CN118236306B - Mugwort leaf extract and application thereof in cosmetics - Google Patents
Mugwort leaf extract and application thereof in cosmetics Download PDFInfo
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- 239000000284 extract Substances 0.000 title claims abstract description 146
- 235000003261 Artemisia vulgaris Nutrition 0.000 title claims abstract description 62
- 239000002537 cosmetic Substances 0.000 title claims abstract description 15
- 241000269837 Artemisia dubia Species 0.000 title 1
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims abstract description 96
- 240000006891 Artemisia vulgaris Species 0.000 claims abstract description 59
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 47
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 43
- 235000002020 sage Nutrition 0.000 claims abstract description 42
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims abstract description 32
- 244000178870 Lavandula angustifolia Species 0.000 claims abstract description 27
- 235000010663 Lavandula angustifolia Nutrition 0.000 claims abstract description 27
- 239000001102 lavandula vera Substances 0.000 claims abstract description 27
- 235000018219 lavender Nutrition 0.000 claims abstract description 27
- 238000002386 leaching Methods 0.000 claims abstract 3
- 239000012071 phase Substances 0.000 claims description 66
- 239000008346 aqueous phase Substances 0.000 claims description 58
- 239000012141 concentrate Substances 0.000 claims description 56
- 239000007788 liquid Substances 0.000 claims description 43
- 241000196324 Embryophyta Species 0.000 claims description 40
- 239000002994 raw material Substances 0.000 claims description 38
- 238000000605 extraction Methods 0.000 claims description 33
- IIEWJVIFRVWJOD-UHFFFAOYSA-N ethyl cyclohexane Natural products CCC1CCCCC1 IIEWJVIFRVWJOD-UHFFFAOYSA-N 0.000 claims description 27
- 238000002360 preparation method Methods 0.000 claims description 25
- 238000003756 stirring Methods 0.000 claims description 18
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000002156 mixing Methods 0.000 claims 1
- 239000003921 oil Substances 0.000 abstract description 55
- 239000007864 aqueous solution Substances 0.000 abstract description 19
- 230000003020 moisturizing effect Effects 0.000 abstract description 11
- 239000000126 substance Substances 0.000 abstract description 6
- 230000003078 antioxidant effect Effects 0.000 abstract description 5
- 239000004480 active ingredient Substances 0.000 abstract description 4
- 239000003963 antioxidant agent Substances 0.000 abstract description 3
- 239000000341 volatile oil Substances 0.000 abstract description 3
- 239000004615 ingredient Substances 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 29
- 239000000706 filtrate Substances 0.000 description 25
- 230000000694 effects Effects 0.000 description 24
- 235000009051 Ambrosia paniculata var. peruviana Nutrition 0.000 description 23
- 235000003097 Artemisia absinthium Nutrition 0.000 description 23
- 235000017731 Artemisia dracunculus ssp. dracunculus Nutrition 0.000 description 23
- 239000001138 artemisia absinthium Substances 0.000 description 23
- HHEAADYXPMHMCT-UHFFFAOYSA-N dpph Chemical compound [O-][N+](=O)C1=CC([N+](=O)[O-])=CC([N+]([O-])=O)=C1[N]N(C=1C=CC=CC=1)C1=CC=CC=C1 HHEAADYXPMHMCT-UHFFFAOYSA-N 0.000 description 23
- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid Chemical compound OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 23
- 239000000243 solution Substances 0.000 description 21
- 239000000203 mixture Substances 0.000 description 19
- 239000000419 plant extract Substances 0.000 description 13
- 238000005292 vacuum distillation Methods 0.000 description 13
- 230000007760 free radical scavenging Effects 0.000 description 12
- 239000012528 membrane Substances 0.000 description 12
- 239000011148 porous material Substances 0.000 description 12
- 150000003254 radicals Chemical class 0.000 description 12
- 239000000047 product Substances 0.000 description 9
- 239000001296 salvia officinalis l. Substances 0.000 description 9
- 238000000034 method Methods 0.000 description 6
- 230000002000 scavenging effect Effects 0.000 description 6
- 238000002835 absorbance Methods 0.000 description 5
- 239000012085 test solution Substances 0.000 description 5
- 230000002292 Radical scavenging effect Effects 0.000 description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 4
- TUJKJAMUKRIRHC-UHFFFAOYSA-N hydroxyl Chemical compound [OH] TUJKJAMUKRIRHC-UHFFFAOYSA-N 0.000 description 4
- 230000001737 promoting effect Effects 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 235000003826 Artemisia Nutrition 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 244000030166 artemisia Species 0.000 description 2
- 235000009052 artemisia Nutrition 0.000 description 2
- 239000001522 artemisia absinthium l. herb extract Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- 229940119569 wormwood extract Drugs 0.000 description 2
- CASFCVRUBIJLBN-UHFFFAOYSA-N 2-(1,10-phenanthrolin-2-yl)ethanol Chemical compound OCCc1ccc2ccc3cccnc3c2n1 CASFCVRUBIJLBN-UHFFFAOYSA-N 0.000 description 1
- 208000003351 Melanosis Diseases 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 230000002421 anti-septic effect Effects 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 230000001815 facial effect Effects 0.000 description 1
- 239000006210 lotion Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005374 membrane filtration Methods 0.000 description 1
- 239000002674 ointment Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000008363 phosphate buffer Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 230000037072 sun protection Effects 0.000 description 1
Classifications
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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
- A61K8/9783—Angiosperms [Magnoliophyta]
- A61K8/9789—Magnoliopsida [dicotyledons]
-
- 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
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0288—Applications, solvents
-
- 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
- A61K2800/80—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
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Veterinary Medicine (AREA)
- Public Health (AREA)
- General Health & Medical Sciences (AREA)
- Dermatology (AREA)
- Chemical & Material Sciences (AREA)
- Gerontology & Geriatric Medicine (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Biotechnology (AREA)
- Botany (AREA)
- Microbiology (AREA)
- Mycology (AREA)
- Birds (AREA)
- Epidemiology (AREA)
- Cosmetics (AREA)
Abstract
Description
技术领域Technical Field
本发明属于日化品技术领域,具体地涉及一种艾叶提取物及其在化妆品中的应用。The invention belongs to the technical field of daily chemical products, and specifically relates to an wormwood leaf extract and application thereof in cosmetics.
背景技术Background technique
化妆品是满足人们对“美”需求的日用消费品,已然成为生活中不可或缺的日常生活用品。化妆品是以涂擦、喷洒或者其他类似方法,施用于皮肤、毛发、指甲、口唇等人体表面,以清洁、保护、美化、修饰为目的的日用化学工业产品。Cosmetics are daily consumer goods that meet people's needs for "beauty" and have become an indispensable daily necessity in life. Cosmetics are daily chemical industrial products that are applied to the skin, hair, nails, lips and other human surfaces by rubbing, spraying or other similar methods for the purpose of cleaning, protecting, beautifying and modifying.
植物提取物是指以物理、化学和生物学等手段分离纯化植物原料中的某一种或多种有效成分为目的而形成的以生物小分子和高分子为主体的植物产品。植物提取物作为活性成分配制的化妆品与传统化妆品相比,具有很多优点:克服了传统化妆品依赖化学合成品的缺点,使产品的安全性能更高;天然植物的提取物更容易被皮肤吸收,所得到的产品的效果更为显著;功能性更突出等。植物提取物在化妆品中的作用主要有:保湿、抗衰老、祛斑、防晒、防腐等,并且植物提取物是绿色、安全的。选择合适的植物提取物、使用合适的植物提取物的量添加到化妆品产品中,才能最大地发挥其作用。Plant extracts refer to plant products mainly composed of small biological molecules and macromolecules, which are formed by separating and purifying one or more effective ingredients in plant raw materials by physical, chemical and biological means. Compared with traditional cosmetics, cosmetics formulated with plant extracts as active ingredients have many advantages: they overcome the shortcomings of traditional cosmetics that rely on chemical synthetic products, making the product safer; natural plant extracts are more easily absorbed by the skin, and the effects of the resulting products are more significant; the functionality is more prominent, etc. The main functions of plant extracts in cosmetics are: moisturizing, anti-aging, freckle removal, sun protection, antiseptic, etc., and plant extracts are green and safe. Only by selecting the right plant extracts and adding the right amount of plant extracts to cosmetic products can their effects be maximized.
