取：按照料液比为1:40m/m加入辛酸/癸酸甘油三酯和氢化聚癸烯(17cSt)复配物(二者按照质量比1:1复配)，80℃条件下搅拌提取1h；
(7)冷却至40℃以下，80目粗滤；
(8)70℃减压浓缩至溶剂一完全去除；
(9)冷却至40℃以下，滤板孔径1μm，精滤至滤液澄清，即得。
实施例12
(1)按照下述重量份配比称取各原料，混匀；
牡丹子4g、紫苏子2g、亚麻子8g、荞麦4g、莲子6g、枸杞子2g、水飞蓟10g、甘草6g；
(2)粗粉碎：将各原料粉碎至60目；
(3)高温高压处理：0.1MPa，130℃，处理10min；
(4)干燥：80℃干燥1.5h；
(5)第一次提取：按照料液比为1:45m/m加入乙醇和丙酮混合溶剂(二者之间按照1:1复配)，混合，80℃条件下提取1h；
(6)第二次提取：按照料液比为1:40m/m加入橄榄油和澳洲坚果油复配物(二者按照质量比1:1复配)，60℃条件下搅拌提取1.5h；
(7)冷却至40℃以下，100目粗滤；
(8)80℃减压浓缩至溶剂一完全去除；
(9)冷却至40℃以下，滤板孔径6μm，精滤至滤液澄清，即得。
实施例13
(1)按照下述重量份配比称取各原料，混匀；
牡丹子3g、紫苏子5g、亚麻子3g、荞麦4g、莲子2g、枸杞子8g、水飞蓟8g、甘草3g；
(2)粗粉碎：将各原料粉碎至30目；
(3)高温高压处理：0.2MPa，100℃，处理30min；
(4)干燥：60℃干燥1h；
(5)第一次提取：按照料液比为1:20m/m加入氯仿和乙醇混合溶剂(二者之间按照质量比1:1复配)，混合，80℃条件下提取2h；
(6)第二次提取：按照料液比为1:60m/m加入白油(16cSt)和氢化聚异丁烯(11cSt)混合溶剂(二者按照质量比1:1复配)，70℃条件下搅拌提取1.5h；
(7)冷却至40℃以下，90目粗滤；
(8)80℃减压浓缩至溶剂一完全去除；
(9)冷却至40℃以下，滤板孔径5μm，精滤至滤液澄清，即得。
实施例14
(1)按照下述重量份配比称取各原料，混匀；
牡丹子10g、紫苏子3g、亚麻子3g、荞麦5g、莲子5g、枸杞子7g、水飞蓟7g、甘草7g；
(2)粗粉碎：将各原料粉碎至40目；
(3)高温高压处理：0.2MPa，120℃，处理10min；
(4)干燥：70℃干燥1h；
(5)第一次提取：按照料液比为1:50m/m加入乙醇，混合，90℃条件下提取1h；
(6)第二次提取：按照料液比为1:50m/m加入葡萄籽油和燕麦油混合溶剂(二者按照质量比1:1复配)，50℃条件下搅拌提取1.5h；
(7)冷却至40℃以下，90目粗滤；
(8)80℃减压浓缩至溶剂一完全去除；
(9)冷却至40℃以下，滤板孔径5μm，精滤至滤液澄清，即得。
实施例15
(1)按照下述重量份配比称取各原料，混匀；
牡丹子7g、紫苏子10g、亚麻子6g、荞麦2g、莲子4g、枸杞子6g、水飞蓟2g、甘草10g；
(2)粗粉碎：将各原料粉碎至40目；
(3)高温高压处理：0.2MPa，130℃，处理10min；
(4)干燥：70℃干燥1h；
(5)第一次提取：按照料液比为1:20m/m加入氯仿，混合，60℃条件下提取1h；
(6)第二次提取：按照料液比为1:20m/m加入甜杏仁油，45℃条件下搅拌提取1h；
(7)冷却至40℃以下，90目粗滤；
(8)80℃减压浓缩至溶剂一完全去除；
(9)冷却至40℃以下，滤板孔径0.5μm，精滤至滤液澄清，即得。
实施例16具有美白亮肤功效的油剂型化妆品
(1)按照下述配比称取各原料；
牡丹籽油5g、紫苏籽油15g、实施例1制备植物提取物75g、丁羟基甲苯0.3g。
(2)将丁羟基甲苯加入所述植物提取物中，60℃下加热搅拌溶解30min；
(3)降温至30℃后加入紫苏籽油和牡丹籽油，搅拌均匀，即得。
实施例17具有美白亮肤功效的油剂型化妆品
(1)按照下述配比称取各原料；
牡丹籽油8g、紫苏籽油5g、实施例8制备植物提取物80g、丁羟基甲苯0.1g。
(2)将丁羟基甲苯加入所述植物提取物中，50℃下加热搅拌溶解20min；
(3)降温至35℃后加入紫苏籽油和牡丹籽油，搅拌均匀，即得。
实施例18具有美白亮肤功效的油剂型化妆品
(1)按照下述配比称取各原料；
牡丹籽油10g、紫苏籽油20g、实施例15制备植物提取物90g、丁羟基甲苯0.2g。
