CN103520078A - Silkworm pupa polypeptide skin-smoothing mask and preparation method thereof - Google Patents
Silkworm pupa polypeptide skin-smoothing mask and preparation method thereof Download PDFInfo
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- 241000255789 Bombyx mori Species 0.000 title claims abstract description 123
- 108090000765 processed proteins & peptides Proteins 0.000 title claims abstract description 85
- 102000004196 processed proteins & peptides Human genes 0.000 title claims abstract description 79
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- 238000002360 preparation method Methods 0.000 title claims description 13
- 241000382353 Pupa Species 0.000 title abstract description 9
- 238000009499 grossing Methods 0.000 title abstract description 3
- 102000004169 proteins and genes Human genes 0.000 claims abstract description 68
- 108090000623 proteins and genes Proteins 0.000 claims abstract description 68
- 239000000284 extract Substances 0.000 claims abstract description 26
- 239000000843 powder Substances 0.000 claims abstract description 23
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 21
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- 235000008390 olive oil Nutrition 0.000 claims abstract description 10
- 229940055729 papain Drugs 0.000 claims abstract description 10
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- 229940010747 sodium hyaluronate Drugs 0.000 claims description 3
- YWIVKILSMZOHHF-QJZPQSOGSA-N sodium;(2s,3s,4s,5r,6r)-6-[(2s,3r,4r,5s,6r)-3-acetamido-2-[(2s,3s,4r,5r,6r)-6-[(2r,3r,4r,5s,6r)-3-acetamido-2,5-dihydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-2-carboxy-4,5-dihydroxyoxan-3-yl]oxy-5-hydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-3,4,5-trihydroxyoxane-2- Chemical compound [Na+].CC(=O)N[C@H]1[C@H](O)O[C@H](CO)[C@@H](O)[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@H](O[C@H]2[C@@H]([C@@H](O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@H](O3)C(O)=O)O)[C@H](O)[C@@H](CO)O2)NC(C)=O)[C@@H](C(O)=O)O1 YWIVKILSMZOHHF-QJZPQSOGSA-N 0.000 claims description 3
- XFNJVJPLKCPIBV-UHFFFAOYSA-N trimethylenediamine Chemical compound NCCCN XFNJVJPLKCPIBV-UHFFFAOYSA-N 0.000 claims description 3
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- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims description 2
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- Cosmetics (AREA)
Abstract
Description
the
技术领域 technical field
本发明涉及化妆品、护肤品技术领域,特别涉及一种蚕蛹多肽嫩肤面膜,还涉及蚕蛹多肽嫩肤面膜的制备方法。 The invention relates to the technical field of cosmetics and skin care products, in particular to a silkworm chrysalis polypeptide skin rejuvenating mask, and also relates to a preparation method of the silkworm chrysalis polypeptide skin rejuvenating mask.
背景技术 Background technique
蚕蛹(silkworm pupa),为蚕蛾科昆虫家蚕蛾的蛹,是丝绸工业的主要副产品。我国是丝绸工业大国,每年仅缫丝厂下脚料就有几十万吨,蚕蛹资源极为丰富,但由于缺乏深加工技术,大部分蚕蛹都作为饲料或肥料使用,甚至被直接丢弃,资源利用率和附加值低,造成了极大的浪费。 Silkworm pupa ( silkworm pupa ) is the chrysalis of Bombyx mori , the silkworm moth, and is the main by-product of the silk industry. my country is a big country in the silk industry. There are hundreds of thousands of tons of leftovers from silk reeling factories every year. Silkworm chrysalis resources are extremely rich. However, due to the lack of deep processing technology, most of the silkworm chrysalis are used as feed or fertilizer, or even discarded directly. The resource utilization rate and The added value is low, resulting in great waste.