关于将艾叶、鼠尾草、薰衣草和橙花进行共同提取得到植物提取物的研究没有公开或者报道过,同时,通过进一步优化提取工艺增强提取物的保湿和抗氧化效果的研究也相对较少。因此,提供一种技术方案,以实现对艾叶、鼠尾草、薰衣草和橙花的提取以及进一步增强保湿和抗氧化效果,是目前亟需解决的技术问题之一。There is no public or reported research on extracting plant extracts from wormwood, sage, lavender and orange blossoms. At the same time, there are relatively few studies on further optimizing the extraction process to enhance the moisturizing and antioxidant effects of the extracts. Therefore, providing a technical solution to extract wormwood, sage, lavender and orange blossoms and further enhance the moisturizing and antioxidant effects is one of the technical problems that need to be solved urgently.
发明内容Summary of the invention
本发明是针对上述技术问题所提出的,本发明涉及日化品技术领域,更具体地涉及一种艾叶提取物及其在化妆品中的应用。The present invention is proposed in view of the above technical problems. The present invention relates to the technical field of daily chemical products, and more specifically to an wormwood leaf extract and its application in cosmetics.
本发明的技术方案具体如下。The technical solution of the present invention is specifically as follows.
一方面地,本发明技术方案包括一种艾叶提取物,所述提取物的制备中使用的植物原料为:1-4份艾叶,0.5-3.5份鼠尾草,0.5-3份薰衣草和0.4-2.5份橙花,以质量份计。On the one hand, the technical solution of the present invention includes an artemisia leaf extract, and the plant raw materials used in the preparation of the extract are: 1-4 parts of artemisia leaf, 0.5-3.5 parts of sage, 0.5-3 parts of lavender and 0.4-2.5 parts of orange blossom, calculated by mass.
作为优选地,所述艾叶提取物的制备包括如下步骤:Preferably, the preparation of the wormwood extract comprises the following steps:
步骤1:按照上述质量份,将艾叶、鼠尾草、薰衣草和橙花混合,加入水,破碎,得到破碎液;Step 1: Mix wormwood leaves, sage, lavender and orange blossom according to the above mass parts, add water, and crush to obtain a crushed liquid;
步骤2:在破碎液中加入乙醇水溶液,搅拌,得到浸提液;Step 2: adding ethanol aqueous solution to the crushing liquid, stirring, and obtaining an extract;
步骤3:将浸提液浓缩,得到浓缩物,浓缩物中加入由油相、水相组成的萃取剂,萃取,将水相倒出,得到萃取物;Step 3: Concentrating the extract to obtain a concentrate, adding an extractant consisting of an oil phase and an aqueous phase to the concentrate, extracting, and pouring out the aqueous phase to obtain an extract;
步骤4:将萃取物过滤,滤液浓缩,干燥,得到所述艾叶提取物。Step 4: Filter the extract, concentrate the filtrate, and dry it to obtain the wormwood leaf extract.
作为优选地,所述艾叶提取物的制备包括如下步骤:Preferably, the preparation of the wormwood extract comprises the following steps:
步骤1:按照上述质量份,将艾叶、鼠尾草、薰衣草和橙花混合,加入植物原料质量1.5-3倍的水,破碎,得到破碎液;Step 1: Mix wormwood leaves, sage, lavender and orange blossom according to the above mass parts, add water 1.5-3 times the mass of the plant raw materials, and crush them to obtain a crushed liquid;
步骤2:在破碎液中加入相较于破碎液质量4-10倍的质量浓度为45%-60%的乙醇水溶液,搅拌20-60小时,得到浸提液;Step 2: adding 45%-60% ethanol aqueous solution with a mass concentration of 4-10 times the mass of the crushing liquid to the crushing liquid, stirring for 20-60 hours to obtain an extract;
步骤3:将浸提液浓缩,得到浓缩物,浓缩物中加入由油相、水相组成的萃取剂,30℃-50℃萃取4-10小时,将水相倒出,得到萃取物;Step 3: Concentrate the extract to obtain a concentrate, add an extractant consisting of an oil phase and an aqueous phase to the concentrate, extract at 30° C.-50° C. for 4-10 hours, and pour out the aqueous phase to obtain an extract;
步骤4:将萃取物过滤,滤液浓缩,干燥,得到所述艾叶提取物;Step 4: filtering the extract, concentrating the filtrate, and drying to obtain the wormwood leaf extract;
其中,萃取剂中水相由水组成;油相由乙酸乙酯和环己烷按照质量为1:3-5组成;水相和油相的质量比为1:2-4;The aqueous phase in the extractant is composed of water; the oil phase is composed of ethyl acetate and cyclohexane in a mass ratio of 1:3-5; the mass ratio of the aqueous phase to the oil phase is 1:2-4;
步骤3中的浓缩物和萃取剂的质量比为1:8-25。The mass ratio of the concentrate to the extractant in step 3 is 1:8-25.
作为优选地,所述艾叶和鼠尾草的质量比为1-2:1、1.1-1.8:1或1.2-1.6:1。Preferably, the mass ratio of the wormwood leaf to the sage is 1-2:1, 1.1-1.8:1 or 1.2-1.6:1.
作为优选地,所述步骤1中水和植物原料的质量比为1.8-3:1、2-2.8:1或2.2-2.7:1。Preferably, in step 1, the mass ratio of water to plant material is 1.8-3:1, 2-2.8:1 or 2.2-2.7:1.
作为优选地,所述步骤2中乙醇水溶液和破碎液的质量比为5-10:1、5.5-9.5:1或6-9:1。Preferably, in step 2, the mass ratio of the ethanol aqueous solution to the crushing liquid is 5-10:1, 5.5-9.5:1 or 6-9:1.
作为优选地,所述步骤2中乙醇水溶液的质量浓度为46%-58%、48%-55%或50%-55%。Preferably, the mass concentration of the ethanol aqueous solution in step 2 is 46%-58%, 48%-55% or 50%-55%.
作为优选地,所述步骤2中的搅拌是在温度为35℃-60℃、40℃-60℃、42℃-55℃下进行。Preferably, the stirring in step 2 is carried out at a temperature of 35°C-60°C, 40°C-60°C, or 42°C-55°C.
作为优选地,所述步骤2中搅拌的时间为22-55小时、24-52小时或25-50小时。Preferably, the stirring time in step 2 is 22-55 hours, 24-52 hours or 25-50 hours.
作为优选地,所述步骤2中搅拌的转速为50-1000转/分、60-800转/分或70-500转/分。Preferably, the stirring speed in step 2 is 50-1000 rpm, 60-800 rpm or 70-500 rpm.
作为优选地,所述步骤3中浓缩为减压浓缩,减压浓缩的温度为55℃-65℃、58℃-64℃或60℃-63℃。Preferably, the concentration in step 3 is reduced-pressure concentration, and the temperature of the reduced-pressure concentration is 55°C-65°C, 58°C-64°C or 60°C-63°C.
作为优选地,所述步骤3中浓缩至浸提液质量的10%-25%、12%-20%或12%-18%。Preferably, in step 3, the extract is concentrated to 10%-25%, 12%-20% or 12%-18% of the mass of the extract.
作为优选地,所述步骤3中的浓缩物和萃取剂的质量比为1:10-20、1:12-18或1:12-16。Preferably, the mass ratio of the concentrate to the extractant in step 3 is 1:10-20, 1:12-18 or 1:12-16.
作为优选地,所述步骤3中的油相由乙酸乙酯和环己烷按照质量为1:3-4.5、1:3.5-4.5或1:3.8-4.2组成。Preferably, the oil phase in step 3 is composed of ethyl acetate and cyclohexane in a mass ratio of 1:3-4.5, 1:3.5-4.5 or 1:3.8-4.2.
作为优选地,所述步骤3中水相和油相的质量比为1:2.5-4、1:2.5-3.5或1:2.8-3.2。Preferably, the mass ratio of the water phase to the oil phase in step 3 is 1:2.5-4, 1:2.5-3.5 or 1:2.8-3.2.
作为优选地,所述步骤3中萃取温度为30℃-45℃、32℃-45℃或35℃-40℃。Preferably, the extraction temperature in step 3 is 30°C-45°C, 32°C-45°C or 35°C-40°C.
作为优选地,所述步骤3中萃取时间为4.5-10小时、5-9小时或5.5-8小时。Preferably, the extraction time in step 3 is 4.5-10 hours, 5-9 hours or 5.5-8 hours.
作为优选地,所述步骤4中过滤选择滤膜过滤,所述滤膜的孔径低于10微米。Preferably, in step 4, filtration is performed by membrane filtration, and the pore size of the membrane is less than 10 microns.