(2)将丁羟基甲苯加入所述植物提取物中，55℃下加热搅拌溶解40min；
(3)降温至40℃后加入紫苏籽油和牡丹籽油，搅拌均匀，即得。
本发明功效实验
本发明溶剂一和溶剂二的配合，结合本发明优化的提取工艺及提取参数，可起到协同增效的功效，使得提取率更高，提取物性质更优异更稳定，提取成本更低，适合工业化应用。
一、本发明溶剂一和溶剂二的选择
1、溶剂一选择植物提取常用的，与各类活性成分兼容性好，提取率高，具有代表性的溶剂；考虑到实验证实的溶剂一极性应大于溶剂二提取效果最好，故最终确定为乙醇、丙酮和氯仿。发明人认为上述技术效果已经达到本案要求故不必再进行进一步溶剂一的筛选，这样也是为了减少溶剂二选择时的工作量。
2、溶剂二的选择过程简述：
溶剂二选择极性小于溶剂一的溶剂，以油脂类为佳。
(1)植物油：各植物油性质相似，故仅选一种为代表，分别与溶剂一的三种溶剂复配提取，均有较好的效果；
(2)白油：选择限定粘度范围内和范围外的两种白油(一般为临界值附近的数值，如26和32)，分别与溶剂一的三种溶剂复配提取，粘度范围内的白油效果好，范围外的效果不好；
(3)氢化聚异丁烯、氢化聚癸烯：这两种都是烯烃聚合物，仅选择一种为代表，重复白油筛选的工作，即选择限定粘度范围内和范围外的，(一般为临界值附近的数值，如26和32)分别实验，得到不同的提取效果；
(4)辛酸/癸酸甘油三酯：与溶剂一的三种溶剂复配提取，均有较好的效果；
(5)异硬脂酸异硬脂醇酯：与溶剂一的三种溶剂复配提取，均有较好的效果；
(6)聚二甲基硅氧烷(硅油)：硅油是硅链，对碳链的活性成分溶解效果差，分别与 溶剂一复配，提取效果均不好。
以上是溶剂筛选部分的实验思路，即溶剂选择部分的样品1～24。样品1～24的原料及制备方法相同，只是提取溶剂不同。
具体制备方法如下：
按照下述重量份配比称取各原料，混匀；
牡丹子5g、紫苏子5g、亚麻子3g、荞麦3g、莲子3g、枸杞子3g、水飞蓟3g、甘草3g
(1)粗粉碎：将各原料碎至40目，混匀；
(2)高温高压处理：0.2MPa，110℃，处理30min；
(3)干燥：60℃干燥1.5h；
(4)第一次提取：按照料液比为1:25m/m加入溶剂一，混合，80℃条件下提取1h；
(5)第二次提取：按照料液比为1:25m/m加入溶剂二，60℃条件下搅拌提取1h；
(6)冷却至40℃以下，60目粗滤；
(7)60℃减压浓缩至溶剂一完全去除；
(8)冷却至40℃以下，滤板孔径0.5μm，精滤至滤液澄清，即得。
样品1～24所用溶剂见表3
表3 样品溶剂表
样品序号 溶剂一 溶剂二
1 氯仿 向日葵籽油
2 乙醇 向日葵籽油
3 丙酮 向日葵籽油
4 氯仿 辛酸/癸酸甘油三酯
5 乙醇 辛酸/癸酸甘油三酯
6 丙酮 辛酸/癸酸甘油三酯
7 氯仿 异硬脂酸异硬脂醇酯
8 乙醇 异硬脂酸异硬脂醇酯
9 丙酮 异硬脂酸异硬脂醇酯
10 氯仿 白油(26cSt)
11 乙醇 白油(26cSt)
12 丙酮 白油(26cSt)
13 氯仿 白油(32cSt)
14 乙醇 白油(32cSt)
15 丙酮 白油(32cSt)
16 氯仿 氢化聚癸烯(30cSt)
17 乙醇 氢化聚癸烯(30cSt)
18 丙酮 氢化聚癸烯(30cSt)
19 氯仿 氢化聚癸烯(46cSt)
20 乙醇 氢化聚癸烯(46cSt)
21 丙酮 氢化聚癸烯(46cSt)
22 氯仿 聚二甲基硅氧烷(PMX200，6cSt)
23 乙醇 聚二甲基硅氧烷(PMX200，6cSt)
24 丙酮 聚二甲基硅氧烷(PMX200，6cSt)
3.测试结果：
本部分内容是对溶剂二的筛选，溶剂一固定为乙醇、氯仿、丙酮。
(1)DPPH清除自由基实验：植物提取物的成分复杂，对于提取物有效成分的分析及定量比较困难，因此本领域技术人员通过对抗氧化活性检测来评定有效成分提取的效率，往往提取效率好的工艺制备得到的提取物会有更优异的抗氧化活性功效。抗氧化活性一般采用DPPH自由基清除实验评价。DPPH(2，2-联苯基-1-苦基肼基)是一种稳定存在的有机氮自由基，广泛应用于体外抗氧化剂能力研究。基于DPPH在515nm左右有特征吸收峰，抗氧化剂提供氢原子将DPPH上的单电子还原使其颜色减弱，据其吸光值的减少量来评价自由基的清除程度。
