CN110200870A - A kind of reparation moisture retention water containing solanum lyratum and Flos Hibisci extract - Google Patents
A kind of reparation moisture retention water containing solanum lyratum and Flos Hibisci extract Download PDFInfo
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- CN110200870A CN110200870A CN201910570117.6A CN201910570117A CN110200870A CN 110200870 A CN110200870 A CN 110200870A CN 201910570117 A CN201910570117 A CN 201910570117A CN 110200870 A CN110200870 A CN 110200870A
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- REJLGAUYTKNVJM-SGXCCWNXSA-N tomatine Chemical compound O([C@H]1[C@H](O)[C@@H](CO)O[C@H]([C@@H]1O[C@H]1[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O1)O)O[C@H]1[C@@H](CO)O[C@H]([C@@H]([C@H]1O)O)O[C@@H]1C[C@@H]2CC[C@H]3[C@@H]4C[C@H]5[C@@H]([C@]4(CC[C@@H]3[C@@]2(C)CC1)C)[C@@H]([C@@]1(NC[C@@H](C)CC1)O5)C)[C@@H]1OC[C@@H](O)[C@H](O)[C@H]1O REJLGAUYTKNVJM-SGXCCWNXSA-N 0.000 description 1
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 1
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 1
- 238000003809 water extraction Methods 0.000 description 1
- 238000004383 yellowing Methods 0.000 description 1
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- A—HUMAN NECESSITIES
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
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- A61K8/34—Alcohols
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Abstract
本发明公开了一种含白毛藤和木槿花提取物的修复保湿水及其制备方法,所述修复保湿水含有白毛藤提取物、木槿花提取物、丙二醇、甘油、β‑葡聚糖、尿囊素、水溶性霍霍巴油、乙二胺四乙酸二钠、柠檬酸、苯氧乙醇、去离子水。功效成分由白毛藤、木槿花提取所得。本发明提供的含白毛藤与木槿花提取物的修复保湿水,具有有一定的保湿、修复皮肤屏障、抗氧化、抗菌等功效;同时本发明生产工艺简单,涂抹后无厚重油腻感、容易吸收,保湿锁水效果良好,使肌肤长效水润。采用的白毛藤提取物、木槿花提取物生物活性良好,温和无刺激。The invention discloses a repairing and moisturizing water containing extracts of vine and hibiscus flowers and a preparation method thereof. The repairing and moisturizing water contains extracts of vines and hibiscus flowers, propylene glycol, glycerin, β-glucan, Allantoin, Jojoba Oil, Disodium EDTA, Citric Acid, Phenoxyethanol, Deionized Water. The functional ingredients are extracted from white hair vine and hibiscus flower. The repairing and moisturizing water containing the extracts of vine and hibiscus provided by the invention has certain effects of moisturizing, repairing the skin barrier, anti-oxidation, and antibacterial; meanwhile, the production process of the invention is simple, and there is no greasy feeling after application, and it is easy to Good absorption, moisturizing and water-locking effect, making the skin moisturized for a long time. The white hair vine extract and hibiscus flower extract used have good biological activity, mild and non-irritating.
Description
技术领域technical field
本发明属于化妆品的技术领域,具体涉及一种含白毛藤和木槿花提取物的修复保湿水。The invention belongs to the technical field of cosmetics, and in particular relates to a repairing and moisturizing water containing extracts of vine and hibiscus flower.
背景技术Background technique
皮肤位于人体体表最外层,具有屏障、吸收、分泌、排泄、代谢、免疫、体温调节及感觉功能,其中,皮肤屏障(skin barrier)功能是基础。1983年美国加利福尼亚大学PeterM.Elias教授(皮肤砖墙结构创始人)详细描述了表皮渗透屏障的结构和功能,提出位于皮肤最外层的角质层起到重要的表皮渗透屏障作用,并形象的将其描述为“砖墙结构”,即角质层中的角质细胞构成“砖墙结构”中的砖块;细胞间脂质则构成“砖墙结构”中的灰浆,角质层中的这种由角质细胞夹杂在细胞间脂质所构成的复层板层膜结构维持着我们正常的表皮渗透屏障功能。对外可以抵御抗原物质、微生物、日光等的侵袭,对内可防止体内营养物质、水分的丢失。表皮渗透屏障受损,经表皮水分流失(transepidermal waterloss,TEWL)增加,皮肤则出现干燥、脱屑、老化、色素沉着,异位性皮炎、湿疹、银屑病、鱼鳞病、日光性皮炎等皮肤敏感、刺激性皮炎、激素依赖性皮炎等皮肤油腻,皮脂溢出性疾病,如座疮、酒糟鼻、脂溢性皮炎。同时,对外界抗原及微生物的抵御能力下降,可导致多种皮肤病的发生。表皮渗透屏障与免疫屏障、酸性屏障及微生态共同构成一个整体防御系统。表皮微生态、pH值可影响表皮渗透屏障,表皮渗透屏障受损,又可影响其他屏障功能。The skin is located in the outermost layer of the human body surface and has barrier, absorption, secretion, excretion, metabolism, immunity, temperature regulation and sensory functions, among which the skin barrier function is the basis. In 1983, Professor Peter M.Elias of the University of California (the founder of the skin brick wall structure) described the structure and function of the epidermal permeability barrier in detail, and proposed that the stratum corneum located in the outermost layer of the skin plays an important role in the epidermal permeability barrier, and vividly It is described as a "brick wall structure", that is, the corneocytes in the stratum corneum make up the bricks in the "brick wall structure"; the intercellular lipids make up the mortar in the "brick wall structure" The multilayer lamellar membrane structure composed of cells intercalated with intercellular lipids maintains our normal epidermal permeability barrier function. Externally, it can resist the invasion of antigenic substances, microorganisms, sunlight, etc. internally, it can prevent the loss of nutrients and water in the body. The epidermal permeability barrier is damaged, transepidermal water loss (TEWL) increases, and the skin appears dry, desquamated, aging, pigmentation, atopic dermatitis, eczema, psoriasis, ichthyosis, solar dermatitis, etc. Sensitive, irritant dermatitis, hormone-dependent dermatitis and other oily skin, seborrhea diseases such as acne, rosacea, seborrheic dermatitis. At the same time, the ability to resist external antigens and microorganisms decreases, which can lead to the occurrence of various skin diseases. Epidermal permeability barrier, immune barrier, acid barrier and microecology together constitute an overall defense system. The epidermal microecology and pH value can affect the epidermal permeability barrier, and the damage of the epidermal permeability barrier can also affect other barrier functions.
随着生活水平的提高,人们也越来越注重皮肤的保养,然而紫外辐射等环境影响以及人体体内代谢缓慢、失调等原因导致各种皮肤问题。据皮肤科医生指出,婴儿内的水分占体重的80%以上,而体内的水分会随年纪而递减,由于婴儿有足够的水分,因此皮肤会显得细致光泽。事实上,成年人有足够的皮脂分泌,但成年女性的皮肤含水量只有65%或更低(其中角质仅15%),远远低于婴儿时期,因此,缺水是一切皮肤问题的根源。With the improvement of living standards, people pay more and more attention to skin care. However, environmental influences such as ultraviolet radiation and slow metabolism in the human body, imbalance and other reasons lead to various skin problems. According to dermatologists, the water in the baby accounts for more than 80% of the body weight, and the water in the body will decrease with age. Because the baby has enough water, the skin will appear delicate and shiny. In fact, adults have enough sebum secretion, but the water content of adult women's skin is only 65% or less (of which keratin is only 15%), which is far lower than that of babies. Therefore, lack of water is the root of all skin problems.