作为优选地,所述步骤4中浓缩为减压蒸馏进行浓缩,减压蒸馏进行浓缩的温度为35℃-45℃、38℃-44℃或39℃-43℃。Preferably, the concentration in step 4 is carried out by vacuum distillation, and the temperature for the vacuum distillation is 35°C-45°C, 38°C-44°C or 39°C-43°C.
作为优选地,所述步骤4中浓缩至过滤液质量的10%-20%、12%-18%或12%-17%。Preferably, in step 4, the concentration is to 10%-20%, 12%-18% or 12%-17% of the mass of the filtrate.
作为优选地,所述步骤4中干燥为真空干燥。真空干燥的温度为45℃-50℃,压力为0.01MPa-0.025MPa,时间为3-20小时。Preferably, the drying in step 4 is vacuum drying. The vacuum drying temperature is 45° C.-50° C., the pressure is 0.01 MPa-0.025 MPa, and the time is 3-20 hours.
另一方面地,本发明还提供将所述艾叶提取物在制备化妆品中的应用。On the other hand, the present invention also provides the use of the wormwood leaf extract in preparing cosmetics.
作为优选地,所述化妆品包括精华、乳液、面膜、霜、膏、粉底等。Preferably, the cosmetics include essence, lotion, facial mask, cream, ointment, foundation and the like.
作为优选地,所述艾叶提取物在化妆品中的质量用量为0.01%-10%、0.05%-8%、0.1%-5%、0.2%-2.5%等。Preferably, the mass dosage of the wormwood leaf extract in cosmetics is 0.01%-10%, 0.05%-8%, 0.1%-5%, 0.2%-2.5%, etc.
本发明的有益效果如下:The beneficial effects of the present invention are as follows:
本发明采用艾叶、鼠尾草、薰衣草和橙花加水破碎,然后使用乙醇水溶液进行浸提,并采取由乙酸乙酯和环己烷组成的油相与水相搭配得到的萃取剂进行萃取,然后进行后处理,能实现对艾叶、鼠尾草、薰衣草和橙花的油性活性成分,例如精油等组分,以及对有机物等成分进行有效提取,赋予提取物优异的抗氧化和保湿效果。The invention adopts the method of adding water to wormwood, sage, lavender and orange blossom to crush them, then using ethanol water solution for extraction, and using an extractant obtained by combining an oil phase composed of ethyl acetate and cyclohexane with a water phase for extraction, and then performing post-treatment, so as to effectively extract oily active ingredients of wormwood, sage, lavender and orange blossom, such as components such as essential oils, and components such as organic matter, and give the extract excellent antioxidant and moisturizing effects.
本发明提取方法所得到的艾叶提取物具有优异的DPPH自由基清除效果,且DPPH自由基清除效率达到87.52%。The wormwood leaf extract obtained by the extraction method of the present invention has an excellent DPPH free radical scavenging effect, and the DPPH free radical scavenging efficiency reaches 87.52%.
本发明采用艾叶、鼠尾草两者的搭配能进一步提高清除DPPH自由基效果,两者在促进清除DPPH自由基效果上具有相互促进的复配关系。当艾叶和鼠尾草的用量比例达到1-2:1时,制备体系所得到的提取物的清除DPPH自由基效果更优。The present invention uses a combination of wormwood and sage to further improve the effect of scavenging DPPH free radicals, and the two have a mutually promoting compound relationship in promoting the effect of scavenging DPPH free radicals. When the usage ratio of wormwood and sage reaches 1-2:1, the extract obtained by the preparation system has a better effect of scavenging DPPH free radicals.
本发明采用由乙酸乙酯和环己烷组成的油相与水相搭配得到的萃取剂进行萃取,得到的提取物清除DPPH自由基的效果优异;本发明油相选择乙酸乙酯和环己烷进行萃取所赋予清除自由基的效果更优。本发明制备体系中的乙酸乙酯和环己烷比例在1:3-5范围内时,所得到的提取物清除DPPH自由基效果更好。The present invention uses an extractant obtained by combining an oil phase composed of ethyl acetate and cyclohexane with an aqueous phase for extraction, and the obtained extract has an excellent effect of removing DPPH free radicals; the oil phase of the present invention selects ethyl acetate and cyclohexane for extraction, which gives a better effect of removing free radicals. When the ratio of ethyl acetate to cyclohexane in the preparation system of the present invention is within the range of 1:3-5, the obtained extract has a better effect of removing DPPH free radicals.
本发明方法所得到植物提取物,具有优异的羟自由基清除效果,且羟自由基清除效率达到82.34%。The plant extract obtained by the method of the present invention has an excellent hydroxyl free radical scavenging effect, and the hydroxyl free radical scavenging efficiency reaches 82.34%.
本发明提取方法所得到植物提取物,具有优异的增加肌肤含水量的效果;在使用本发明提取物2小时,能增加肌肤含水量的比例达到45.72%;在使用本发明提取物6小时,能增加肌肤含水量的比例达到30.48%;在使用本发明提取物10小时,能增加肌肤含水量的比例达到18.54%。The plant extract obtained by the extraction method of the present invention has an excellent effect of increasing the moisture content of the skin; after using the extract of the present invention for 2 hours, the moisture content of the skin can be increased by 45.72%; after using the extract of the present invention for 6 hours, the moisture content of the skin can be increased by 30.48%; after using the extract of the present invention for 10 hours, the moisture content of the skin can be increased by 18.54%.
本发明采用由乙酸乙酯和环己烷组成的油相与水相搭配得到的萃取剂进行萃取,得到的提取物增加肌肤含水量的效果优异;本发明油相选择乙酸乙酯和环己烷搭配相较于其他油相所得的萃取剂进行萃取所得到的提取物,增加皮肤含水量的效果更为显著。且本发明制备体系中的乙酸乙酯和环己烷比例在1:3-5范围内时,所得到的提取物保湿肌肤效果更好。The present invention uses an extractant obtained by combining an oil phase composed of ethyl acetate and cyclohexane with an aqueous phase for extraction, and the obtained extract has an excellent effect of increasing the moisture content of the skin; the extract obtained by combining ethyl acetate and cyclohexane in the oil phase of the present invention has a more significant effect of increasing the moisture content of the skin than the extractant obtained by other oil phases. When the ratio of ethyl acetate to cyclohexane in the preparation system of the present invention is within the range of 1:3-5, the obtained extract has a better effect of moisturizing the skin.
本发明得到的产品效果优异,具有较好的应用前景。The product obtained by the invention has excellent effect and good application prospect.
具体实施方式Detailed ways
下文将结合具体实施方式阐述本发明的技术方案,本发明技术方案的效果将因此而更清楚和具体化。The technical solution of the present invention will be described below in conjunction with specific implementation methods, and the effects of the technical solution of the present invention will be made clearer and more specific.
一、提取物的制备1. Preparation of Extracts
提取物1:Extract 1:
具体制备方案如下:步骤1:按照质量份称取植物原料:3份艾叶,2份鼠尾草,1.2份薰衣草和0.8份橙花;将植物原料混合,加入植物原料总质量2.3倍的水,破碎,得到破碎液;The specific preparation scheme is as follows: Step 1: Weigh plant raw materials according to mass: 3 parts of mugwort, 2 parts of sage, 1.2 parts of lavender and 0.8 parts of orange blossom; mix the plant raw materials, add 2.3 times the total mass of water of the plant raw materials, and crush them to obtain a crushed liquid;
步骤2:在破碎液中加入相较于破碎液质量8倍的质量浓度为52%的乙醇水溶液,在温度为45℃、转速为80转/分搅拌30小时,得到浸提液;Step 2: adding 52% ethanol aqueous solution with a mass concentration of 8 times the mass of the crushing liquid to the crushing liquid, stirring at a temperature of 45° C. and a rotation speed of 80 rpm for 30 hours to obtain an extract;
步骤3:将浸提液在温度为62.5℃进行减压浓缩至浸提液质量的15%,得到浓缩物;浓缩物中加入由油相、水相组成的萃取剂,38℃萃取6.5小时,将水相倒出,得到萃取物;Step 3: The extract is concentrated under reduced pressure at a temperature of 62.5° C. to 15% of the mass of the extract to obtain a concentrate; an extractant consisting of an oil phase and an aqueous phase is added to the concentrate, and extraction is performed at 38° C. for 6.5 hours, and the aqueous phase is poured out to obtain an extract;
步骤4:将萃取物采用孔径为1微米的滤膜过滤,滤液在42℃减压蒸馏进行浓缩,至滤液质量的15%;然后在温度为50℃、压力为0.012MPa下真空干燥6.2小时,得到提取物;Step 4: Filter the extract through a filter membrane with a pore size of 1 micron, and concentrate the filtrate by vacuum distillation at 42°C to 15% of the filtrate mass; then vacuum dry at a temperature of 50°C and a pressure of 0.012MPa for 6.2 hours to obtain an extract;
其中,萃取剂中水相由水组成;油相由乙酸乙酯和环己烷按照质量为1:4组成;水相和油相的质量比为1:3;步骤3中的浓缩物和萃取剂的质量比为1:12;步骤1中艾叶和鼠尾草的质量比为1.5:1。Among them, the aqueous phase in the extractant is composed of water; the oil phase is composed of ethyl acetate and cyclohexane in a mass ratio of 1:4; the mass ratio of the aqueous phase to the oil phase is 1:3; the mass ratio of the concentrate to the extractant in step 3 is 1:12; the mass ratio of mugwort and sage in step 1 is 1.5:1.