样品1～24抗氧化活性实验结果见图1。
(2)稳定性实验，见表4。
表4 不同溶剂提取样品的稳定性比较
Figure PCTCN2019070952-appb-000004
Figure PCTCN2019070952-appb-000005
Figure PCTCN2019070952-appb-000006
Figure PCTCN2019070952-appb-000007
实验结果：
1.样品1～3为植物油(植物油性质相似，仅以向日葵籽油为例)分别与溶剂一复配提取，植物油与乙醇、丙酮、氯仿复配，均有良好的提取效果。
2.样品4～6为辛酸/癸酸甘油三酯分别与乙醇、丙酮、氯仿复配提取，均有良好 的提取效果。
3.样品7～9为异硬脂酸异硬脂醇酯分别与乙醇、丙酮、氯仿复配提取，均有较好的提取效果。
4.样品10～12是白油(26cSt，符合本发明限定的运动粘度≤30cSt的要求)分别与乙醇、丙酮、氯仿复配提取，均有较好的提取效果。
5.样品13～15是白油(32cSt，不符合本发明限定的运动粘度≤30cSt的要求)分别与乙醇、丙酮、氯仿复配提取，提取效果都较差。
6.样品10～15是将运动粘度≤30cSt的白油，与运动粘度＞30cSt的白油作对比，通过提取效果的差异，说明选择运动粘度≤30cSt白油的原因。
7.样品16～18是氢化聚癸烯(30cSt，符合本发明限定的运动粘度≤30cSt的要求)分别与乙醇、丙酮、氯仿复配提取，均有较好的提取效果。
8.样品19～21是氢化聚癸烯(46cSt，不符合本发明限定的运动粘度≤30cSt的要求)分别与乙醇、丙酮、氯仿复配提取，提取效果都较差。
9.样品16～21与白油类似，是将运动粘度≤30cSt的氢化聚癸烯，与运动粘度＞30cSt的作对比，通过提取效果的差异，说明选择运动粘度≤30cSt氢化聚癸烯的原因。另外，氢化聚癸烯和氢化聚异丁烯都是聚合物，因此仅以氢化聚癸烯为例进行说明。
10.样品22～24是聚二甲基硅氧烷(硅油，PMX200，6cSt)分别与乙醇、丙酮、氯仿复配提取，由于硅油是硅链结构，对碳链的活性成分溶解效果差，因此提取效果均很差，表现为DPPH清除率极低；由于兼容性差，导致其稳定性也不好，表现为样品混浊或活性成分析出(沉淀)。
通过上述实验，本发明优选出的溶剂二包括植物油(样品1～3)，辛酸/癸酸甘油三酯(样品4～6)，异硬脂酸异硬脂醇酯(样品7～9)，运动粘度(40℃)≤30cSt的白油(样品10～12)，运动粘度(40℃)≤30cSt的氢化聚异丁烯(与氢化聚癸烯同为烯烃聚合物，仅以氢化聚癸烯为例进行实验)，运动粘度(40℃)≤30cSt的氢化聚癸烯(样品16～18)。
本发明作为对比反例的溶剂二包括运动粘度(40℃)＞30cSt的白油(样品13～15)，运动粘度(40℃)＞30cSt的氢化聚癸烯(样品19～21)，6cSt聚二甲基硅氧烷PMX200(样品22～24)。
根据上文中的对比实验可知，通过分别和溶剂一(乙醇、丙酮、氯仿)进行复配提取，植物油，辛酸/癸酸甘油三酯，异硬脂酸异硬脂醇酯，运动粘度(40℃)≤30cSt的白油、氢化聚异丁烯和氢化聚癸烯，均具有较好的提取效果，且提取后的产品稳定 性好，适合作为本发明的溶剂二，与溶剂一配合，实现本发明中的提取工艺。而运动粘度(40℃)＞30cSt的白油、氢化聚异丁烯和氢化聚癸烯，由于粘度增大，不利于提取过程中的物质传递，导致提取效果不理想，不适合作为本发明的溶剂二。硅油(聚二甲基硅氧烷)由于结构差异，与植物中的碳链活性成分相容性不好，进而导致提取效率低，且提取后的产品稳定性差，也不适合作为本发明的溶剂二使用。
二、本案提取参数的确定
1.第二次提取温度选择实验：第二步是溶剂一溶剂二协同提取，因此此步骤提取至关重要，第二步提取温度直接影响到两溶剂的互溶程度及提取效率。
在本实验中溶剂一以乙醇为例，溶剂二以辛酸癸酸甘油三酯为例。
具体制备工艺如实验一，具体步骤如下：
(1)按照下述重量份配比称取各原料，混匀；
牡丹子5g、紫苏子5g、亚麻子3g、荞麦3g、莲子3g、枸杞子3g、水飞蓟3g、甘草3g
(2)粗粉碎：将各原料碎至40目，混匀；
(2)高温高压处理：0.2MPa，110℃，处理30min；
(3)干燥：60℃干燥1.5h；
(4)第一次提取：按照料液比为1:25m/m加入乙醇，混合，80℃条件下提取1h；