水分蒸发无非是三个原因:高温、干燥和大风,肌肤的水分也不例外。因此,一年四季的气候特征都或多或少地包含了这些因素,所以一年四季都需要补水保湿。以上三个原因只是环境因素,肌肤流失水分还包括肌肤本身的问题。除此之外,城市生活压力大,疲劳、加班、熬夜、饮食不合理,加重了皮肤的缺水状况。肌肤会因为拥有充足水份而看上去细嫩光滑,皮肤缺水会导致干燥、发黄、暗淡无光泽,松弛、皱纹等衰老现象,并容易绷紧,还会在眼下及鼻旁出现细纹。同时现代人生活节奏快,工作劳碌,因此急需一种使用便捷、有效的肌肤保湿水以满足人们的需求。然而,无论是通过何种途径给肌肤补水,都非常容易蒸发到空气中,而油脂是最好的保湿成分,能够保住肌肤水分不流失。There are three reasons for water evaporation: high temperature, dryness and wind, and the moisture of the skin is no exception. Therefore, the climate characteristics of the four seasons more or less include these factors, so it is necessary to replenish water and moisturize all the year round. The above three reasons are only environmental factors. The loss of moisture from the skin also includes the problems of the skin itself. In addition, urban life is stressful, fatigue, overtime, staying up late, and unreasonable diet, which aggravates the water shortage of the skin. The skin will look delicate and smooth because of sufficient moisture. The lack of moisture in the skin will lead to dryness, yellowing, dullness, sagging, wrinkles and other aging phenomena, and it is easy to tighten, and fine lines will appear under the eyes and around the nose. Simultaneously modern people's rhythm of life is fast, work is busy, therefore be badly in need of a kind of easy to use, effective skin moisturizing water to satisfy people's demand. However, no matter what method is used to hydrate the skin, it is very easy to evaporate into the air, and oil is the best moisturizing ingredient, which can keep the skin moisture from losing.
在护肤品领域,补水保湿是一直以来不变的话题,如何做好补水保湿,是保护皮肤的首要问题。目前市场上保湿水的种类繁多,但是补水保湿效果不尽如人意,大多酒精含量较高,且刺激性较大,不适宜长期使用。植物油脂在这方面不同于动物油脂,多数植物油脂在常温处于液态,且大多数植物油内部含有的不饱和脂肪酸和微量元素、维生素E等物质,天然具有抗氧化特性。同时,植物天然产物温和、不刺激、满足多数群体需要,大量的临床研究也展示天然产物活性成分的多样性、耐受性及对皮肤的安全性比化学合成品更具优越性。因此,从全球化妆品近几年发展趋势看,天然化妆品热度呈现上升趋势,这给天然化妆品带来了机遇。In the field of skin care products, moisturizing has always been a constant topic. How to do a good job of moisturizing is the most important issue in protecting the skin. At present, there are many types of moisturizing water on the market, but the moisturizing effect is not satisfactory. Most of them have high alcohol content and are irritating, so they are not suitable for long-term use. Vegetable oils are different from animal oils in this aspect. Most vegetable oils are liquid at room temperature, and most vegetable oils contain unsaturated fatty acids, trace elements, vitamin E and other substances, which naturally have antioxidant properties. At the same time, plant natural products are mild, non-irritating, and meet the needs of most groups. A large number of clinical studies have also shown that the diversity, tolerance and safety of natural product active ingredients are superior to chemical synthetic products. Therefore, judging from the development trend of global cosmetics in recent years, the popularity of natural cosmetics is on the rise, which brings opportunities for natural cosmetics.
白毛藤Solanum lyratum Thunb是多年生蔓性草本,属于茄科茄属植物,药用历史悠久。从白毛藤中分离出的化合物有皂甙类、有机酸类、萜类、多酚类、黄酮类、甾醇类、香豆素类、多糖类和其他类型的化合物。其中所含的甾体生物碱和皂苷均有抗菌活性,其中番茄碱的作用更强,具有消炎、抗过敏、止痒和免疫抑制作用。2001年,Wei-Wen Kuo等在研究白英的粗提物保护表皮细胞的抗氧化性,结果表明白英粗提物能够清除DPPH,还可以推迟剂量依赖性低密度脂蛋白的氧化,同事还减弱了氧化低密度脂蛋白诱导产生活性氧水平,减少了内皮氧化蛋白酶的表达。Solanum lyratum Thunb is a perennial herb belonging to the family Solanaceae and has a long history of medicinal use. Compounds isolated from vine include saponins, organic acids, terpenoids, polyphenols, flavonoids, sterols, coumarins, polysaccharides and other types of compounds. The steroidal alkaloids and saponins contained therein have antibacterial activity, among which tomatine has a stronger effect, and has anti-inflammatory, anti-allergic, antipruritic and immunosuppressive effects. In 2001, Wei-Wen Kuo et al. studied the antioxidant properties of the crude extract of Baiying to protect epidermal cells. The results showed that the crude extract of Baiying could clear DPPH and delay the oxidation of low-density lipoprotein in a dose-dependent manner. Colleagues also Attenuated the level of reactive oxygen species induced by oxidized LDL and decreased the expression of endothelial oxidative protease.
木槿Hibiscussyriacus,属锦葵木槿属,落叶灌木或小乔木。是一种庭园常见的灌木花种,广泛分布于我国热带亚热带地区。木槿花含植物油脂、必需氨基酸、多糖、多元醇粘液质,具有保湿和抗氧化、清除自由基的功能。木槿花原种的总酚和总黄酮含量最高,抗氧化性最强。金月亭等的论文《木槿花生物活性的初步研究》表明,1g木槿花相当于5.19mg维生素C,有清除DPPH的能力;而其抗氧化能力相当于9.12mg维生素C。木槿花提取液对细菌和霉菌均有一定的抑制作用,且对细菌的抑制作用明显大于霉菌的。其根皮具有环状缩氨酸、原花青素,因此同样具有杀菌消毒作用。民间有用此花汁洗脸美容的习俗。在木槿花汁中添加适量甘油和乳化剂,维生素E等,配成水包油型(O/W)护肤液,适于中性皮肤使用,尤其对中老年手上有老年斑者有一定的祛斑作用,同时又起到润滑保湿的功效,弥补了普通护肤液生物活性物成分及微量元素的不足的缺陷。木槿花中含有的原花青素可以清除细胞膜中水溶性和脂溶性的自由基,因此,抑制了释放某些酶去伤害毛细血管壁的过程。原花青素连接在胶原蛋白上,可以阻止那些破坏胶原蛋白的酶的危害。原花青素不仅帮助胶原蛋白纤维形成交联结构,而且可以帮助恢复因受伤和自由基所引起的过度交联的损害。过度交联会使结缔组织窒息和硬化,从而使皮肤起皱纹和过早老化。花青素还保护人体免受阳光伤害,促进治愈牛皮癣和寿斑。原花青素也是局部施用的皮肤霜的极好添加剂。能使皮肤年轻化、健康化、细胞富有活力,能恢复其伸展性和弹性,修复皮肤。Hibiscus syriacus is a deciduous shrub or small tree belonging to the genus Malvacea hibiscus. It is a common shrub flower species in gardens, widely distributed in tropical and subtropical regions of my country. Hibiscus flower contains vegetable oil, essential amino acid, polysaccharide, and polyol mucilage, which has the functions of moisturizing, anti-oxidation and scavenging free radicals. The original species of hibiscus had the highest content of total phenols and total flavonoids, and the strongest antioxidant activity. The paper "Preliminary Study on Biological Activity of Hibiscus Flower" by Jin Yueting et al. showed that 1g of Hibiscus Flower is equivalent to 5.19mg of vitamin C and has the ability to remove DPPH; while its antioxidant capacity is equivalent to 9.12mg of vitamin C. The hibiscus flower extract has a certain inhibitory effect on both bacteria and mold, and the inhibitory effect on bacteria is obviously greater than that on mold. Its root bark has cyclic peptides and proanthocyanidins, so it also has bactericidal and disinfecting effects. Folks use this flower juice to wash their faces and improve their beauty. Add appropriate amount of glycerin, emulsifier, vitamin E, etc. to hibiscus flower juice to make an oil-in-water (O/W) skin care lotion, which is suitable for neutral skin, especially for middle-aged and elderly people with age spots on their hands. At the same time, it has the effect of lubricating and moisturizing, which makes up for the shortcomings of the lack of biological active ingredients and trace elements in ordinary skin care lotions. The proanthocyanidins contained in hibiscus can scavenge water-soluble and fat-soluble free radicals in cell membranes, thus inhibiting the process of releasing certain enzymes to damage capillary walls. Proanthocyanidins are attached to collagen, which can prevent the damage of enzymes that destroy collagen. Proanthocyanidins not only help collagen fibers form a cross-linked structure, but also help restore damage caused by excessive cross-linking caused by injuries and free radicals. Excessive cross-linking suffocates and hardens connective tissue, which wrinkles and prematurely ages the skin. Anthocyanins also protect the body from sun damage and promote the healing of psoriasis and age spots. Proanthocyanidins are also excellent additions to topically applied skin creams. It can make the skin rejuvenated and healthy, the cells are full of vitality, restore its stretch and elasticity, and repair the skin.