蚕蛹含多种活性物质,其中蚕蛹蛋白含量约为干蚕蛹的45%-50%,是一种具有极大开发潜力的天然蛋白资源。蚕蛹蛋白属于全价蛋白,经测定在蚕蛹蛋白中含有18种氨基酸,包含8种人体必需的氨基酸,且必需氨基酸含量达到80%,组成合理,符合联合国粮农组织(FAO)和世界卫生组织(WHO)的相关要求,是一种优质蛋白资源。研究发现,蚕蛹蛋白具有促进生长发育、补充机体营养、抗氧化、抗疲劳、抗衰老、提高人体免疫功能等多种功能,其精深加工愈来愈受到关注。 Silkworm chrysalis contains a variety of active substances, among which the protein content of silkworm chrysalis is about 45%-50% of that of dry silkworm chrysalis. It is a natural protein resource with great development potential. Silkworm chrysalis protein is a complete protein. It has been determined that silkworm chrysalis protein contains 18 kinds of amino acids, including 8 kinds of amino acids necessary for human body, and the content of essential amino acids reaches 80%. ) is a high-quality protein resource. Studies have found that silkworm chrysalis protein has multiple functions such as promoting growth and development, supplementing body nutrition, anti-oxidation, anti-fatigue, anti-aging, and improving human immune function, and its intensive processing has attracted more and more attention.
蚕蛹多作为饲料用,浪费了其中的活性蛋白成分,如果能通过将其应用于化妆品生产中,利用其所具备的自由基清除能力来起到延缓皮肤衰老的作用,能提高其附加值,带来巨大的经济效益。 Silkworm chrysalis is mostly used as feed, wasting the active protein components in it. If it can be used in the production of cosmetics and use its free radical scavenging ability to delay skin aging, it can increase its added value and bring to huge economic benefits.
将蚕蛹应用于化妆品生产行业,有以下需要克服和解决的问题: Applying silkworm chrysalis to the cosmetics production industry has the following problems that need to be overcome and solved:
1.缫丝过程一般需经过高温处理,因此蚕蛹蛋白热变性程度高,溶解性较差,如将其直接应用于化妆品制备中,不容易为皮肤所吸收;须将其转变为可溶性的易于为皮肤所吸收的物质; 1. The silk reeling process generally requires high temperature treatment, so the silkworm chrysalis protein has a high degree of thermal denaturation and poor solubility. If it is directly used in the preparation of cosmetics, it is not easy to be absorbed by the skin; Substances absorbed by the skin;
2.蚕蛹蛋白为高蛋白含量的物质,由于部分人群对高蛋白过敏,如果将其中所含的蛋白成分直接应用于化妆品行业,也会导致部分使用人群产生过敏现象。 2. Silkworm chrysalis protein is a substance with high protein content. Since some people are allergic to high protein, if the protein ingredients contained in it are directly used in the cosmetics industry, it will also cause allergies to some users. the
发明内容 Invention content
为了解决以上蚕蛹蛋白在化妆品中应用所存在的问题,本发明提供了一种过敏率低、活性成分较大限度的保留且易于为人体所吸收的蚕蛹多肽嫩肤膜。 In order to solve the above problems in the application of silkworm chrysalis protein in cosmetics, the present invention provides a silkworm chrysalis polypeptide skin rejuvenation film with low allergy rate, maximum retention of active ingredients and easy absorption by human body.
本发明还提供了所述蚕蛹多肽嫩肤膜的制备方法。 The invention also provides a preparation method of the silkworm chrysalis polypeptide skin rejuvenation film.
本发明是通过以下措施实现的: The present invention is achieved through the following measures:
一种蚕蛹多肽嫩肤面膜,含有以下重量配比的原料: A silkworm chrysalis polypeptide rejuvenating facial mask contains the following raw materials in weight ratio:
蚕蛹蛋白多肽5~10份,迷迭香精油1~2份,石榴籽提取物1~3份,海藻提取物1~6份,甘油3~6份,橄榄油 1~4,辛酸癸酸甘油三酯2~5份,珍珠粉 1~3份。 Silkworm chrysalis protein polypeptide 5-10 parts, rosemary essential oil 1-2 parts, pomegranate seed extract 1-3 parts, seaweed extract 1-6 parts, glycerin 3-6 parts, olive oil 1-4 parts, caprylic acid glycerin Triester 2-5 parts, pearl powder 1-3 parts.