(5)第二次提取：按照料液比为1:25m/m加入辛酸/癸酸甘油三酯，提取温度具体见表5，搅拌提取1h；
提取2h；
(6)冷却至40℃以下，60目粗滤；
(7)60℃减压浓缩至溶剂一完全去除；
(8)冷却至40℃以下，滤板孔径0.5μm，精滤至滤液澄清，即得。
表5
样品序号 步骤(5)提取温度
25 30℃
26 40℃
27 60℃
28 75℃
29 90℃
30 95℃
样品25～30提取效果通过DPPH清除率评价，实验方法见DPPH自由基清除实验。结果见图2。可见，在提取物温度在40～90度之间提取效率最高，低于40度或高于90度的情况下提取效率过低，如果采用不良温度只能通过延长提取时间来提高提取率，那么会影响提取工艺在工业应用上的经济效益。
样品25～30的稳定性实验方法见稳定性比较，结果见表6所示。
表6 不同温度提取样品的稳定性比较
Figure PCTCN2019070952-appb-000008
Figure PCTCN2019070952-appb-000009
本部分内容是对第二步提取的工艺参数筛选，以温度为例，比较了30℃、40℃、60℃、75℃、90℃和95℃六个温度条件下，产品的DPPH和稳定性，40～90℃提取效果(DPPH)和稳定性都较好，30℃提取效果差，95℃提取效果较差，由于温度过高，产品的稳定性也较差，出现变色和异味，因此最终的提取温度推荐采用40℃～90℃范围，最佳提取温度是60℃。
2.第二次提取料液比实验：第二步是溶剂一溶剂二协同提取，此步骤提取至关重要，第二步提取料液比直接影响溶剂一和溶剂二的互溶度，配合提取的提取效率
在本实验中溶剂一以乙醇为例，溶剂二以辛酸癸酸甘油三酯为例。
具体制备工艺如实验一，具体步骤如下：
(1)按照下述重量份配比称取各原料，混匀；
牡丹子5g、紫苏子5g、亚麻子3g、荞麦3g、莲子3g、枸杞子3g、水飞蓟3g、甘草3g
(2)粗粉碎：将各原料碎至40目，混匀；
(2)高温高压处理：0.2MPa，110℃，处理30min；
(3)干燥：60℃干燥1.5h；
(4)第一次提取：按照料液比为1:25m/m加入乙醇，混合，80℃条件下提取1h；
(5)第二次提取：按照表7料液比加入辛酸癸酸甘油三酯，提取温度60℃，搅拌提取1h；
(6)冷却至40℃以下，60目粗滤；
(7)60℃减压浓缩至溶剂一完全去除；
(8)冷却至40℃以下，滤板孔径0.5μm，精滤至滤液澄清，即得。
表7
样品序号 步骤(4)料液比
31 1:2
32 1:10
33 1:25
34 1:50
35 1:100
36 1:150
样品31～36提取效果通过DPPH清除率评价，实验方法见DPPH自由基清除实验。 结果见图3。可见，在料液比为1:10～100提取效率高，且在1:10～50提取效率最佳。
三、本案组合物的各原料药及配伍选择优化
本发明组方思路：本发明选择的组合物以中医“气行则血行”的理论为指导，按照“君、臣、佐、使”的组方原则，通过君药、臣药行气活血，佐药补益滋养，使药清热解毒，达到美白亮肤的功效，结合对制备方法的改进，显著增加了活性成分的提取效率，从而得到一种高效的植物提取物。
本实验各样品的制备方法相同，原料药总质量是10g，各样品组方的组分及配伍关系不同，详见表8。具体制备方法步骤如下：
(1)按照表8重量份配比称取各原料，混匀；
(2)粗粉碎：将各原料粉碎至40目；
(3)高温高压处理：0.10MPa，100℃处理30min；
(4)干燥：60℃干燥2h；
(5)第一次提取：按照料液比为1:25m/m加入乙醇，混合，80℃条件下提取1h；
(6)第二次提取：按照料液比为1:25m/m加入辛酸癸酸甘油三酯，60℃条件下提取1h；
(7)冷却至40℃以下，60目粗滤得滤液；
(8)60℃减压浓缩至溶剂一完全去除；
(9)冷却至40℃以下，滤板孔径0.5μm，精滤至滤液澄清，即得。
表8
Figure PCTCN2019070952-appb-000010
Figure PCTCN2019070952-appb-000011
1.DPPH清除率实验
样品1～10组方效果通过DPPH清除率评价，实验方法见DPPH自由基清除实验。结果见图4。结果表明，样品5(本案组方)的组方及用量DPPH清除率最高，效果最好，缺少组方原料的样品1～4及不在本组方配比范围内的6～10组方DPPH清除率明显低于样品5。