针对肌肤敏感缺水的现象,出现了很多抗敏修复护肤品,主要有抗过敏护肤品,主要通过减少香料、色素、酒精和防腐剂等刺激成分,或者添加芦荟提取液,洋甘菊萃取液等原料达到抗过敏的效果;另外,有添加激素,可以在皮肤发生敏感现象后,对肌肤起到一定的修复作用。由上述可知,现有护肤品的效果单一,针对于敏感肌肤不能达到抗敏和修护的双重功效,且修复周期长;甚至对含激素类产品产生依赖。Aiming at the phenomenon of skin sensitivity and dehydration, many anti-allergic and repairing skin care products have appeared, mainly including anti-allergic skin care products, mainly by reducing stimulating ingredients such as spices, pigments, alcohol and preservatives, or adding raw materials such as aloe vera extract and chamomile extract Achieve anti-allergic effect; in addition, there are added hormones, which can repair the skin to a certain extent after skin sensitivity occurs. It can be seen from the above that the existing skin care products have single effects, and cannot achieve the dual effects of anti-allergic and repairing for sensitive skin, and the repair cycle is long; they even rely on hormone-containing products.
中国专利申请CN 106236696 B(申请号201610744048.2)公开了一种含有叶绿素的舒敏保湿水及其制备方法。但存在叶绿素不稳定且提取工艺繁琐等问题,功效有待考察。中国专利申请CN102000011A(申请号CN201010561334)公开了一种木槿花护肤液及其制备方法。但其提取工艺存在提取液含杂质多、提取效率低。经检索,尚未发现有白毛藤提取物和木槿花提取物的复配物在保湿化妆品中的应用。Chinese patent application CN 106236696 B (application number 201610744048.2) discloses a soothing moisturizing water containing chlorophyll and a preparation method thereof. However, there are problems such as unstable chlorophyll and cumbersome extraction process, and the efficacy needs to be investigated. Chinese patent application CN102000011A (application number CN201010561334) discloses a hibiscus flower skin care lotion and a preparation method thereof. However, in the extraction process, the extract contains many impurities and the extraction efficiency is low. After searching, it has not been found that there is any application of the compound of the extract of the white hair vine and the extract of the hibiscus flower in moisturizing cosmetics.
由于天然产物的粗提液中混有多种有机化合物,且生物活性含量低、不稳定、分离纯化难度大,对于含有皂苷类的植物,普通的水提法,容易使其分解,且减压过滤会出现大量泡沫,难以浓缩,因此需要更高效的纯化方法,以获得纯净的提取物。Since the crude extract of natural products contains a variety of organic compounds, and the biological activity content is low, unstable, and difficult to separate and purify, for plants containing saponins, it is easy to decompose them by ordinary water extraction, and decompression Filtration produces a lot of foam and is difficult to concentrate, so more efficient purification methods are required to obtain pure extracts.
发明内容Contents of the invention
为了解决上述问题,本发明提供一种含有白毛藤、木槿花提取物的修复保湿水,其温和亲肤,易吸收,安全无刺激,保湿、舒敏效果好,且体系稳定。In order to solve the above-mentioned problems, the present invention provides a repairing moisturizing water containing extracts of vine and hibiscus, which is mild and skin-friendly, easy to absorb, safe and non-irritating, has good moisturizing and soothing effects, and has a stable system.
本发明的目的是通过以下技术方案实现的:The purpose of the present invention is achieved through the following technical solutions:
一种含白毛藤和木槿花提取物的修复保湿水,由下述重量份的组分制成:A kind of repairing moisturizing water containing the extracts of Alba vine and hibiscus flower, which is made of the following components by weight:
进一步的,所述白毛藤提取物的制备方法如下:Further, the preparation method of the vine extract is as follows:
(1)称取一定量的白毛藤洗净晾干,将其磨成粉末,过60目筛得白毛藤粉末,称取20~50重量份;(1) Take a certain amount of white hair rattan, wash and dry it, grind it into powder, and get the white hair rattan powder through a 60-mesh sieve, and take 20 to 50 parts by weight;
(2)将白毛藤粉末分散于去离子水中,搅拌充分混合得白毛藤悬浮液;白毛藤粉末与去离子水的质量比为1:10~20;(2) Disperse the white hair rattan powder in deionized water, stir and mix thoroughly to obtain the white hair rattan suspension; the mass ratio of the white hair rattan powder to the deionized water is 1:10~20;
(3)加热白毛藤悬浮液至40~55℃,接着加入1.0-1.5重量份纤维素酶,搅拌,充分反应2-3h;(3) Heating the suspension of rattan to 40-55° C., then adding 1.0-1.5 parts by weight of cellulase, stirring, and fully reacting for 2-3 hours;
(4)在步骤(3)的混合溶液中加入0.6-1.2重量份的果胶酶,搅拌,充分反应1-2h;(4) Add 0.6-1.2 parts by weight of pectinase to the mixed solution in step (3), stir, and fully react for 1-2h;
(5)步骤(4)混合溶液降低温度至35~50℃,用pH调节剂调节pH至4~5,过滤,除去滤渣;(5) The temperature of the mixed solution in step (4) is lowered to 35-50° C., adjusted to 4-5 with a pH regulator, and filtered to remove the filter residue;
(6)将滤液浓缩至120-150重量份,即得白毛藤提取物。(6) Concentrate the filtrate to 120-150 parts by weight to obtain the extract of Rattan alba.
进一步的,所述木槿花提取物的制备方法如下:Further, the preparation method of the hibiscus flower extract is as follows:
A1、将刚采摘的新鲜木槿花洗净沥干,将其花瓣分离,再将其低温冻干;A1. Wash and drain the freshly picked hibiscus flowers, separate the petals, and freeze-dry them at low temperature;
A2、称取20~40重量份干燥后的木槿花,将其搅碎成粉,过40目筛,得到木槿花粉末;A2. Weigh 20-40 parts by weight of the dried hibiscus flower, grind it into powder, and pass through a 40-mesh sieve to obtain the hibiscus flower powder;
A3、加入木槿花粉末3倍重量的去离子水浸泡,加pH调节剂调pH至4,加0.5~1重量份纤维素酶,充分搅拌,置40~50℃恒温水浴中1.5h,加木槿花粉末5倍重量的质量浓度为75%的乙醇溶液回流提取1~2h,趁热过滤,得第一次提取液和药渣;A3. Add 3 times the weight of hibiscus flower powder to soak in deionized water, add pH regulator to adjust pH to 4, add 0.5-1 weight part of cellulase, stir well, put in 40-50°C constant temperature water bath for 1.5h, add hibiscus The flower powder is 5 times the weight of the ethanol solution with a mass concentration of 75% and is refluxed for 1 to 2 hours, and filtered while it is hot to obtain the first extract and medicinal residues;
A4、往药渣中加药渣5倍重量的质量浓度为50%的乙醇溶液回流提取0.5~1h,趁热过滤,得第二次提取液;A4. Adding 5 times the weight of the medicinal residues to the medicinal residues with an ethanol solution with a mass concentration of 50% for reflux extraction for 0.5 to 1 hour, and filtering while hot to obtain a second extract;
A5、将第一次提取液和第二次提取液混合,蒸发,回收乙醇,离心,取上层清液用,正丁醇萃取3次,挥发正丁醇,得到木槿花提取物。A5. Mix the first extract and the second extract, evaporate, recover ethanol, centrifuge, take the supernatant, extract with n-butanol for 3 times, and volatilize n-butanol to obtain hibiscus flower extract.
进一步的,所述pH调节剂为2.5mol/L的盐酸溶液。Further, the pH regulator is 2.5mol/L hydrochloric acid solution.