石榴籽提取物和海藻提取物均为醇提取物。 Both pomegranate seed extract and seaweed extract are alcoholic extracts.
蚕蛹多肽嫩肤面膜中还含有防腐剂0.05~0.1份,增稠剂1~5份,乳化剂1~2份,乙醇3-5份,去离子水30~40份。 The silkworm chrysalis polypeptide rejuvenating facial mask also contains 0.05-0.1 parts of preservatives, 1-5 parts of thickeners, 1-2 parts of emulsifiers, 3-5 parts of ethanol, and 30-40 parts of deionized water.
优选所述防腐剂为对羟基苯甲酸甲酯、对羟基苯甲酸乙酯、对羟基苯甲酸丙酯、苯甲酸和苯氧乙醇中的一种以上。 Preferably, the preservative is one or more of methyl p-hydroxybenzoate, ethyl p-hydroxybenzoate, propyl p-hydroxybenzoate, benzoic acid and phenoxyethanol.
优选所述增稠剂为果胶、透明质酸钠、瓜尔胶、汉生胶、 丙烯酸酯、十六烷基乙氧基(20)衣康酸酯共聚物、十六烷基乙氧基(20)甲基丙烯酸酯共聚物、羧甲基纤维素、纤维素胶、乙基纤维素、小麦胚芽氨基丙基氧化胺和大豆氨基丙基氧化胺中的一种以上。 Preferably, the thickener is pectin, sodium hyaluronate, guar gum, xanthan gum, acrylate, cetyl ethoxy (20) itaconate copolymer, cetyl ethoxy (20) More than one of methacrylate copolymer, carboxymethyl cellulose, cellulose gum, ethyl cellulose, wheat germ aminopropyl amine oxide and soybean aminopropyl amine oxide.
优选所述乳化剂为吐温20、吐温-60和吐温80中的一种以上。 Preferably, the emulsifier is more than one of Tween 20, Tween-60 and Tween 80.
优选所述的蚕蛹蛋白多肽是通过以下步骤得到的: Preferably, the silkworm chrysalis protein polypeptide is obtained through the following steps:
(1)配制蚕蛹蛋白水溶液,加入木瓜蛋白酶酶解,加酶量8000-60000IU/g蚕蛹蛋白,酶解结束后灭酶得到酶解液; (1) Prepare silkworm chrysalis protein aqueous solution, add papain enzymolysis, add enzyme amount 8000-60000IU/g silkworm chrysalis protein, after enzymolysis finishes, kill enzyme to obtain enzymolysis solution;
(2)调节酶解液pH至8.0~11.0,加入Esperase蛋白酶,加酶量0.075-0.225KNPU/g蚕蛹蛋白,酶解; (2) Adjust the pH of the enzymatic hydrolysis solution to 8.0-11.0, add Esperase protease, the amount of enzyme added is 0.075-0.225KNPU/g silkworm chrysalis protein, and enzymatically hydrolyze;
(3)步骤(2)的产物灭酶后过滤除去不溶物,滤液过超微滤膜,收集分子量为3000Da以下的滤液; (3) After the product of step (2) deactivates the enzyme, it is filtered to remove insoluble matter, the filtrate is passed through an ultra-microfiltration membrane, and the filtrate with a molecular weight of less than 3000 Da is collected;
(4)滤液经脱色、脱盐、浓缩、干燥,得蚕蛹蛋白多肽。 (4) The filtrate is decolorized, desalted, concentrated and dried to obtain the silkworm chrysalis protein polypeptide.