2.影响B16细胞黑素合成
小鼠黑素瘤细胞(B16)具有高表达黑色素的特点，是研究黑素合成常用的细胞模型。
实验方法：B16细胞用RPMI－1640完全培养基(含体积分数为10％的胎牛血清)在37℃，5％CO2(培养箱内空气中CO2的体积分数为5％)条件下培养。
将培养的第3代B16细胞接种于6孔板，24h后用添加样品1-10的新鲜培养基换液。空白以RPMI－1640完全培养基代替样品溶液。继续孵育72h后，弃去上清液。每孔加入质量浓度2.5g/L胰蛋白酶消化液1mL,于室温下消化5min。加入4mL RPMI－1640完全培养基中止消化，并吹打成单细胞悬液。取0.5mL作细胞计数，其余细胞悬液于1500rpm离心10min，弃上清液，加入1mol/L的NaOH溶液1mL，80℃水浴30min，在酶标仪470nm处测其吸光度。
按下列公式计算样品对黑色素合成的抑制率：
Figure PCTCN2019070952-appb-000012
结果见图5。结果表明，样品5(本案组方)的抑制率最高，效果最好，优于样品1～4及不在本组方配比范围内的6～10组方。
四、本发明方法与现有技术方法提取效率比较
植物提取物的成分复杂，对于提取物有效成分的分析及定量比较困难，因此本领域技术人员通过对抗氧化活性的检测来评定有效成分提取的效率，往往提取效率好的工艺制备得到的提取物会有更优异的功效。
抗氧化活性一般采用DPPH自由基清除实验评价。DPPH(2，2-联苯基-1-苦基肼基)是一种稳定存在的有机氮自由基，广泛应用于体外抗氧化剂能力研究。基于DPPH在515nm左右有特征吸收峰，抗氧化剂提供氢原子将DPPH上的单电子还原使其颜色减弱，据其吸光值的减少量来评价自由基的清除程度。
本发明功效实验的样品制备如下述
(1)样品1(现有技术油脂提取)：取牡丹子5g、紫苏子5g、亚麻子3g、荞麦3g、莲子3g、枸杞子3g、水飞蓟3g、甘草3g，粗粉碎至40目，混匀；0.2MPa，110℃，处理30min；60℃干燥2h；按照料液比为1:25m/m加入辛酸/癸酸甘油三酯，80℃条件下搅拌提取1h；按料液比1:25(m/m)加入辛酸/癸酸甘油三酯，60℃搅拌提取1h；冷却至40℃以下，60目粗滤，滤板孔径0.5μm，精滤至滤液澄清，即得样品1。
(2)样品2(现有技术乙醇提取)：取牡丹子5g、紫苏子5g、亚麻子3g、荞麦3g、莲子3g、枸杞子3g、水飞蓟3g、甘草3g，粗粉碎至40目，混匀；0.2MPa，110℃，处理30min；60℃干燥2h；按照料液比为1:25m/m加入乙醇，混合，80℃条件下提取1h；按料液比1:25(m/m)加入乙醇，60℃搅拌提取1h；冷却至40℃以下，60目粗滤；60℃减压浓缩，冷却至40℃以下，滤板孔径0.5μm，精滤至滤液澄清，即得样品2。
(3)样品3(溶剂一极性小于溶剂二的情况下两次提取)：取牡丹子5g、紫苏子5g、亚麻子3g、荞麦3g、莲子3g、枸杞子3g、水飞蓟3g、甘草3g，粗粉碎至40目，混匀；0.2MPa，110℃，处理30min；60℃干燥2h；料液比1:25(m/m)，加入环己烷，80℃搅拌提取1h；按料液比1:25(m/m)加入丁二醇，60℃搅拌提取1h；冷却至40℃以下，60目粗滤；60℃减压浓缩，除去环己烷；冷却至40℃以下，滤板孔径0.5μm，精滤，得到样品3。
(4)样品4：实施例10。
1.DPPH自由基清除实验
(1)实验方法：取DPPH溶液1mL和样品液1mL，充分振荡混合均匀，静置30min，用酶标仪在517nm波长下测定其吸光度。
DPPH自由基清除率计算公式：
DPPH自由基清除率％＝[(B+C)-A]/B*100
式中：A为试样溶液与DPPH溶液混合后的OD值，B为无水乙醇与DPPH溶液混合后的OD值，C为无水乙醇与试样溶液混合后的OD值。
(2)实验结论：如表8所示。
表10 不同工艺制备样品DPPH清除率对比
样品名称 受试浓度％ 清除率％
样品1 5 29
样品2 5 56
样品3 5 33
样品4 5 88
样品1采用油脂直接提取，由于油脂分子量较大，不易通过细胞壁和细胞膜，提取胞内活性成分，且粘度较高，不利于提取过程中的物质传递，故DPPH清除率低。