本发明还包括一种含白毛藤和木槿花提取物的修复保湿水的制备方法,包括以下步骤:The present invention also includes a preparation method of repairing and moisturizing water containing the extracts of vine and hibiscus flower, comprising the following steps:
S1、在去离子水中加入丙二醇、甘油、β-葡聚糖、尿囊素、水溶性霍霍巴油、柠檬酸和乙二胺四乙酸二钠,并加热至70~80℃,保温状态下,搅拌20~30min至均匀,得到物料A;S1. Add propylene glycol, glycerin, β-glucan, allantoin, water-soluble jojoba oil, citric acid and disodium edetate into deionized water, and heat to 70-80°C. Stir for 20-30 minutes until uniform, and obtain material A;
S2、将物料A降温至30~40℃,加入苯氧乙醇、白毛藤提取物和木槿花提取物,继续搅拌至均匀,得到物料B;S2. Cool down the material A to 30-40°C, add phenoxyethanol, white hair vine extract and hibiscus flower extract, continue to stir until uniform, and obtain material B;
S3、物料B冷却至-5~-10℃,保温30~60min后,过滤,最后杀菌即得修复保湿水。S3. Material B is cooled to -5~-10°C, kept warm for 30~60 minutes, filtered, and finally sterilized to obtain repairing moisturizing water.
本发明的有益效果:Beneficial effects of the present invention:
1.本发明采用天然植物,兼有营养和药理双重作用,不含激素,不含重金属等有害成分,无毒无副作用,符合化妆品长效和添加天然成分的要求。1. The present invention uses natural plants, which have both nutritional and pharmacological effects, do not contain hormones, do not contain harmful ingredients such as heavy metals, are non-toxic and have no side effects, and meet the requirements of long-acting cosmetics and adding natural ingredients.
2.白毛藤提取物具有抗氧化、抗炎、抗菌、抗敏等功效;同时木槿花含原花青素等黄酮类化合物以及多糖,具有保湿作用,能有效促进血液循环,淡化色斑,营养肌肤,增加皮肤弹性,且具有抗辐射功能。2. The extract of white hair vine has anti-oxidation, anti-inflammatory, anti-bacterial, anti-allergic effects; at the same time, hibiscus flower contains flavonoids such as proanthocyanidins and polysaccharides, which have moisturizing effect, can effectively promote blood circulation, dilute pigmentation, and nourish the skin. Increase skin elasticity, and has anti-radiation function.
3.本发明具有保湿、锁住肌肤水分,活化肌肤,抗菌,抗炎,抗敏,修复皮肤的作用,且温和不刺激皮肤。3. The present invention has the effects of moisturizing, locking skin moisture, activating skin, antibacterial, anti-inflammatory, anti-allergic, and repairing skin, and is mild and does not irritate the skin.
4.本发明成本适中,适合各种类型肌肤使用。特别是敏感肌肤以及皮肤屏障受损肌肤。4. The cost of the present invention is moderate, and it is suitable for various types of skin. Especially sensitive skin and skin with compromised skin barrier.
5.本发明方法简单、易于实施;采用酶提取法与冻干技术,低温下,能够在一定程度上,保持生物活性,防止流失,提高了产率和成效,提纯效果好,解决了生物活性成分在加工过程中易分解失活的问题。采用酶提取法,反应温和。5. The method of the present invention is simple and easy to implement; by adopting enzyme extraction method and freeze-drying technology, at low temperature, the biological activity can be maintained to a certain extent, preventing loss, improving the yield and effectiveness, good purification effect, and solving the problem of biological activity. Components are easily decomposed and inactivated during processing. Using enzyme extraction method, the reaction is mild.
具体实施方式Detailed ways
为了更好的理解本发明,下面通过实施例对本发明进进一步说明,实施例只用于解释本发明,并不会对本发明构成任何限定。In order to better understand the present invention, the present invention will be further described by the following examples, which are only used to explain the present invention and do not constitute any limitation to the present invention.
以下实施例用于说明本发明,但不用来限制本发明的范围。若未特别指明,实施例中所用的技术手段为本领域技术人员所熟知的常规手段,所用原料均为市售商品。The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention. Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art, and the raw materials used are all commercially available products.
实施例1Example 1
1)配方1) Recipe
一种含有白毛藤、木槿花提取物的修复保湿水由如下重量份数的组分组成:A repairing and moisturizing water containing extracts of vine and hibiscus consists of the following components in parts by weight:
白毛藤提取液:10份;木槿花提取液:10份;丙二醇:1份;甘油:2份;β-葡聚糖:1份;尿囊素:1份;水溶性霍霍巴油:0.3份;EDTA二钠:0.0008份;柠檬酸:0.3份;苯氧乙醇0.2份;去离子水74.1992份。Alba vine extract: 10 parts; Hibiscus flower extract: 10 parts; Propylene glycol: 1 part; Glycerin: 2 parts; β-glucan: 1 part; Allantoin: 1 part; Water-soluble jojoba oil: 0.3 EDTA disodium: 0.0008 parts; citric acid: 0.3 parts; phenoxyethanol 0.2 parts; deionized water 74.1992 parts.
2)制备2) Preparation
所述的白毛藤提取物,是按照以下方法制备得到的:The extract of the vine extract is prepared according to the following method:
(1)白毛藤洗净晾干,将其磨成粉末,过60目筛得白毛藤粉末,称取20重量份;(1) the white hair rattan is washed and dried, and it is ground into powder, and the white hair rattan powder is crossed through a 60-mesh sieve, and 20 parts by weight are weighed;
(2)将白毛藤粉末分散于去离子水中,搅拌充分混合得白毛藤悬浮液;白毛藤粉末与去离子水的质量比为1:10;(2) Disperse the white hair rattan powder in deionized water, stir and mix thoroughly to obtain the white hair rattan suspension; the mass ratio of the white hair rattan powder to the deionized water is 1:10;
(3)加热白毛藤悬浮液至40℃,接着加入1.0重量份纤维素酶,搅拌,充分反应2h;(3) Heating the suspension of rattan to 40°C, then adding 1.0 parts by weight of cellulase, stirring, and fully reacting for 2 hours;
(4)在步骤(3)的混合溶液中加入0.6重量份的果胶酶,搅拌,充分反应1h;(4) Add 0.6 parts by weight of pectinase to the mixed solution of step (3), stir, and fully react for 1 hour;
(5)步骤(4)混合溶液降低温度至35℃,用2.5mol/L的盐酸调节pH至4~5,过滤,除去滤渣;(5) The temperature of the mixed solution in step (4) is lowered to 35° C., the pH is adjusted to 4 to 5 with 2.5 mol/L hydrochloric acid, filtered, and the filter residue is removed;
(6)将滤液浓缩至120重量份,即得白毛藤提取物。(6) Concentrate the filtrate to 120 parts by weight to obtain the extract of Ceruleus albicans.
所述木槿花提取物的制备方法如下:The preparation method of the hibiscus flower extract is as follows:
(1)将刚采摘的新鲜木槿花洗净沥干,将其花瓣分离,再将其低温冻干;(1) Wash and drain the freshly picked hibiscus flowers, separate the petals, and freeze-dry them at low temperature;
(2)称取20重量份干燥后的木槿花,将其放入搅碎机搅碎成粉,过40目筛,得到木槿花粉末;(2) Take 20 parts by weight of dried hibiscus, put it into a pulverizer and grind it into powder, and cross a 40-mesh sieve to obtain hibiscus powder;
(3)加入木槿花粉末3倍重量的去离子水浸泡,加2.5mol/L盐酸调pH至4,加0.5重量份纤维素酶,充分搅拌,置40℃恒温水浴中1.5h,加木槿花粉末5倍质量浓度为75%的乙醇溶液回流提取1h,趁热过滤,得第一次提取液和药渣;(3) Add 3 times the weight of hibiscus flower powder for soaking in deionized water, add 2.5mol/L hydrochloric acid to adjust the pH to 4, add 0.5 parts by weight of cellulase, stir well, put it in a constant temperature water bath at 40°C for 1.5h, add hibiscus flower 5 times the mass concentration of the powder is 75% ethanol solution for reflux extraction for 1 hour, and filtered while hot to obtain the first extract and dregs;
(4)往药渣中加药渣5倍重量的质量浓度为50%的乙醇溶液回流提取0.5h,趁热过滤,得第二次提取液;(4) Adding 5 times the mass concentration of the medicinal residues to the medicinal residues is reflux extraction of 50% ethanol solution for 0.5h, and filtering while hot to obtain the second extract;
(5)将第一次提取液和第二次提取液混合,旋转蒸发仪蒸发,回收乙醇,离心,取上层清液用,正丁醇萃取3次,挥发正丁醇,得到木槿花提取物。(5) Mix the first extract and the second extract, evaporate with a rotary evaporator, recover ethanol, centrifuge, take the supernatant, extract with n-butanol for 3 times, volatilize n-butanol, and obtain the hibiscus flower extract .