优选木瓜蛋白酶加酶量为20000IU/g蚕蛹蛋白,Esperase蛋白酶加酶量为0.15KNPU/g蚕蛹蛋白。 Preferably, the enzyme amount of papain added is 20000IU/g silkworm chrysalis protein, and the enzyme amount of Esperase protease added is 0.15KNPU/g silkworm chrysalis protein.
优选步骤(1)中酶解温度45~60℃,pH值6.5~8.0,酶解时间2~4h。 Preferably, in the step (1), the enzymolysis temperature is 45-60° C., the pH value is 6.5-8.0, and the enzymolysis time is 2-4 hours.
优选步骤(2)中酶解温度45℃~60℃,时间2~4h。 Preferably, the enzymolysis temperature in step (2) is 45°C-60°C, and the time is 2-4h.
一种含蚕蛹多肽嫩肤面膜的制备方法,包括以下步骤: A preparation method for skin rejuvenation mask containing silkworm chrysalis polypeptide, comprising the following steps:
(1)将去离子水分成两等份,将蚕蛹蛋白多肽、海藻提取物加入第一份去离子水中,加热至40℃~50℃溶解,此混合物为组分一; (1) Divide deionized water into two equal parts, add silkworm chrysalis protein polypeptide and seaweed extract to the first part of deionized water, heat to 40°C-50°C to dissolve, this mixture is component 1;
(2)将石榴籽提取物、橄榄油、辛酸癸酸甘油三酯、防腐剂用乙醇溶解,搅拌均匀,然后加入乳化剂,加热至40~45℃,充分混匀,制得组分二; (2) Dissolve pomegranate seed extract, olive oil, caprylic capric triglyceride, and preservatives in ethanol, stir evenly, then add emulsifier, heat to 40-45°C, and mix well to obtain component 2;
(3)将增稠剂置于容器中,加入另一份去离子水溶解,加入珍珠粉、甘油,加热至50℃~60℃保温5~10min,搅拌均匀,此为组分三; (3) Put the thickener in the container, add another portion of deionized water to dissolve, add pearl powder and glycerin, heat to 50°C-60°C and keep it warm for 5-10min, stir evenly, this is component three;
(4)将上述组分一、二、三混合,于60~75℃搅拌混匀,冷却后加入迷迭香精油,混合均匀即得蚕蛹多肽面膜。 (4) Mix the above components 1, 2 and 3, stir and mix at 60-75°C, add rosemary essential oil after cooling, and mix well to get silkworm chrysalis polypeptide mask.
在化妆产品的研究中,历年对生物活性多肽包括细胞生长因子尤为重视,这类物质在人体内含量甚微,但生物活性高,在多种细胞生理功能和代谢活动中起着重要的生理调节作用,直接或间接地影响细胞的生长、分裂、分化、增殖和迁移。因此,本发明拟应用生物定向酶解技术,将蚕蛹蛋白深度水解,并经进一步分离纯化,获得分子量小于3KDa的活性蚕蛹多肽,此分子量范围的小分子多肽具有具有较强的水溶性和渗透性,易于为肌肤所吸收,可以给皮肤充足的营养。除此之外,此分子量范围的蚕蛹多肽已被证明具有很强的自由基清除能力,且过敏原已完全被破坏,非常适合作为活性成分应用于护肤品中。 In the research of cosmetic products, special attention has been paid to biologically active peptides including cell growth factors over the years. These substances have very little content in the human body, but they have high biological activity and play an important role in physiological regulation of various cell physiological functions and metabolic activities. directly or indirectly affect cell growth, division, differentiation, proliferation and migration. Therefore, the present invention intends to use bio-directed enzymatic hydrolysis technology to deeply hydrolyze the silkworm chrysalis protein, and after further separation and purification, an active silkworm chrysalis polypeptide with a molecular weight of less than 3KDa is obtained. Small molecule polypeptides in this molecular weight range have strong water solubility and permeability. , easy to be absorbed by the skin, can give the skin sufficient nutrition. In addition, silkworm chrysalis polypeptides in this molecular weight range have been proven to have a strong ability to scavenge free radicals, and the allergens have been completely destroyed, making them very suitable for use as active ingredients in skin care products.