提取物2:Extract 2:
具体制备方案如下:步骤1:按照质量份称取植物原料:2.5份艾叶,2.5份鼠尾草,1份薰衣草和1份橙花;将植物原料混合,加入植物原料总质量2.3倍的水,破碎,得到破碎液;The specific preparation scheme is as follows: Step 1: Weigh plant raw materials according to mass: 2.5 parts of mugwort, 2.5 parts of sage, 1 part of lavender and 1 part of orange blossom; mix the plant raw materials, add 2.3 times the total mass of water of the plant raw materials, and crush them to obtain a crushed liquid;
步骤2:在破碎液中加入相较于破碎液质量8倍的质量浓度为55%的乙醇水溶液,在温度为43℃、转速为70转/分搅拌25小时,得到浸提液;Step 2: adding 55% ethanol aqueous solution with a mass concentration of 8 times that of the crushing liquid to the crushing liquid, stirring at a temperature of 43° C. and a rotation speed of 70 rpm for 25 hours to obtain an extract;
步骤3:将浸提液在温度为62℃进行减压浓缩至浸提液质量的15%,得到浓缩物;浓缩物中加入由油相、水相组成的萃取剂,40℃萃取6小时,将水相倒出,得到萃取物;Step 3: The extract is concentrated under reduced pressure at 62° C. to 15% of the mass of the extract to obtain a concentrate; an extractant consisting of an oil phase and an aqueous phase is added to the concentrate, and extraction is performed at 40° C. for 6 hours, and the aqueous phase is poured out to obtain an extract;
步骤4:将萃取物采用孔径为1微米的滤膜过滤,滤液在40℃减压蒸馏进行浓缩,至滤液质量的15%;然后在温度为52℃、压力为0.014MPa下真空干燥6小时,得到提取物;Step 4: Filter the extract through a filter membrane with a pore size of 1 micron, and concentrate the filtrate by vacuum distillation at 40°C to 15% of the filtrate mass; then vacuum dry at a temperature of 52°C and a pressure of 0.014 MPa for 6 hours to obtain an extract;
其中,萃取剂中水相由水组成;油相由乙酸乙酯和环己烷按照质量为1:3组成;水相和油相的质量比为1:3;步骤3中的浓缩物和萃取剂的质量比为1:12;步骤1中艾叶和鼠尾草的质量比为1:1。Among them, the aqueous phase in the extractant is composed of water; the oil phase is composed of ethyl acetate and cyclohexane in a mass ratio of 1:3; the mass ratio of the aqueous phase to the oil phase is 1:3; the mass ratio of the concentrate to the extractant in step 3 is 1:12; the mass ratio of mugwort and sage in step 1 is 1:1.
提取物3:Extract 3:
具体制备方案如下:步骤1:按照质量份称取植物原料:5份鼠尾草,1.2份薰衣草和0.8份橙花;将植物原料混合,加入植物原料总质量2.3倍的水,破碎,得到破碎液;The specific preparation scheme is as follows: Step 1: Weigh plant raw materials according to mass: 5 parts of sage, 1.2 parts of lavender and 0.8 parts of orange blossom; mix the plant raw materials, add 2.3 times the total mass of water of the plant raw materials, and crush them to obtain a crushed liquid;
步骤2:在破碎液中加入相较于破碎液质量8倍的质量浓度为52%的乙醇水溶液,在温度为45℃、转速为80转/分搅拌30小时,得到浸提液;Step 2: adding 52% ethanol aqueous solution with a mass concentration of 8 times the mass of the crushing liquid to the crushing liquid, stirring at a temperature of 45° C. and a rotation speed of 80 rpm for 30 hours to obtain an extract;
步骤3:将浸提液在温度为62.5℃进行减压浓缩至浸提液质量的15%,得到浓缩物;浓缩物中加入由油相、水相组成的萃取剂,38℃萃取6.5小时,将水相倒出,得到萃取物;Step 3: The extract is concentrated under reduced pressure at a temperature of 62.5° C. to 15% of the mass of the extract to obtain a concentrate; an extractant consisting of an oil phase and an aqueous phase is added to the concentrate, and extraction is performed at 38° C. for 6.5 hours, and the aqueous phase is poured out to obtain an extract;
步骤4:将萃取物采用孔径为1微米的滤膜过滤,滤液在42℃减压蒸馏进行浓缩,至滤液质量的15%;然后在温度为50℃、压力为0.012MPa下真空干燥6.2小时,得到提取物;Step 4: Filter the extract through a filter membrane with a pore size of 1 micron, and concentrate the filtrate by vacuum distillation at 42°C to 15% of the filtrate mass; then vacuum dry at a temperature of 50°C and a pressure of 0.012MPa for 6.2 hours to obtain an extract;
其中,萃取剂中水相由水组成;油相由乙酸乙酯和环己烷按照质量为1:4组成;水相和油相的质量比为1:3;步骤3中的浓缩物和萃取剂的质量比为1:12。Among them, the aqueous phase in the extractant is composed of water; the oil phase is composed of ethyl acetate and cyclohexane in a mass ratio of 1:4; the mass ratio of the aqueous phase to the oil phase is 1:3; the mass ratio of the concentrate to the extractant in step 3 is 1:12.
提取物4:Extract 4:
具体制备方案如下:步骤1:按照质量份称取植物原料:5份艾叶,1.2份薰衣草和0.8份橙花;将植物原料混合,加入植物原料总质量2.3倍的水,破碎,得到破碎液;The specific preparation scheme is as follows: Step 1: Weigh plant raw materials according to mass: 5 parts of mugwort, 1.2 parts of lavender and 0.8 parts of orange blossom; mix the plant raw materials, add 2.3 times the total mass of water of the plant raw materials, and crush them to obtain a crushed liquid;
步骤2:在破碎液中加入相较于破碎液质量8倍的质量浓度为52%的乙醇水溶液,在温度为45℃、转速为80转/分搅拌30小时,得到浸提液;Step 2: adding 52% ethanol aqueous solution with a mass concentration of 8 times the mass of the crushing liquid to the crushing liquid, stirring at a temperature of 45° C. and a rotation speed of 80 rpm for 30 hours to obtain an extract;
步骤3:将浸提液在温度为62.5℃进行减压浓缩至浸提液质量的15%,得到浓缩物;浓缩物中加入由油相、水相组成的萃取剂,38℃萃取6.5小时,将水相倒出,得到萃取物;Step 3: The extract is concentrated under reduced pressure at a temperature of 62.5° C. to 15% of the mass of the extract to obtain a concentrate; an extractant consisting of an oil phase and an aqueous phase is added to the concentrate, and extraction is performed at 38° C. for 6.5 hours, and the aqueous phase is poured out to obtain an extract;
步骤4:将萃取物采用孔径为1微米的滤膜过滤,滤液在42℃减压蒸馏进行浓缩,至滤液质量的15%;然后在温度为50℃、压力为0.012MPa下真空干燥6.2小时,得到提取物;Step 4: Filter the extract through a filter membrane with a pore size of 1 micron, and concentrate the filtrate by vacuum distillation at 42°C to 15% of the filtrate mass; then vacuum dry at a temperature of 50°C and a pressure of 0.012MPa for 6.2 hours to obtain an extract;
其中,萃取剂中水相由水组成;油相由乙酸乙酯和环己烷按照质量为1:4组成;水相和油相的质量比为1:3;步骤3中的浓缩物和萃取剂的质量比为1:12。Among them, the aqueous phase in the extractant is composed of water; the oil phase is composed of ethyl acetate and cyclohexane in a mass ratio of 1:4; the mass ratio of the aqueous phase to the oil phase is 1:3; the mass ratio of the concentrate to the extractant in step 3 is 1:12.