所述的含白毛藤、木槿花提取物的修复保湿水,是按照以下方法制备得到的:The described repairing and moisturizing water containing the extracts of vine and hibiscus is prepared according to the following method:
(1)在去离子水中加入丙二醇、甘油、β-葡聚糖、尿囊素、水溶性霍霍巴油、柠檬酸和乙二胺四乙酸二钠,并加热至70℃,保温状态下,搅拌20min至均匀,得到物料A;(1) Add propylene glycol, glycerin, β-glucan, allantoin, water-soluble jojoba oil, citric acid and disodium edetate into deionized water, and heat to 70°C. 20min to uniformity, to obtain material A;
(2)将物料A降温至30℃,加入苯氧乙醇、白毛藤提取物和木槿花提取物,继续搅拌至均匀,得到物料B;(2) Cool down the material A to 30°C, add phenoxyethanol, white hair vine extract and hibiscus flower extract, continue to stir until uniform, and obtain material B;
(3)物料B冷却至-5℃,保温30min后,过滤,最后杀菌即得修复保湿水。(3) Material B was cooled to -5°C, kept warm for 30 minutes, filtered, and finally sterilized to obtain repairing moisturizing water.
实施例2Example 2
1)配方1) Recipe
一种含有白毛藤、木槿花提取物的修复保湿水由如下重量份的组分组成:A repairing and moisturizing water containing extracts of vine and hibiscus consists of the following components by weight:
白毛藤提取液:15份;木槿花提取液:20份;丙二醇:2份;甘油:2份;β-葡聚糖:1份;尿囊素:1份;水溶性霍霍巴油:0.3份;EDTA二钠:0.002份;柠檬酸:1份;苯氧乙醇0.2份;去离子水57.498份。Alba vine extract: 15 parts; hibiscus flower extract: 20 parts; propylene glycol: 2 parts; glycerin: 2 parts; β-glucan: 1 part; allantoin: 1 part; water-soluble jojoba oil: 0.3 0.002 parts of disodium EDTA; 1 part of citric acid; 0.2 parts of phenoxyethanol; 57.498 parts of deionized water.
2)制备2) Preparation
所述的白毛藤提取物,是按照以下方法制备得到的:The extract of the vine extract is prepared according to the following method:
(1)称取白毛藤洗净晾干,将其磨成粉末,过60目筛得白毛藤粉末,称取20~50重量份;(1) Take the white hair rattan, wash and dry it, grind it into powder, and pass through a 60-mesh sieve to get the white hair rattan powder, and take 20 to 50 parts by weight;
(2)将白毛藤粉末分散于去离子水中,搅拌充分混合得白毛藤悬浮液;白毛藤粉末与去离子水的质量比为1:10~1:20。;(2) Disperse the white hair rattan powder in deionized water, stir and mix thoroughly to obtain the white hair rattan suspension; the mass ratio of the white hair rattan powder to the deionized water is 1:10-1:20. ;
(3)加热白毛藤悬浮液至40~55℃,接着加入1.0-1.5重量份纤维素酶,搅拌,充分反应2-3h;(3) Heating the suspension of rattan to 40-55° C., then adding 1.0-1.5 parts by weight of cellulase, stirring, and fully reacting for 2-3 hours;
(4)在步骤(3)的混合溶液中加入1.2重量份的果胶酶,搅拌,充分反应1-2h;(4) Add 1.2 parts by weight of pectinase to the mixed solution of step (3), stir, and fully react for 1-2h;
(5)步骤(4)混合溶液降低温度至35~50℃,用2.5mol/L的盐酸调节pH至4~5,过滤,除去滤渣;(5) The temperature of the mixed solution in step (4) is lowered to 35-50° C., the pH is adjusted to 4-5 with 2.5 mol/L hydrochloric acid, filtered, and the filter residue is removed;
(6)将滤液浓缩至150重量份,即得白毛藤提取物。(6) Concentrate the filtrate to 150 parts by weight to obtain the Rhizoma alba extract.
所述木槿花提取物的制备方法如下:The preparation method of the hibiscus flower extract is as follows:
(1)将刚采摘的新鲜木槿花洗净沥干,将其花瓣分离,再将其低温冻干;(1) Wash and drain the freshly picked hibiscus flowers, separate the petals, and freeze-dry them at low temperature;
(2)称取40重量份干燥后的木槿花,将其放入搅碎机搅碎成粉,过40目筛,得到木槿花粉末;(2) Take by weighing 40 parts by weight of dried hibiscus, put it into a pulverizer and grind it into powder, and cross a 40-mesh sieve to obtain hibiscus powder;
(3)加入木槿花粉末3倍重量的去离子水浸泡,加2.5mol/L盐酸调pH至4,加1重量份纤维素酶,充分搅拌,置40~50℃恒温水浴中1.5h,加木槿花粉末5倍质量浓度为75%的乙醇溶液回流提取1h,趁热过滤,得第一次提取液和药渣;(3) Add 3 times the weight of hibiscus flower powder to soak in deionized water, add 2.5mol/L hydrochloric acid to adjust the pH to 4, add 1 part by weight of cellulase, stir well, put it in a constant temperature water bath at 40-50°C for 1.5h, add Hibiscus flower powder 5 times the mass concentration of 75% ethanol solution for reflux extraction for 1 hour, filtered while hot, to obtain the first extract and dregs;
(4)往药渣中加药渣5倍重量的质量浓度为50%的乙醇溶液回流提取1h,趁热过滤,得第二次提取液;(4) Adding 5 times the mass concentration of the medicinal residues to the medicinal residues is reflux extraction of 50% ethanol solution for 1 hour, and filtering while hot to obtain the second extract;
(5)两次滤液合并,旋转蒸发仪蒸发,回收乙醇,离心,取上层清液用,正丁醇萃取3次,挥发正丁醇,得到木槿花提取物。(5) The two filtrates were combined, evaporated by a rotary evaporator, recovered ethanol, centrifuged, used for supernatant, extracted with n-butanol for 3 times, and volatilized n-butanol to obtain hibiscus flower extract.
所述的含白毛藤、木槿花提取物的修复保湿水,是按照以下方法制备得到的:The described repairing and moisturizing water containing the extracts of vine and hibiscus is prepared according to the following method:
(1)在去离子水中加入丙二醇、甘油、β-葡聚糖、尿囊素、水溶性霍霍巴油、柠檬酸和乙二胺四乙酸二钠,并加热至80℃,保温状态下,搅拌30min至均匀,得到物料A;(1) Add propylene glycol, glycerin, β-glucan, allantoin, water-soluble jojoba oil, citric acid and disodium edetate into deionized water, and heat to 80°C. 30min to uniformity, to obtain material A;
(2)将物料A降温至40℃,加入苯氧乙醇、白毛藤提取物和木槿花提取物,继续搅拌至均匀,得到物料B;(2) Cool down the material A to 40°C, add phenoxyethanol, extracts of the white hair rattan and hibiscus flower extract, continue to stir until uniform, and obtain the material B;
(3)物料B冷却至-5~-10℃,保温60min后,过滤,最后杀菌即得修复保湿水。(3) Material B is cooled to -5~-10°C, kept warm for 60 minutes, filtered, and finally sterilized to obtain repairing moisturizing water.
实施例3Example 3
1)配方1) Recipe
一种含有白毛藤、木槿花提取物的修复保湿水由如下重量份的组分组成:A repairing and moisturizing water containing extracts of vine and hibiscus consists of the following components by weight:
白毛藤提取液:15份;木槿花提取液:25份;丙二醇:3份;甘油:1份;β-葡聚糖:1份;尿囊素:2份;水溶性霍霍巴油:0.4份;EDTA二钠:0.003份;柠檬酸:2份;苯氧乙醇0.2份;去离子水54.498份。Alba vine extract: 15 parts; Hibiscus flower extract: 25 parts; Propylene glycol: 3 parts; Glycerin: 1 part; β-glucan: 1 part; Allantoin: 2 parts; Water-soluble jojoba oil: 0.4 0.003 parts of disodium EDTA; 2 parts of citric acid; 0.2 parts of phenoxyethanol; 54.498 parts of deionized water.