样品2采用乙醇提取，乙醇是优良的溶剂，提取出油溶活性成分的同时，大量的水溶性多糖也随之溶出；浓缩时，多糖等粘性物质裹挟部分油溶活性成分析出，形成沉淀，造成了活性成分的损失，故DPPH清除率较低。
样品3采用两步法双溶剂提取，但溶剂1(与溶剂2比)极性较弱，溶剂2(与溶剂1比)极性较强，溶剂1与细胞膜相互作用弱，不利于两种溶剂进入细胞提取活性成分，破坏两溶剂间的协同增效作用，导致提取率降低，故DPPH清除率较低。
样品4为本发明的实施例10制备提取物，样品4提取物时间料液比等参数与样品1、2和3相同，但DPPH清除率显著高于样品1、2和3，且远远优于样品1和2的效果之和。
发明人用其它实施例做了同样的对比，得出相同的实验结论。
五、本发明与现有技术相比得到的提取物在油剂型化妆品中稳定性比较
1.用于油剂型化妆品中澄清度比较
(1)实验方法：取样品液3.0g和油剂型化妆品常用辅料油脂27.0g，加热至50℃左右，搅拌溶解20min，静置冷却1h后，观察样品在油脂中的溶解情况。样品与油脂相容性好，则溶解后的样品澄清透明；样品和油脂相容性差，则溶解后的样品变浑浊。因此，样品在油脂中的溶解性可以用其溶解后的浑浊程度(浊度)来表征。
浊度属于一种光学特性，是由于液体中的微小颗粒引起的光的散射，浊度越高则散射光量越大。本实验采用HI93414高精度数据型浊度测量仪检测样品浊度。所测数值越低证明浊度越低澄清度越好，证明产品稳定性佳。
(2)样品制备工艺：与DPPH自由基清除实验样品相同。
表12 不同工艺样品浊度对比
Figure PCTCN2019070952-appb-000013
(3)实验结论：如表14所示。
样品1本身为油脂提取，因此在油剂型化妆品辅料中浊度比较优异；样品2为醇溶性提取物，与油脂的相容性较差，故浊度高。样品3的提取溶剂，颠倒了本发明的溶剂极性，使得终产品的溶剂极性较强，与油脂相容性差，故浊度高。样品4采用溶剂一和溶剂二配合提取，并优化了提取工艺，使得活性成分与化妆品常用辅料油脂的相容性好，故浊度较低，甚至优于油脂提取得到的提取物。
发明人用本发明其他实施例做了同样的对比，得到相同的结论。
2.稳定性实验
(1)实验方法：取样品液10g和辛酸/癸酸甘油三酯190g，加热至50℃左右，搅拌溶解20min，将配置好的样品平均分成五份，分别放置于避光(室温暗盒中)、冷藏(4℃冰箱)、光照(28℃光照培养箱)、热(45℃烘箱)、冷冻(-15℃冰箱)五个条件下，并分别在第7天、14天、30天观察稳定性。
(2)样品信息：上述样品1、2、3、4。
表13 不同工艺样品稳定性对比
Figure PCTCN2019070952-appb-000014
Figure PCTCN2019070952-appb-000015
Figure PCTCN2019070952-appb-000016
(3)实验结论：如表15所示。
样品1(油脂提取)30天稳定性实验可见其有少量沉淀，并且具有轻微异味，说明样品变质。样品2(乙醇提取)30天稳定性实验可见其有大量沉淀，说明样品稳定性变差。样品3(溶剂一极性小于溶剂二的情况)30天稳定性实验可见，其外观具有大量沉淀，说明样品稳定性变差。样品4(实施例10)30天稳定性实验可见，外观澄清透明，气味正常，说明本案制备提取物稳定性优于样品1、2和3。
发明人用本发明其他实施例做了同样的对比，得到相同的结论。
六、本发明方法与现有方法技术成本比较
根据DPPH自由基清除实验结果可知，提取条件相同时(料液比、提取温度、提取时间)，本发明(样品4)的提取效率远高于油脂直接提取(样品1)及乙醇提取(样品2)。
表14 本发明与现有技术工业化应用的成本比较
Figure PCTCN2019070952-appb-000017
Figure PCTCN2019070952-appb-000018
通过上述表格可知，本发明提取效率远远优于样品1和样品2。如果想达到与本案相同提取效率，原料需要增加至现有两倍用量。原料增加的同时，提取溶剂也需要成倍增加，现有技术乙醇提取已经比本案有机溶剂用量多了至少一倍，如果增加原料至两倍量，有机溶剂至少比本案多三倍。因此本发明与现有提取工艺相比成本低廉，原料、提取溶剂用量更少，在制备、储存和运输上的成本更低。并且由于本案大幅度减少了有机溶剂的用量，有效的避免了有机溶剂回收及排放的成本，更重要的是极大的降低了对环境污染的风险。综上，本案与现有技术相比具有节约成本、减少物料、减少能量消耗、环保的优点，非常适用于目前节能减排的工业化大生产。