提取物5:Extract 5:
具体制备方案如下:步骤1:按照质量份称取植物原料:1.6份艾叶,3.4份鼠尾草,1.2份薰衣草和0.8份橙花;将植物原料混合,加入植物原料总质量2.3倍的水,破碎,得到破碎液;The specific preparation scheme is as follows: Step 1: Weigh plant raw materials according to mass: 1.6 parts of mugwort, 3.4 parts of sage, 1.2 parts of lavender and 0.8 parts of orange blossom; mix the plant raw materials, add 2.3 times the total mass of water of the plant raw materials, and crush them to obtain a crushed liquid;
步骤2:在破碎液中加入相较于破碎液质量8倍的质量浓度为52%的乙醇水溶液,在温度为45℃、转速为80转/分搅拌30小时,得到浸提液;Step 2: adding 52% ethanol aqueous solution with a mass concentration of 8 times the mass of the crushing liquid to the crushing liquid, stirring at a temperature of 45° C. and a rotation speed of 80 rpm for 30 hours to obtain an extract;
步骤3:将浸提液在温度为62.5℃进行减压浓缩至浸提液质量的15%,得到浓缩物;浓缩物中加入由油相、水相组成的萃取剂,38℃萃取6.5小时,将水相倒出,得到萃取物;Step 3: The extract is concentrated under reduced pressure at a temperature of 62.5° C. to 15% of the mass of the extract to obtain a concentrate; an extractant consisting of an oil phase and an aqueous phase is added to the concentrate, and extraction is performed at 38° C. for 6.5 hours, and the aqueous phase is poured out to obtain an extract;
步骤4:将萃取物采用孔径为1微米的滤膜过滤,滤液在42℃减压蒸馏进行浓缩,至滤液质量的15%;然后在温度为50℃、压力为0.012MPa下真空干燥6.2小时,得到提取物;Step 4: Filter the extract through a filter membrane with a pore size of 1 micron, and concentrate the filtrate by vacuum distillation at 42°C to 15% of the filtrate mass; then vacuum dry at a temperature of 50°C and a pressure of 0.012MPa for 6.2 hours to obtain an extract;
其中,萃取剂中水相由水组成;油相由乙酸乙酯和环己烷按照质量为1:4组成;水相和油相的质量比为1:3;步骤3中的浓缩物和萃取剂的质量比为1:12;步骤1中艾叶和鼠尾草的质量比为0.47:1。Among them, the aqueous phase in the extractant is composed of water; the oil phase is composed of ethyl acetate and cyclohexane in a mass ratio of 1:4; the mass ratio of the aqueous phase to the oil phase is 1:3; the mass ratio of the concentrate to the extractant in step 3 is 1:12; the mass ratio of mugwort and sage in step 1 is 0.47:1.
提取物6:Extract 6:
具体制备方案如下:步骤1:按照质量份称取植物原料:4份艾叶,1份鼠尾草,1.2份薰衣草和0.8份橙花;将植物原料混合,加入植物原料总质量2.3倍的水,破碎,得到破碎液;The specific preparation scheme is as follows: Step 1: Weigh plant raw materials according to mass: 4 parts of mugwort, 1 part of sage, 1.2 parts of lavender and 0.8 parts of orange blossom; mix the plant raw materials, add 2.3 times the total mass of water of the plant raw materials, and crush them to obtain a crushed liquid;
步骤2:在破碎液中加入相较于破碎液质量8倍的质量浓度为52%的乙醇水溶液,在温度为45℃、转速为80转/分搅拌30小时,得到浸提液;Step 2: adding 52% ethanol aqueous solution with a mass concentration of 8 times the mass of the crushing liquid to the crushing liquid, stirring at a temperature of 45° C. and a rotation speed of 80 rpm for 30 hours to obtain an extract;
步骤3:将浸提液在温度为62.5℃进行减压浓缩至浸提液质量的15%,得到浓缩物;浓缩物中加入由油相、水相组成的萃取剂,38℃萃取6.5小时,将水相倒出,得到萃取物;Step 3: The extract is concentrated under reduced pressure at a temperature of 62.5° C. to 15% of the mass of the extract to obtain a concentrate; an extractant consisting of an oil phase and an aqueous phase is added to the concentrate, and extraction is performed at 38° C. for 6.5 hours, and the aqueous phase is poured out to obtain an extract;
步骤4:将萃取物采用孔径为1微米的滤膜过滤,滤液在42℃减压蒸馏进行浓缩,至滤液质量的15%;然后在温度为50℃、压力为0.012MPa下真空干燥6.2小时,得到提取物;Step 4: Filter the extract through a filter membrane with a pore size of 1 micron, and concentrate the filtrate by vacuum distillation at 42°C to 15% of the filtrate mass; then vacuum dry at a temperature of 50°C and a pressure of 0.012MPa for 6.2 hours to obtain an extract;
其中,萃取剂中水相由水组成;油相由乙酸乙酯和环己烷按照质量为1:4组成;水相和油相的质量比为1:3;步骤3中的浓缩物和萃取剂的质量比为1:12;步骤1中艾叶和鼠尾草的质量比为4:1。Among them, the aqueous phase in the extractant is composed of water; the oil phase is composed of ethyl acetate and cyclohexane in a mass ratio of 1:4; the mass ratio of the aqueous phase to the oil phase is 1:3; the mass ratio of the concentrate to the extractant in step 3 is 1:12; the mass ratio of mugwort and sage in step 1 is 4:1.
提取物7:Extract 7:
具体制备方案如下:步骤1:按照质量份称取植物原料:3份艾叶,2份鼠尾草,1.2份薰衣草和0.8份橙花;将植物原料混合,加入植物原料总质量2.3倍的水,破碎,得到破碎液;The specific preparation scheme is as follows: Step 1: Weigh plant raw materials according to mass: 3 parts of mugwort, 2 parts of sage, 1.2 parts of lavender and 0.8 parts of orange blossom; mix the plant raw materials, add 2.3 times the total mass of water of the plant raw materials, and crush them to obtain a crushed liquid;
步骤2:在破碎液中加入相较于破碎液质量8倍的质量浓度为52%的乙醇水溶液,在温度为45℃、转速为80转/分搅拌30小时,得到浸提液;Step 2: adding 52% ethanol aqueous solution with a mass concentration of 8 times the mass of the crushing liquid to the crushing liquid, stirring at a temperature of 45° C. and a rotation speed of 80 rpm for 30 hours to obtain an extract;
步骤3:将浸提液在温度为62.5℃进行减压浓缩至浸提液质量的15%,得到浓缩物;浓缩物中加入由油相、水相组成的萃取剂,38℃萃取6.5小时,将水相倒出,得到萃取物;Step 3: The extract is concentrated under reduced pressure at a temperature of 62.5° C. to 15% of the mass of the extract to obtain a concentrate; an extractant consisting of an oil phase and an aqueous phase is added to the concentrate, and extraction is performed at 38° C. for 6.5 hours, and the aqueous phase is poured out to obtain an extract;
步骤4:将萃取物采用孔径为1微米的滤膜过滤,滤液在42℃减压蒸馏进行浓缩,至滤液质量的15%;然后在温度为50℃、压力为0.012MPa下真空干燥6.2小时,得到提取物;Step 4: Filter the extract through a filter membrane with a pore size of 1 micron, and concentrate the filtrate by vacuum distillation at 42°C to 15% of the filtrate mass; then vacuum dry at a temperature of 50°C and a pressure of 0.012MPa for 6.2 hours to obtain an extract;
其中,萃取剂中水相由水组成;油相由乙酸乙酯和环己烷按照质量为1:1组成;水相和油相的质量比为1:3;步骤3中的浓缩物和萃取剂的质量比为1:12;步骤1中艾叶和鼠尾草的质量比为1.5:1。Among them, the aqueous phase in the extractant is composed of water; the oil phase is composed of ethyl acetate and cyclohexane in a mass ratio of 1:1; the mass ratio of the aqueous phase to the oil phase is 1:3; the mass ratio of the concentrate to the extractant in step 3 is 1:12; the mass ratio of mugwort and sage in step 1 is 1.5:1.