2)制备2) Preparation
所述的白毛藤提取物,是按照以下方法制备得到的:The extract of the vine extract is prepared according to the following method:
(1)称取白毛藤洗净晾干,将其磨成粉末,过60目筛得白毛藤粉末,称取20~50重量份;(1) Take the white hair rattan, wash and dry it, grind it into powder, and pass through a 60-mesh sieve to get the white hair rattan powder, and take 20 to 50 parts by weight;
(2)将白毛藤粉末分散于去离子水中,搅拌充分混合得白毛藤悬浮液;白毛藤粉末与去离子水的质量比为1:10~1:20;(2) Disperse the white hair rattan powder in deionized water, stir and mix thoroughly to get the white hair rattan suspension; the mass ratio of the white hair rattan powder to the deionized water is 1:10~1:20;
(3)加热白毛藤悬浮液至40~55℃,接着加入1.0-1.5重量份纤维素酶,搅拌,充分反应2-3h;(3) Heating the suspension of rattan to 40-55° C., then adding 1.0-1.5 parts by weight of cellulase, stirring, and fully reacting for 2-3 hours;
(4)在步骤(3)的混合溶液中加入1.2重量份的果胶酶,搅拌,充分反应1-2h;(4) Add 1.2 parts by weight of pectinase to the mixed solution of step (3), stir, and fully react for 1-2h;
(5)步骤(4)混合溶液降低温度至35~50℃,用2.5mol/L的盐酸调节pH至4~5,过滤,除去滤渣;(5) The temperature of the mixed solution in step (4) is lowered to 35-50° C., the pH is adjusted to 4-5 with 2.5 mol/L hydrochloric acid, filtered, and the filter residue is removed;
(6)将滤液浓缩至150重量份,即得白毛藤提取物。(6) Concentrate the filtrate to 150 parts by weight to obtain the Rhizoma alba extract.
所述木槿花提取物的制备方法如下:The preparation method of the hibiscus flower extract is as follows:
(1)将刚采摘的新鲜木槿花洗净沥干,将其花瓣分离,再将其低温冻干;(1) Wash and drain the freshly picked hibiscus flowers, separate the petals, and freeze-dry them at low temperature;
(2)称取40重量份干燥后的木槿花,将其放入搅碎机搅碎成粉,过40目筛,得到木槿花粉末;(2) Take by weighing 40 parts by weight of dried hibiscus, put it into a pulverizer and grind it into powder, and cross a 40-mesh sieve to obtain hibiscus powder;
(3)加入木槿花粉末3倍重量的去离子水浸泡,加2.5mol/L盐酸调pH至4,加1重量份纤维素酶,充分搅拌,置40~50℃恒温水浴中1.5h,加木槿花粉末5倍质量浓度为75%的乙醇溶液回流提取1h,趁热过滤,得第一次提取液和药渣;(3) Add 3 times the weight of hibiscus flower powder to soak in deionized water, add 2.5mol/L hydrochloric acid to adjust the pH to 4, add 1 weight part of cellulase, stir well, put it in a constant temperature water bath at 40-50°C for 1.5h, add Hibiscus flower powder 5 times the mass concentration of 75% ethanol solution for reflux extraction for 1 hour, filtered while hot, to obtain the first extract and dregs;
(4)往药渣中加药渣5倍重量的质量浓度为50%的乙醇溶液回流提取1h,趁热过滤,得第二次提取液;(4) Adding 5 times the mass concentration of the medicinal residues to the medicinal residues is reflux extraction of 50% ethanol solution for 1 hour, and filtering while hot to obtain the second extract;
(5)两次滤液合并,旋转蒸发仪蒸发,回收乙醇,离心,取上层清液用,正丁醇萃取3次,挥发正丁醇,得到木槿花提取物。(5) The two filtrates were combined, evaporated by a rotary evaporator, ethanol was recovered, centrifuged, the supernatant was taken, extracted with n-butanol three times, and n-butanol was volatilized to obtain hibiscus flower extract.
所述的含白毛藤、木槿花提取物的修复保湿水,是按照以下方法制备得到的:The described repairing and moisturizing water containing the extracts of vine and hibiscus is prepared according to the following method:
(1)在去离子水中加入丙二醇、甘油、β-葡聚糖、尿囊素、水溶性霍霍巴油、柠檬酸和乙二胺四乙酸二钠,并加热至80℃,保温状态下,搅拌30min至均匀,得到物料A;(1) Add propylene glycol, glycerin, β-glucan, allantoin, water-soluble jojoba oil, citric acid and disodium edetate into deionized water, and heat to 80°C. 30min to uniformity, to obtain material A;
(2)将物料A降温至40℃,加入苯氧乙醇、白毛藤提取物和木槿花提取物,继续搅拌至均匀,得到物料B;(2) Cool down the material A to 40°C, add phenoxyethanol, extracts of the white hair rattan and hibiscus flower extract, continue to stir until uniform, and obtain the material B;
(3)物料B冷却至-5~-10℃,保温60min后,过滤,最后杀菌即得修复保湿水。(3) Material B is cooled to -5~-10°C, kept warm for 60 minutes, filtered, and finally sterilized to obtain repairing moisturizing water.
试验例1感官检验Test Example 1 Sensory Test
1.1外观:取试样在室温和非阳光直射下目测观察。1.1 Appearance: Take the sample and observe it visually at room temperature and without direct sunlight.
1.2香气:先将等量的试样和规定试样(按企业内部规定)分别放在相同的容器内,用宽0.5cm~1.0cm、长10cm~15cm的吸水纸作为评香纸,分别蘸取试样和规定试样约1cm-2cm(两者应接近),用嗅觉来鉴别。1.2 Fragrance: First put the same amount of samples and specified samples (according to the internal regulations of the enterprise) in the same container, use absorbent paper with a width of 0.5cm to 1.0cm and a length of 10cm to 15cm as the fragrance evaluation paper, and dip them in Take the sample and the specified sample about 1cm-2cm (the two should be close to each other), and use the sense of smell to identify.
表1.感官检验结果:Table 1. Sensory test results:
试验例2理化指标检验Test example 2 physical and chemical index inspection
2.1 pH:按GB/T135531.1中规定的方法测定(直测法)。2.1 pH: Measured according to the method specified in GB/T135531.1 (direct measurement method).
2.2耐热2.2 heat resistance
2.2.1仪器:恒温培养箱:温控精度±1℃。2.2.1 Instrument: constant temperature incubator: temperature control accuracy ± 1 ℃.
2.2.2操作程序:预先将恒温培养箱调节到(40±1)℃,把包装好完整的试样一瓶置于恒温培养箱内。24h后取出,恢复至室温后目测观察。2.2.2 Operating procedures: adjust the constant temperature incubator to (40±1)°C in advance, and place a bottle of the packaged complete sample in the constant temperature incubator. Take it out after 24 hours, and observe it visually after returning to room temperature.
2.3耐寒2.3 cold resistance
2.3.1仪器:恒温培养箱:温控精度±1℃。2.3.1 Instrument: constant temperature incubator: temperature control accuracy ± 1 ℃.
2.3.2操作程序:预先将恒温培养箱调节到(5士1)℃,把包装完整的试样一瓶置于恒温培养箱内。24h后取出,恢复至室温后目测观察。2.3.2 Operating procedures: adjust the constant temperature incubator to (5±1)°C in advance, and place a bottle of the fully packaged sample in the constant temperature incubator. Take it out after 24 hours, and observe it visually after returning to room temperature.