七、本发明制备的油剂型化妆品人体功效实验
表15 人体测试样品配方
Figure PCTCN2019070952-appb-000019
样品分别为实施例10、16、17、18，空白组添加样品为等量的辛酸/癸酸甘油三酯。实施例16、17和18为油剂型产品，可以单独使用，也可以与本实验一样作为添加剂使用，具体使用方法不对最终效果产生影响。
在测试周期内，筛选32人进行研究，测试部位为曲臂内侧，组间脱落2人，受试人群中未出现明显的全身不良反应或3级以上的皮肤刺激，本次测试的有效志愿者人数为30人。
1.降低皮肤黑色素含量
采用皮肤红黑色素测试仪(Mexameter MX18)评估受试者使用本发明前后，皮肤黑色素含量变化。该测试方法是基于光谱吸收的原理，通过测定特定波长的光照在人体皮肤上后的反射量来确定皮肤中黑色素的含量。皮肤黑色素含量MI值表征黑素指数，MI值越大，皮肤黑色素含量越高。测定结果如下表所示。
表16 样品使用前后皮肤黑色素含量MI值变化
样品 使用前 第2周 第4周 第6周
空白 179 178 180 181
实施例10 180 176 173 169
实施例16 180 175 169 168
实施例17 179 176 170 168
实施例18 181 176 168 168
受试者使用本发明实施例制备的外用护肤制剂后，肌肤黑色素含量相比使用前呈降低趋势，说明本发明制备的外用护肤制剂可有效降低肌肤黑色素含量。发明人用本发明其他实施例做了同样的对比，得到相同的结论。
2.提高皮肤亮白度
采用皮肤色差测试探头及多功能皮肤测试系统(CL400和MPA9)测试受试者使用本发明前后，皮肤白度(亮度)L*值和皮肤明亮度(暗黄度)ITA°值的变化。L*值为白平衡，L*值越大，颜色越偏向白色。ITA°值为皮肤个体类型角，ITA°值越大，皮肤越明亮。
样品同1.降低皮肤黑色素含量实验。
表17 样品使用前后皮肤白度L*值变化
样品 使用前 第2周 第4周 第6周
空白 65 64 66 63
实施例10 67 69 71 74
实施例16 64 66 69 70
实施例17 65 68 69 71
实施例18 67 70 73 75
表18 样品使用前后皮肤明亮度ITA°值变化
样品 使用前 第2周 第4周 第6周
空白组 42.68 42.59 42.64 42.95
实施例10 42.23 44.56 45.65 46.69
实施例16 43.01 45.35 46.41 47.56
实施例17 43.42 44.93 46.09 47.24
实施例18 42.89 45.21 46.45 47.69
结果显示，受试者使用本发明实施例制备的外用护肤制剂6周后，肌肤亮白度L*值以及肌肤明亮度ITA°值相比使用前呈升高趋势，说明本发明制备的外用护肤组合物制剂可有效提高肌肤亮白度和亮度。发明人用本发明其他实施例做了同样的对比，得到相同的结论。

Claims (24)

  1. 一种具有美白亮肤功效的外用植物提取物，其特征在于，所述植物提取物由下述重量份配比的原料经下述方法制备而成：
    (1)按照下述重量份配比称取各原料，混匀；
    牡丹子1～10份、紫苏子1～10份、亚麻子1～10份、荞麦1～10份、莲子1～10份、枸杞子1～10份、水飞蓟1～10份、甘草1～10份；
    (2)第一次提取：按照料液比为1:10～100m/m混合原料和溶剂一，40～90℃条件下提取0.5～2h；
    (3)第二次提取：按照料液比为1:10～100m/m加入溶剂二，40～90℃条件下提取0.5～2h；
    (4)去除溶剂一；
    (5)精滤至澄清，即得提取物；
    所述溶剂一为乙醇、氯仿和丙酮中的一种或多种的混合；
    所述溶剂二为白油、氢化聚异丁烯、氢化聚癸烯、辛酸/癸酸甘油三酯、异硬脂酸异硬脂醇酯和植物油中的一种或多种的混合。
  2. 根据权利要求1所述的具有美白亮肤功效的外用植物提取物，其特征在于，所述步骤(2)中料液比为1:10～50m/m。