提取物8:Extract 8:
具体制备方案如下:步骤1:按照质量份称取植物原料:3份艾叶,2份鼠尾草,1.2份薰衣草和0.8份橙花;将植物原料混合,加入植物原料总质量2.3倍的水,破碎,得到破碎液;The specific preparation scheme is as follows: Step 1: Weigh plant raw materials according to mass: 3 parts of mugwort, 2 parts of sage, 1.2 parts of lavender and 0.8 parts of orange blossom; mix the plant raw materials, add 2.3 times the total mass of water of the plant raw materials, and crush them to obtain a crushed liquid;
步骤2:在破碎液中加入相较于破碎液质量8倍的质量浓度为52%的乙醇水溶液,在温度为45℃、转速为80转/分搅拌30小时,得到浸提液;Step 2: adding 52% ethanol aqueous solution with a mass concentration of 8 times the mass of the crushing liquid to the crushing liquid, stirring at a temperature of 45° C. and a rotation speed of 80 rpm for 30 hours to obtain an extract;
步骤3:将浸提液在温度为62.5℃进行减压浓缩至浸提液质量的15%,得到浓缩物;浓缩物中加入由油相、水相组成的萃取剂,38℃萃取6.5小时,将水相倒出,得到萃取物;Step 3: The extract is concentrated under reduced pressure at a temperature of 62.5° C. to 15% of the mass of the extract to obtain a concentrate; an extractant consisting of an oil phase and an aqueous phase is added to the concentrate, and extraction is performed at 38° C. for 6.5 hours, and the aqueous phase is poured out to obtain an extract;
步骤4:将萃取物采用孔径为1微米的滤膜过滤,滤液在42℃减压蒸馏进行浓缩,至滤液质量的15%;然后在温度为50℃、压力为0.012MPa下真空干燥6.2小时,得到提取物;Step 4: Filter the extract through a filter membrane with a pore size of 1 micron, and concentrate the filtrate by vacuum distillation at 42°C to 15% of the filtrate mass; then vacuum dry at a temperature of 50°C and a pressure of 0.012MPa for 6.2 hours to obtain an extract;
其中,萃取剂中水相由水组成;油相由乙酸乙酯和环己烷按照质量为1:2组成;水相和油相的质量比为1:3;步骤3中的浓缩物和萃取剂的质量比为1:12;步骤1中艾叶和鼠尾草的质量比为1.5:1。Among them, the aqueous phase in the extractant is composed of water; the oil phase is composed of ethyl acetate and cyclohexane in a mass ratio of 1:2; the mass ratio of the aqueous phase to the oil phase is 1:3; the mass ratio of the concentrate to the extractant in step 3 is 1:12; the mass ratio of mugwort and sage in step 1 is 1.5:1.
提取物9:Extract 9:
具体制备方案如下:步骤1:按照质量份称取植物原料:3份艾叶,2份鼠尾草,1.2份薰衣草和0.8份橙花;将植物原料混合,加入植物原料总质量2.3倍的水,破碎,得到破碎液;The specific preparation scheme is as follows: Step 1: Weigh plant raw materials according to mass: 3 parts of mugwort, 2 parts of sage, 1.2 parts of lavender and 0.8 parts of orange blossom; mix the plant raw materials, add 2.3 times the total mass of water of the plant raw materials, and crush them to obtain a crushed liquid;
步骤2:在破碎液中加入相较于破碎液质量8倍的质量浓度为52%的乙醇水溶液,在温度为45℃、转速为80转/分搅拌30小时,得到浸提液;Step 2: adding 52% ethanol aqueous solution with a mass concentration of 8 times the mass of the crushing liquid to the crushing liquid, stirring at a temperature of 45° C. and a rotation speed of 80 rpm for 30 hours to obtain an extract;
步骤3:将浸提液在温度为62.5℃进行减压浓缩至浸提液质量的15%,得到浓缩物;浓缩物中加入由油相、水相组成的萃取剂,38℃萃取6.5小时,将水相倒出,得到萃取物;Step 3: The extract is concentrated under reduced pressure at a temperature of 62.5° C. to 15% of the mass of the extract to obtain a concentrate; an extractant consisting of an oil phase and an aqueous phase is added to the concentrate, and extraction is performed at 38° C. for 6.5 hours, and the aqueous phase is poured out to obtain an extract;
步骤4:将萃取物采用孔径为1微米的滤膜过滤,滤液在42℃减压蒸馏进行浓缩,至滤液质量的15%;然后在温度为50℃、压力为0.012MPa下真空干燥6.2小时,得到提取物;Step 4: Filter the extract through a filter membrane with a pore size of 1 micron, and concentrate the filtrate by vacuum distillation at 42°C to 15% of the filtrate mass; then vacuum dry at a temperature of 50°C and a pressure of 0.012MPa for 6.2 hours to obtain an extract;
其中,萃取剂中水相由水组成;油相由乙酸乙酯和环己烷按照质量为1:6.5组成;水相和油相的质量比为1:3;步骤3中的浓缩物和萃取剂的质量比为1:12;步骤1中艾叶和鼠尾草的质量比为1.5:1。Among them, the aqueous phase in the extractant is composed of water; the oil phase is composed of ethyl acetate and cyclohexane in a mass ratio of 1:6.5; the mass ratio of the aqueous phase to the oil phase is 1:3; the mass ratio of the concentrate to the extractant in step 3 is 1:12; the mass ratio of mugwort and sage in step 1 is 1.5:1.
提取物10:Extract 10:
具体制备方案如下:步骤1:按照质量份称取植物原料:3份艾叶,2份鼠尾草,1.2份薰衣草和0.8份橙花;将植物原料混合,加入植物原料总质量2.3倍的水,破碎,得到破碎液;The specific preparation scheme is as follows: Step 1: Weigh plant raw materials according to mass: 3 parts of mugwort, 2 parts of sage, 1.2 parts of lavender and 0.8 parts of orange blossom; mix the plant raw materials, add 2.3 times the total mass of water of the plant raw materials, and crush them to obtain a crushed liquid;
步骤2:在破碎液中加入相较于破碎液质量8倍的质量浓度为52%的乙醇水溶液,在温度为45℃、转速为80转/分搅拌30小时,得到浸提液;Step 2: adding 52% ethanol aqueous solution with a mass concentration of 8 times the mass of the crushing liquid to the crushing liquid, stirring at a temperature of 45° C. and a rotation speed of 80 rpm for 30 hours to obtain an extract;
步骤3:将浸提液在温度为62.5℃进行减压浓缩至浸提液质量的15%,得到浓缩物;浓缩物中加入由油相、水相组成的萃取剂,38℃萃取6.5小时,将水相倒出,得到萃取物;Step 3: The extract is concentrated under reduced pressure at a temperature of 62.5° C. to 15% of the mass of the extract to obtain a concentrate; an extractant consisting of an oil phase and an aqueous phase is added to the concentrate, and extraction is performed at 38° C. for 6.5 hours, and the aqueous phase is poured out to obtain an extract;
步骤4:将萃取物采用孔径为1微米的滤膜过滤,滤液在42℃减压蒸馏进行浓缩,至滤液质量的15%;然后在温度为50℃、压力为0.012MPa下真空干燥6.2小时,得到提取物;Step 4: Filter the extract through a filter membrane with a pore size of 1 micron, and concentrate the filtrate by vacuum distillation at 42°C to 15% of the filtrate mass; then vacuum dry at a temperature of 50°C and a pressure of 0.012MPa for 6.2 hours to obtain an extract;
其中,萃取剂中水相由水组成;油相由乙酸乙酯和环己烷按照质量为1:8组成;水相和油相的质量比为1:3;步骤3中的浓缩物和萃取剂的质量比为1:12;步骤1中艾叶和鼠尾草的质量比为1.5:1。Among them, the aqueous phase in the extractant is composed of water; the oil phase is composed of ethyl acetate and cyclohexane in a mass ratio of 1:8; the mass ratio of the aqueous phase to the oil phase is 1:3; the mass ratio of the concentrate to the extractant in step 3 is 1:12; the mass ratio of mugwort and sage in step 1 is 1.5:1.