表2.理化检验结果:Table 2. Physical and chemical test results:
试验例3产品皮肤刺激性/腐蚀性测试Test Example 3 Product skin irritation/corrosion test
根据《化妆品卫生规范》(2015年版)皮肤刺激性/腐蚀性试验对实施例1~3的含白毛藤和木槿花提取物修复保湿水进行皮肤反应评分,测试本发明对哺乳动物皮肤局部是否具有刺激作用或腐蚀作用及其程度。具体操作如下:According to " Hygienic Standards for Cosmetics " (2015 edition) skin irritation/corrosion test carries out skin reaction score to the repairing moisturizing water containing the extracts of vine and hibiscus flower of embodiments 1 to 3, and tests whether the present invention has local effects on mammalian skin Irritation or corrosion and its degree. The specific operation is as follows:
3.1受试物:实施例1~3的含白毛藤和木槿花提取物修复保湿水,不需稀释,可直接使用原液。3.1 Tested substance: the repairing and moisturizing lotion containing the extracts of vine and hibiscus flower in Examples 1-3, the original solution can be used directly without dilution.
3.2实验动物和饲养环境3.2 Experimental animals and feeding environment
首选4只成年、健康、皮肤无损伤的白色家兔,雌性和雄性均可,但雌性动物应是未孕和未曾严产仔的。实验动物应单笼饲养,试验前动物要在实验动物房环境中至少适应3d时间。The first choice is 4 adult, healthy white rabbits with no skin damage, both female and male, but the female animals should be non-pregnant and have never given birth. The experimental animals should be kept in single cages, and the animals should be acclimatized in the environment of the experimental animal room for at least 3 days before the experiment.
实验动物及实验动物房符合国家相应规定。选用标准配合饲料,饮水不限制。Experimental animals and experimental animal rooms comply with the corresponding national regulations. Standard compound feed was selected, and drinking water was not restricted.
3.3急性皮肤刺激性试验步骤3.3 Acute skin irritation test procedure
3.3.1试验前约24h,将实验动物背部脊柱两侧毛剪掉,不可损伤表皮,去毛范围左、右各约3cmx3cm。3.3.1 About 24 hours before the test, cut off the hair on both sides of the back and spine of the experimental animal, without damaging the epidermis, and the left and right sides of the hair removal area are about 3cmx3cm each.
3.3.2取实施例1~3的含白毛藤和木槿花提取物修复保湿水约0.5mL(g)直接涂在皮肤上,然后用二层纱布(2.5cmx2.5cm)和一层玻璃纸或类似物覆盖,再用无刺激性胶布和绷带加以固定。另一侧皮肤作为对照。采用封闭试验。每天涂抹1次,连续涂抹14d。从第二天开始,每次涂抹前剪毛,用水清除残留受试物。1小时后观察涂抹部位皮肤反应,按表3、4进行皮肤反应评分,对照区和试验区同样处理。3.3.2 Take about 0.5mL (g) of the repairing and moisturizing water containing the extracts of vine and hibiscus in Examples 1-3 and apply it directly on the skin, and then use two layers of gauze (2.5cmx2.5cm) and a layer of cellophane or similar Cover with non-irritating adhesive tape and bandages. The skin on the other side served as a control. A closed test is used. Apply once a day for 14 days. From the second day on, the hair was clipped before each application, and the residual test substance was removed with water. After 1 hour, observe the skin reaction at the application site, and score the skin reaction according to Table 3 and 4, and treat the control area and the test area in the same way.
3.3.3结果评价:按下列公式计算每天每只动物平均积分。以表5判定皮肤刺激强度。3.3.3 Result evaluation: Calculate the average score of each animal per day according to the following formula. Table 5 was used to determine the intensity of skin irritation.
每天每只动物平均积分=(∑红斑水肿积分/受试动物数)/14Average score per animal per day = (∑ erythematous edema score/number of animals tested)/14
皮肤刺激反应评价标准:Skin irritation evaluation criteria:
表3皮肤红斑和焦痂评价标准Table 3 Evaluation criteria for skin erythema and eschar
表4皮肤水肿评价标准Table 4 Skin edema evaluation criteria
表5皮肤刺激性评价标准Table 5 Skin irritation evaluation criteria
表6皮肤刺激强度评分结果Table 6 Skin irritation intensity score results
结论:由表6知,试验区和对照区,几乎无红斑形成,和水肿出现,说明该含白毛藤和木槿花提取物修复保湿水对白色家兔的皮肤无刺激性。Conclusion: Known from Table 6, there is almost no erythema formation and edema in the test area and the control area, indicating that the repairing and moisturizing water containing the extracts of vine and hibiscus has no irritation to the skin of white rabbits.
试验例4人体对照试验Test Example 4 Human Controlled Test
对本发明进行皮肤刺激实验,选取皮肤健康的6名成年女性做皮肤刺激实验,以前臂内侧区域为受试部位,一侧为实验区,另一侧为对照区,取化妆棉三块,分别涂上含实施例1制备的白毛藤和木槿花保湿水0.05g、娥佩兰薏仁水0.05g、薇诺娜舒敏保湿润肤水0.05g,贴在前臂内侧实验区,用医用胶布固定,试验期间适用者不食用辛辣食物、刺激性食物,实验部位不沾水。24h揭开观察.观查结果见表7。Carry out skin stimulation test to the present invention, choose 6 adult females with healthy skin to do skin stimulation test, forearm medial area is test site, one side is experiment area, the other side is control area, take three pieces of cotton pads, apply respectively It contains 0.05g of white hair rattan and hibiscus flower moisturizing water prepared in Example 1, 0.05g of Epeilan barley water, and 0.05g of Winona Shumin moisturizing lotion, and sticks it on the experimental area on the inner side of the forearm, and fixes it with medical adhesive tape. Applicable persons do not eat spicy food or irritating food, and the experimental site does not touch water. 24h to uncover the observation. The observation results are shown in Table 7.
表7.含白毛藤、木槿花提取物的修复保湿水皮肤试验检测结果:Table 7. Skin test results of the repairing moisturizing water containing the extracts of vine and hibiscus:
测试结果:实验组含白毛藤、木槿花提取物的修复保湿水和对照组已上市的薏仁水、薇诺娜舒敏保湿润肤水的结果无明显差异,和对照区也无差异。Test results: There was no significant difference in the results of the experimental group's repairing moisturizing water containing the extracts of Alba vine and hibiscus flower, and the results of the control group's marketed barley water and Winona Shumin moisturizing lotion, and there was no difference between the results of the control group.
试验例5产品功效评价Test Example 5 Product Efficacy Evaluation
5.1保湿效果测试:重量法测定失水率实验5.1 Moisturizing effect test: Determination of water loss rate experiment by gravimetric method
5.1.1测试前准备重量法测定保湿剂失水率须在恒温、恒湿环境下进行。5.1.1 Preparation before the test The gravimetric method to determine the water loss rate of the humectant must be carried out in a constant temperature and humidity environment.
5.1.2实验前一日,在干燥器底部放置一定体积的饱和碳酸钾溶液,使液体深度大于1cm,其上放置多孔隔板,盖上盖子,保持密封状态,放置于25℃环境中,待空气中水蒸气分压恒定后,可维持约43%的相对湿度。5.1.2 One day before the experiment, place a certain volume of saturated potassium carbonate solution at the bottom of the desiccator to make the liquid depth greater than 1cm, place a porous partition on it, cover it with a lid, keep it sealed, and place it in an environment of 25°C. After the partial pressure of water vapor in the air is constant, it can maintain a relative humidity of about 43%.
5.1.3以实施例1~3的含白毛藤、木槿花提取物的修复保湿水作为待测样品。5.1.3 The repairing and moisturizing water containing the extracts of vine and hibiscus in Examples 1 to 3 was used as the sample to be tested.
5.1.4称取一定量试样,均匀涂覆在贴有3M胶带的玻璃板(5cm×5cm的相对湿度。样品用量约为2mg/cm2,置于盛有碳酸钾饱和水溶液(RH43%)的干燥器内,放置段时间后(2h、4h、6h、8h)称量样品的质量,平行三次实验,取平均值。5.1.4 Weigh a certain amount of sample, and evenly coat it on a glass plate with 3M adhesive tape (5cm×5cm relative humidity. The amount of sample is about 2mg/cm2, and place it in a container filled with a saturated aqueous solution of potassium carbonate (RH43%) In the desiccator, weigh the mass of the sample after standing for a period of time (2h, 4h, 6h, 8h), perform three experiments in parallel, and take the average value.
5.1.5计算失水率。5.1.5 Calculate the water loss rate.