  3. 根据权利要求1所述的具有美白亮肤功效的外用植物提取物，其特征在于，所述步骤(3)中料液比为1:10～50m/m。
  4. 根据权利要求1所述的具有美白亮肤功效的外用植物提取物，其特征在于，所述步骤(4)中利用40～80℃减压浓缩至完全去除溶剂一。
  5. 根据权利要求1所述的具有美白亮肤功效的外用植物提取物，其特征在于，所述步骤(5)使用0.2～10μm孔径的滤板精滤。
  6. 根据权利要求1所述的具有美白亮肤功效的外用植物提取物，其特征在于，所述步骤(5)精滤之前还包括冷却步骤，冷却至40℃或40℃以下。
  7. 根据权利要求1至6中任意一项所述的具有美白亮肤功效的外用植物提取物，其特征在于，在步骤(3)和步骤(4)之间还包括60～100目粗滤。
  8. 根据权利要求7所述的具有美白亮肤功效的外用植物提取物，其特征在于，所述粗滤之前还包括冷却步骤，冷却至40℃或40℃以下。
  9. 根据权利要求1至6中任意一项所述的具有美白亮肤功效的外用植物提取物，其特征在于，所述植物原料在第一次提取之前做预处理，所述预处理的步骤为：
    (1)粗粉碎：将原料粉碎至20～60目；
    (2)高温高压处理；
    (3)干燥。
  10. 根据权利要求9所述的具有美白亮肤功效的外用植物提取物，其特征在于，所述高温高压的条件是：粗粉碎后的原料在0.1～0.2MPa，100～130℃，处理5～30min。
  11. 根据权利要求9所述的具有美白亮肤功效的外用植物提取物，其特征在于，所述干燥条件是50～80℃干燥1～2h。
  12. 根据权利要求7所述的具有美白亮肤功效的外用植物提取物，其特征在于，所述植物原料在第一次提取之前做预处理，所述预处理的步骤为：
    (1)粗粉碎：将原料粉碎至20～60目；
    (2)高温高压处理；
    (3)干燥。
  13. 根据权利要求12所述的具有美白亮肤功效的外用植物提取物，其特征在于，所述高温高压处理条件是：粗粉碎后的原料在0.1～0.2MPa，100～130℃条件下处理5～30min。
  14. 根据权利要求12所述的具有美白亮肤功效的外用植物提取物，其特征在于，所述干燥条件是50～80℃干燥1～2h。
  15. 权利要求1至6中任意一项所述的植物提取物在制备具有美白亮肤功效的化妆品中的应用。
  16. 权利要求7所述的植物提取物在制备具有美白亮肤功效的化妆品中的应用。
  17. 一种具有美白亮肤功效的化妆品，其特征在于，所述化妆品由权利要求1至6中任意一项所述的植物提取物及化妆品领域可接受辅料制成。
  18. 根据权利要求17所述的化妆品，其特征在于，所述化妆品为油剂型化妆品。
  19. 一种具有美白亮肤功效的化妆品，其特征在于，所述化妆品由权利要求7所述的植物提取物及化妆品领域常用辅料制成。
  20. 一种具有美白亮肤功效的化妆品，其特征在于，所述化妆品由权利要求8所述的植物提取物及化妆品领域常用辅料制成。
  21. 一种具有美白亮肤功效的化妆品，其特征在于，所述化妆品由权利要求9所述的植物提取物及化妆品领域常用辅料制成。
  22. 一种具有美白亮肤功效的化妆品，其特征在于，所述化妆品由权利要求12所述的植物提取物及化妆品领域常用辅料制成。
  23. 一种具有美白亮肤功效的化妆品，其特征在于，所述化妆品由下述重量份配 比的原料制成：
    牡丹籽油5～10、紫苏籽油5～20、权利要求1至6中任意一项所述的植物提取物75～90、丁羟基甲苯0.1～0.3。
  24. 一种权利要求23所述化妆品的制备方法，其特征在于，所述的制备方法步骤如下：
    (1)按照权利要求23所述配比称取各原料；
    (2)将丁羟基甲苯加入所述植物提取物中，50～60℃下加热搅拌溶解20～40min；
    (3)降温至30～40℃后加入紫苏籽油和牡丹籽油，搅拌均匀，即得。
PCT/CN2019/070952 2018-01-10 2019-01-09 具有美白亮肤功效的外用植物提取物、化妆品及其制备方法 WO2019137387A1 (zh)

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