提取物11:Extract 11:
具体制备方案如下:步骤1:按照质量份称取植物原料:3份艾叶,2份鼠尾草,1.2份薰衣草和0.8份橙花;将植物原料混合,加入植物原料总质量2.3倍的水,破碎,得到破碎液;The specific preparation scheme is as follows: Step 1: Weigh plant raw materials according to mass: 3 parts of mugwort, 2 parts of sage, 1.2 parts of lavender and 0.8 parts of orange blossom; mix the plant raw materials, add 2.3 times the total mass of water of the plant raw materials, and crush them to obtain a crushed liquid;
步骤2:在破碎液中加入相较于破碎液质量8倍的质量浓度为52%的乙醇水溶液,在温度为45℃、转速为80转/分搅拌30小时,得到浸提液;Step 2: adding 52% ethanol aqueous solution with a mass concentration of 8 times the mass of the crushing liquid to the crushing liquid, stirring at a temperature of 45° C. and a rotation speed of 80 rpm for 30 hours to obtain an extract;
步骤3:将浸提液在温度为62.5℃进行减压浓缩至浸提液质量的15%,得到浓缩物;浓缩物中加入由油相、水相组成的萃取剂,38℃萃取6.5小时,将水相倒出,得到萃取物;Step 3: The extract is concentrated under reduced pressure at a temperature of 62.5° C. to 15% of the mass of the extract to obtain a concentrate; an extractant consisting of an oil phase and an aqueous phase is added to the concentrate, and extraction is performed at 38° C. for 6.5 hours, and the aqueous phase is poured out to obtain an extract;
步骤4:将萃取物采用孔径为1微米的滤膜过滤,滤液在42℃减压蒸馏进行浓缩,至滤液质量的15%;然后在温度为50℃、压力为0.012MPa下真空干燥6.2小时,得到提取物;Step 4: Filter the extract through a filter membrane with a pore size of 1 micron, and concentrate the filtrate by vacuum distillation at 42°C to 15% of the filtrate mass; then vacuum dry at a temperature of 50°C and a pressure of 0.012MPa for 6.2 hours to obtain an extract;
其中,萃取剂中水相由水组成;油相由石油醚组成;水相和油相的质量比为1:3;步骤3中的浓缩物和萃取剂的质量比为1:12;步骤1中艾叶和鼠尾草的质量比为1.5:1。Among them, the aqueous phase in the extractant is composed of water; the oil phase is composed of petroleum ether; the mass ratio of the aqueous phase to the oil phase is 1:3; the mass ratio of the concentrate to the extractant in step 3 is 1:12; and the mass ratio of mugwort and sage in step 1 is 1.5:1.
二、测试2. Testing
1、DPPH自由基清除效果测试1. DPPH free radical scavenging effect test
将4mgDPPH用无水乙醇定容至50mL,得到DPPH溶液;将0.5mg提取物1-11用无水乙醇定容至50mL,得到待测样品(根据提取物1-11的顺序,命名得到的待测样品依次为样品A1-11)。将DPPH溶液、待测样品密封并置于37℃避光环境静置1小时。在517nm下测定各测试溶液的吸光度K值,并计算待测样品的DPPH自由基清除率,计算公式为[1-(K1-K2)/K3]×100%,其中,K1为2mL待测样品和2mLDPPH溶液的混合物517nm的吸光度;K2为2mL待测样品和2mL无水乙醇的混合物517nm的吸光度;K3为2ml无水乙醇与2mLDPPH溶液的混合物517nm的吸光度。具体测试结果见表1内容。4 mg DPPH was diluted to 50 mL with anhydrous ethanol to obtain a DPPH solution; 0.5 mg extracts 1-11 were diluted to 50 mL with anhydrous ethanol to obtain the samples to be tested (according to the order of extracts 1-11, the samples to be tested were named sample A1-11 in sequence). The DPPH solution and the samples to be tested were sealed and placed in a light-proof environment at 37°C for 1 hour. The absorbance K value of each test solution was measured at 517 nm, and the DPPH free radical scavenging rate of the sample to be tested was calculated using the formula [1-(K1-K2)/K3]×100%, where K1 is the absorbance at 517 nm of a mixture of 2 mL of the sample to be tested and 2 mL of DPPH solution; K2 is the absorbance at 517 nm of a mixture of 2 mL of the sample to be tested and 2 mL of anhydrous ethanol; and K3 is the absorbance at 517 nm of a mixture of 2 ml of anhydrous ethanol and 2 mL of DPPH solution. The specific test results are shown in Table 1.
表1 DPPH自由基清除效果测试Table 1 DPPH free radical scavenging effect test
根据表1测试结果可以得到,本发明采用艾叶、鼠尾草、薰衣草和橙花加水破碎,然后使用乙醇水溶液进行浸提,并采取由乙酸乙酯和环己烷组成的油相与水相搭配得到的萃取剂进行萃取,然后进行后处理,所得到植物提取物,具有优异的DPPH自由基清除效果,且DPPH自由基清除效率达到87.52%。According to the test results in Table 1, the present invention uses wormwood, sage, lavender and orange blossom to crush with water, then uses ethanol aqueous solution for extraction, and uses an extractant obtained by combining an oil phase composed of ethyl acetate and cyclohexane with an aqueous phase for extraction, and then performs post-treatment. The obtained plant extract has excellent DPPH free radical scavenging effect, and the DPPH free radical scavenging efficiency reaches 87.52%.
根据样品A1、3-4的测试结果可以得到,本发明采用艾叶、鼠尾草两者的搭配能进一步提高清除DPPH自由基效果,两者在促进清除DPPH自由基效果上具有相互促进的复配关系。当艾叶和鼠尾草的用量比例达到1-2:1时,制备体系所得到的提取物的清除DPPH自由基效果更优。According to the test results of samples A1 and 3-4, the combination of wormwood and sage in the present invention can further improve the effect of scavenging DPPH free radicals, and the two have a mutually promoting compound relationship in promoting the effect of scavenging DPPH free radicals. When the usage ratio of wormwood and sage reaches 1-2:1, the extract obtained by the preparation system has a better effect of scavenging DPPH free radicals.
本发明采用由乙酸乙酯和环己烷组成的油相与水相搭配得到的萃取剂进行萃取,得到的提取物清除DPPH自由基的效果优异;通过样品A1、A2和A11的测试结果可以得到,本发明油相选择乙酸乙酯和环己烷进行萃取所赋予清除自由基的效果更优。且通过A1、A7-10的测试结果可以得到,本发明制备体系中的乙酸乙酯和环己烷比例在1:3-5范围内时,所得到的提取物清除DPPH自由基效果更好。The present invention uses an extractant obtained by combining an oil phase composed of ethyl acetate and cyclohexane with an aqueous phase for extraction, and the obtained extract has an excellent effect of removing DPPH free radicals; through the test results of samples A1, A2 and A11, it can be obtained that the oil phase of the present invention selects ethyl acetate and cyclohexane for extraction to give a better effect of removing free radicals. And through the test results of A1 and A7-10, it can be obtained that when the ratio of ethyl acetate to cyclohexane in the preparation system of the present invention is within the range of 1:3-5, the obtained extract has a better effect of removing DPPH free radicals.
2、羟自由基清除效果测试2. Hydroxyl free radical scavenging effect test
将0.5mg提取物1-11用无水乙醇定容至50mL,得到待测样品(根据提取物1-11的顺序,命名得到的待测样品依次为样品B1-11)。0.5 mg of extracts 1-11 were diluted to 50 mL with anhydrous ethanol to obtain the samples to be tested (according to the order of extracts 1-11, the samples to be tested were named sample B1-11).
取0.5mL浓度为0.75mmol/L邻二氮菲的乙醇溶液于容器中,加入2mL浓度为0.2mol/L且pH值为7.4磷酸盐缓冲液和1mL待测样品,混匀,加入0.5mL浓度为0.75mmol/L的FeSO4水溶液,混匀,加入0.5mL质量浓度为0.01%的H2O2溶液,混匀得到测试组溶液。Take 0.5mL of 0.75mmol/L phenanthroline ethanol solution in a container, add 2mL of 0.2mol/L phosphate buffer with a pH value of 7.4 and 1mL of the sample to be tested, mix well, add 0.5mL of 0.75mmol/L FeSO 4 aqueous solution, mix well, add 0.5mL of 0.01% H 2 O 2 solution, mix well to obtain the test group solution.
重复上述测试溶液的制备步骤,使用等量去离子水替换待测样品进行制备,得到空白组溶液。Repeat the above test solution preparation steps, use an equal amount of deionized water to replace the sample to be tested to prepare a blank group solution.
重复上述测试溶液的制备步骤,使用等量去离子水替换H2O2溶液进行制备,得到替换组溶液。Repeat the above test solution preparation steps, using an equal amount of deionized water to replace the H 2 O 2 solution to prepare a replacement group solution.