5.1.6失水率 5.1.6 Water loss rate
M1-放置前样品的质量;M 1 - the mass of the sample before placement;
M2-放置后样品的质量。M 2 - the mass of the sample after standing.
5.1.7失水率结果见表7.5.1.7 The results of water loss rate are shown in Table 7.
表7.失水率测试结果Table 7. Water loss test results
5.2抗菌效果测试:5.2 Antibacterial effect test:
5.2.1细菌培养:试验前取金黄色葡萄球菌、大肠埃希菌、沙门菌、铜绿假单胞菌、白色念珠菌等新鲜菌种斜面,,接种至营养肉汤培养基和改良马丁培养基中,于适宜温度培养适宜时间后,以生理盐水稀释至适宜浓度,测定活菌数,备用。5.2.1 Bacterial culture: Take Staphylococcus aureus, Escherichia coli, Salmonella, Pseudomonas aeruginosa, Candida albicans and other fresh strains before the test, and inoculate them into nutrient broth medium and modified Martin medium After incubating at a suitable temperature for a suitable time, dilute it with normal saline to a suitable concentration, measure the number of viable bacteria, and set aside.
5.2.2试验时取灭菌小试管若干支,用相应的培养基稀释实施例1含白毛藤、木槿花提取物的修复保湿水分别为100、50、25、12.5、6.25、3.12、1.56、0.78mg/ml分别装入每管各1ml取适宜的稀释级菌液0.1ml于各抑菌试管中,接种量为105试验菌,摇匀,使试验菌与药液充分接触,置于37℃培养箱内培养16-24观察试验菌生长情况。以细菌不生长的最低药物浓度为该药物的最低抑菌浓度。5.2.2 During the test, take several sterilized small test tubes, and dilute the repairing moisturizing water containing the extracts of vine and hibiscus flower in Example 1 with the corresponding medium to 100, 50, 25, 12.5, 6.25, 3.12, 1.56 respectively , 0.78mg/ml into 1ml of each tube, take 0.1ml of appropriate dilution grade bacteria solution in each antibacterial test tube, the inoculation amount is 105 test bacteria, shake well, make the test bacteria fully contact with the medicine solution, place in 37 Cultivate in the incubator for 16-24 to observe the growth of the test bacteria. The minimum inhibitory concentration of the drug is defined as the lowest drug concentration at which bacteria do not grow.
5.2.3抑菌结果见表8.5.2.3 The antibacterial results are shown in Table 8.
表8.含白毛藤、木槿花提取物的修复保湿水的抑菌效果测定结果:Table 8. Determination of the antibacterial effect of the repairing moisturizing water containing the extracts of Alba vine and hibiscus:
备注:--表示没有长菌,+表示少量长菌,++表示适度长菌,+++表示大量长菌。Remarks: -- indicates no bacteria growth, + indicates a small amount of bacteria growth, ++ indicates moderate bacteria growth, and +++ indicates a large number of bacteria growth.
表9.含白毛藤、木槿花提取物的修复保湿水的抑菌抑菌圈结果:Table 9. The results of antibacterial and antibacterial zones of the repairing moisturizing water containing the extracts of vine and hibiscus:
由表8知,含白毛藤、木槿花提取物的修复保湿水对金黄色葡萄球菌,大肠埃杀菌,沙门菌,白色念珠菌的最低抑菌浓度(MIC)为100mg/ml,对铜绿假单胞菌的最低抑菌浓度(MIC)为50mg/ml。Known from Table 8, the repairing moisturizing water containing the extracts of Alba vine and hibiscus is 100mg/ml to Staphylococcus aureus, Escherichia coli, Salmonella, Candida albicans minimum inhibitory concentration (MIC), and is 100mg/ml to Pseudomonas aeruginosa The minimum inhibitory concentration (MIC) of monocellular bacteria is 50mg/ml.
根据抗菌圈试验判定标准:抗菌圈直径大于20mm为极敏感;15~20mm为高敏感;10~15mm,为中敏感;7~9mm为低敏感;小于7mm为不敏感。由表9可知,含白毛藤、木槿花提取物的修复保湿水对以上三种常见的细菌都有一定的抗菌性。According to the judgment standard of the antibacterial circle test: the antibacterial circle diameter greater than 20mm is extremely sensitive; 15-20mm is highly sensitive; 10-15mm is moderately sensitive; 7-9mm is low-sensitive; less than 7mm is not sensitive. It can be seen from Table 9 that the repairing moisturizing water containing the extracts of Alba vine and Hibiscus flower has certain antibacterial properties against the above three common bacteria.
试验例6人体体验感评价Test Example 6 Evaluation of Human Experience
邀请90位20~50岁之间、皮肤健康的女性志愿者,随机分为9组,每组20人,平均年龄22±2岁,分别试用实施例1~3制得的保湿水,观察和感受使用效果。使用方法:志愿者清洁脸部后,将上述保湿水大约3mL倒在化妆棉上,润湿化妆棉却又不会滴落,且确定棉片方向,使得棉片纤维走向与手指垂直,将棉片全部覆盖在肌肤表面,轻轻用手指按压,轻轻擦拭,使得修复保湿水渗透进入肌肤,擦拭后,用轻拍的方式加速渗透,每日早晚各使用一次,坚持使用一个月,每周至少检查一次以了解有无全身及局部不良反应,并详细记录结果。测试评估结果如下表10:Invite 90 female volunteers with healthy skin between the ages of 20 and 50, and randomly divide them into 9 groups, 20 people in each group, with an average age of 22 ± 2 years old, try the moisturizing water prepared in Examples 1 to 3 respectively, observe and Feel the effect of use. How to use: After the volunteer cleans the face, pour about 3mL of the above moisturizing water on the cotton pad, moisten the cotton pad without dripping, and determine the direction of the cotton pad so that the fiber direction of the cotton pad is perpendicular to the finger, put the cotton pad All the tablets cover the skin surface, gently press with your fingers, and wipe gently, so that the repairing moisturizing water penetrates into the skin, after wiping, use the way of patting to speed up the penetration, use it once a day in the morning and evening, insist on using it for a month, every week Check at least once for systemic and local adverse reactions, and record the results in detail. The test evaluation results are shown in Table 10:
表10.含白毛藤、木槿花提取物的修复保湿水的试用(一个月)反馈总结表Table 10. Feedback summary table for the trial (one month) of the repairing moisturizing water containing the extracts of Alba vine and Hibiscus flower
由上表10可知:It can be seen from Table 10 above that:
本发明实广受试用志愿者的喜爱和认可,试用志愿者表示该款修复保湿水温和亲肤、不刺激、易吸收,使用后脸部清爽不油腻,试用一个月后感觉皮肤干燥、粗糙、红血丝等问题得到明显改善,毛孔减少,皮肤变得光滑水润,有弹性。The invention is widely loved and recognized by the trial volunteers. The trial volunteers said that the repairing moisturizing water is warm, skin-friendly, non-irritating, and easy to absorb. After use, the face is refreshing and not greasy. After a month of trial, the skin feels dry, rough, and red. Problems such as bloodshot eyes have been significantly improved, pores have been reduced, and the skin has become smooth, hydrated and elastic.
同时全部试用志愿者中未有人出现过敏现象,也均未出现皮肤瘙痒、刺痛、红肿等状况。At the same time, none of the trial volunteers experienced allergies, nor did they experience skin itching, tingling, redness and swelling.
因此,本发明一种含白毛藤和木槿花提取物的修复保湿水温和安全,可长期使用。Therefore, a kind of repairing and moisturizing water containing the extracts of vine and hibiscus of the present invention is warm and safe, and can be used for a long time.
上述实施例仅例示性说明本发明的原理及其功效,而非用于限制本发明。任何熟悉此技术的人士皆可在不违背本发明的精神及范畴下,对上述实施例进行修饰或改变。因此,举凡所属技术领域中具有通常知识者在未脱离本发明所揭示的精神与技术思想下所完成的一切等效修饰或改变,仍应由本发明的权利要求所涵盖。The above-mentioned embodiments only illustrate the principles and effects of the present invention, but are not intended to limit the present invention. Anyone skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Therefore, all equivalent modifications or changes made by those skilled in the art without departing from the spirit and technical ideas disclosed in the present invention should still be covered by the claims of the present invention.
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