将上述制备的测试组溶液、空白组溶液、替换组溶液分别在37℃恒温水浴1小时后,在536nm下测量测试溶液吸光度值,依次记为A1、A2和A3值。计算待测样品的羟自由基清除率,计算公式为[(A1-A3)/(A2-A3)]×100%。具体结果见表2内容。After the test group solution, blank group solution and replacement group solution prepared above were placed in a constant temperature water bath at 37°C for 1 hour, the absorbance values of the test solutions were measured at 536nm, which were recorded as A1, A2 and A3 values respectively. The hydroxyl radical scavenging rate of the sample to be tested was calculated using the formula [(A1-A3)/(A2-A3)]×100%. The specific results are shown in Table 2.
表2羟自由基清除效果测试Table 2 Hydroxyl radical scavenging effect test
根据表2测试结果可以得到,本发明采用艾叶、鼠尾草、薰衣草和橙花加水破碎,然后使用乙醇水溶液进行浸提,并采取由乙酸乙酯和环己烷组成的油相与水相搭配得到的萃取剂进行萃取,然后进行后处理,所得到植物提取物,具有优异的羟自由基清除效果,且羟自由基清除效率达到82.34%。According to the test results in Table 2, the present invention uses wormwood, sage, lavender and orange blossom to crush with water, then uses ethanol aqueous solution for extraction, and uses an extractant obtained by combining an oil phase composed of ethyl acetate and cyclohexane with an aqueous phase for extraction, and then performs post-treatment. The obtained plant extract has excellent hydroxyl radical scavenging effect, and the hydroxyl radical scavenging efficiency reaches 82.34%.
3、保湿效果测试3. Moisturizing effect test
将上述提取物(提取物1、2、7-11)与乙二醇、水按照质量比为1:4:20混合,得到待测样品(根据提取物1、2、7-11的顺序,命名得到的待测样品依次为样品C1、2、7-11),进行保湿效果测试。The above extracts (extracts 1, 2, 7-11) were mixed with ethylene glycol and water in a mass ratio of 1:4:20 to obtain test samples (according to the order of extracts 1, 2, 7-11, the test samples were named as samples C1, 2, 7-11, respectively), and the moisturizing effect was tested.
测试方法如下:选择年龄为30-55岁的志愿者,随机分为6组,每组男性和女性志愿者各3名。选择志愿者左臂手掌上方同一位置的皮肤作为测试区域,面积为3×3厘米。在涂抹待测样品前,将测试区域皮肤使用清水清洗干净并使用织布擦干,再使用CorneometerCM 825测试仪器对测试区域皮肤在涂抹待测样品前的皮肤含水量进行测试并收集数据。然后各组志愿者在测试区域滴加待测样品并涂抹均匀,每个志愿者的每个测试区域使用的待测样品的量为0.2g。然后在涂抹均匀后的第2小时、6小时和12小时使用上述相同测试方法测试志愿者测试区域内皮肤含水量。然后计算使用待测样品的不同时间相较于使用待测溶液前的皮肤含水量的增加比率σ值。其中,使用待测样品2小时的皮肤含水量增加比率σ2值=(使用待测样品2小时的皮肤含水量-使用待测样品前的皮肤含水量)/使用待测样品前的皮肤含水量×100%,使用待测样品6小时的皮肤含水量增加比率σ6值=(使用待测样品6小时的皮肤含水量-使用待测样品前的皮肤含水量)/使用待测样品前的皮肤含水量×100%,使用待测样品10小时的皮肤含水量增加比率σ10值=(使用待测样品10小时的皮肤含水量-使用待测样品前的皮肤含水量)/使用待测样品的皮肤含水量×100%。具体结果见表3内容。The test method is as follows: Volunteers aged 30-55 were selected and randomly divided into 6 groups, with 3 male and 3 female volunteers in each group. The skin at the same position above the palm of the left arm of the volunteer was selected as the test area, with an area of 3×3 cm. Before applying the sample to be tested, the skin in the test area was cleaned with clean water and wiped dry with a woven cloth, and then the skin moisture content of the skin in the test area before applying the sample to be tested was tested using a CorneometerCM 825 test instrument and data was collected. Then each group of volunteers dripped the sample to be tested on the test area and applied it evenly, and the amount of the sample to be tested used in each test area of each volunteer was 0.2g. Then, the skin moisture content in the test area of the volunteer was tested using the same test method at 2 hours, 6 hours and 12 hours after the uniform application. Then, the increase ratio σ value of the skin moisture content at different times of using the sample to be tested compared to before using the test solution was calculated. Among them, the skin moisture content increase ratio σ2 value after using the sample to be tested for 2 hours = (skin moisture content after using the sample to be tested for 2 hours - skin moisture content before using the sample to be tested) / skin moisture content before using the sample to be tested × 100%, the skin moisture content increase ratio σ6 value after using the sample to be tested for 6 hours = (skin moisture content after using the sample to be tested for 6 hours - skin moisture content before using the sample to be tested) / skin moisture content before using the sample to be tested × 100%, and the skin moisture content increase ratio σ10 value after using the sample to be tested for 10 hours = (skin moisture content after using the sample to be tested for 10 hours - skin moisture content before using the sample to be tested) / skin moisture content of the sample to be tested × 100%. The specific results are shown in Table 3.
表3保湿效果测试Table 3 Moisturizing effect test
根据表3测试结果可以得到,本发明采用艾叶、鼠尾草、薰衣草和橙花加水破碎,然后使用乙醇水溶液进行浸提,并采取由乙酸乙酯和环己烷组成的油相与水相搭配得到的萃取剂进行萃取,然后进行后处理,所得到植物提取物,具有优异的增加肌肤含水量的效果;在使用本发明提取物2小时,能增加肌肤含水量的比例达到45.72%;在使用本发明提取物6小时,能增加肌肤含水量的比例达到30.48%;在使用本发明提取物10小时,能增加肌肤含水量的比例达到18.54%。According to the test results in Table 3, the present invention uses wormwood, sage, lavender and orange blossom to add water and crush, then use ethanol water solution for extraction, and use an extractant obtained by combining an oil phase composed of ethyl acetate and cyclohexane with an aqueous phase for extraction, and then perform post-treatment. The obtained plant extract has an excellent effect of increasing skin moisture content; after using the extract of the present invention for 2 hours, the proportion of skin moisture content can be increased by 45.72%; after using the extract of the present invention for 6 hours, the proportion of skin moisture content can be increased by 30.48%; after using the extract of the present invention for 10 hours, the proportion of skin moisture content can be increased by 18.54%.
本发明采用由乙酸乙酯和环己烷组成的油相与水相搭配得到的萃取剂进行萃取,得到的提取物增加肌肤含水量的效果优异;通过样品A1、A2-11的测试结果可以得到,本发明油相选择乙酸乙酯和环己烷搭配相较于其他油相所得的萃取剂进行萃取所得到的提取物,增加皮肤含水量的效果更为显著。且本发明制备体系中的乙酸乙酯和环己烷比例在1:3-5范围内时,所得到的提取物保湿肌肤效果更好。The present invention uses an extractant obtained by combining an oil phase composed of ethyl acetate and cyclohexane with an aqueous phase for extraction, and the obtained extract has an excellent effect of increasing the moisture content of the skin; the test results of samples A1 and A2-11 show that the extract obtained by combining ethyl acetate and cyclohexane in the oil phase of the present invention has a more significant effect of increasing the moisture content of the skin than the extractant obtained by other oil phases. When the ratio of ethyl acetate to cyclohexane in the preparation system of the present invention is within the range of 1:3-5, the obtained extract has a better effect of moisturizing the skin.
本发明采用艾叶、鼠尾草、薰衣草和橙花加水破碎,然后使用乙醇水溶液进行浸提,并采取由乙酸乙酯和环己烷组成的油相与水相搭配得到的萃取剂进行萃取,然后进行后处理,能实现对艾叶、鼠尾草、薰衣草和橙花的油性活性成分,例如精油等组分,以及对有机物等成分进行有效提取,赋予提取物优异的抗氧化和保湿效果。The invention adopts the method of adding water to wormwood, sage, lavender and orange blossom to crush them, then using ethanol water solution for extraction, and using an extractant obtained by combining an oil phase composed of ethyl acetate and cyclohexane with a water phase for extraction, and then performing post-treatment, so as to effectively extract oily active ingredients of wormwood, sage, lavender and orange blossom, such as components such as essential oils, and components such as organic matter, and give the extract excellent antioxidant and moisturizing effects.
本领域的技术人员可以对本发明进行各种改动和变型,若这些修改和变型属于本发明权利要求及其等同技术的范围之内,则本发明也意图包含这些改动和变型在内。Those skilled in the art may make various changes and modifications to the present invention. If these changes and modifications fall within the scope of the claims of the present invention and their equivalents, the present invention is intended to include these changes and modifications.
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