本发明的有益效果: Beneficial effects of the present invention:
本产品所使用的蚕蛹多肽,原料为丝绸产业下脚料,充分利用缫丝蚕蛹,不仅可以减少环境污染和资源浪费,而且可以增加丝绸工业的附加值,获得更高的经济效益。与动物源性胶原多肽相比,蚕蛹多肽不仅氨基酸种类、生物活性等毫不逊色,且具有无病原隐患的优势, 适合应用于护肤品。本发明所使用的蚕蛹多肽,原料价格低廉,来源丰富。蚕蛹多肽嫩肤面膜中的活性蚕蛹多肽与迷迭香提取物、石榴籽提取物等活性物质结合,能帮助肌肤抵御自由基和胶原蛋白酶的伤害,从而有效预防及对抗皱纹生成,增加皮肤弹性,延缓衰老。本发明采用蚕蛹蛋白和植物提取物为原料制备得到的面膜,天然、温和、对皮肤无刺激,而且多种活性物质协同作用于皮肤,其效果要优于普通的面膜。 The silkworm chrysalis polypeptide used in this product is made of leftovers from the silk industry. Making full use of reeled silkworm chrysalis can not only reduce environmental pollution and waste of resources, but also increase the added value of the silk industry and obtain higher economic benefits. Compared with animal-derived collagen peptides, silkworm chrysalis peptides are not only inferior in amino acid types and biological activities, but also have the advantage of no hidden pathogens, so they are suitable for skin care products. The silkworm chrysalis polypeptide used in the present invention has low raw material price and abundant sources. The active silkworm chrysalis polypeptide in the silkworm chrysalis polypeptide skin rejuvenation mask is combined with active substances such as rosemary extract and pomegranate seed extract, which can help the skin resist the damage of free radicals and collagenase, thereby effectively preventing and resisting the formation of wrinkles and increasing skin elasticity. anti aging. The facial mask prepared by using silkworm chrysalis protein and plant extracts as raw materials is natural, mild and non-irritating to the skin, and multiple active substances act synergistically on the skin, and the effect is better than that of ordinary facial masks.
具体实施方式 Detailed ways
下面结合具体实施例对本发明作更进一步的说明,以便本领域的技术人员更了解本发明,但并不因此限制本发明。以下涉及成分均按重量比。 The present invention will be further described below in conjunction with specific embodiments, so that those skilled in the art can better understand the present invention, but the present invention is not limited thereby. The following ingredients are all in weight ratio.
实施例1 Example 1
步骤一:双步酶解制备蚕蛹蛋白多肽Step 1: Two-step enzymatic hydrolysis to prepare silkworm chrysalis protein polypeptide
(1)用去离子水配制浓度12%的蚕蛹蛋白溶液,加入木瓜蛋白酶,加酶量20000IU/g蚕蛹蛋白,酶解温度55℃,pH值7.0,酶解时间3h,酶解完成后92℃灭酶13min; (1) Prepare a silkworm chrysalis protein solution with a concentration of 12% with deionized water, add papain, the enzyme amount is 20000IU/g silkworm chrysalis protein, the enzymatic hydrolysis temperature is 55°C, the pH value is 7.0, the enzymatic hydrolysis time is 3h, and the enzymatic hydrolysis is completed at 92°C Inactivate the enzyme for 13 minutes;
(2)第一步酶解完成后,调节酶解液pH至9.0,加入Esperase蛋白酶,加酶量0.15KNPU/g蚕蛹蛋白,酶解3h,酶解温度55℃,酶解完成后92℃灭酶13min; (2) After the first step of enzymatic hydrolysis is completed, adjust the pH of the enzymatic hydrolysis solution to 9.0, add Esperase protease, the amount of enzyme added is 0.15KNPU/g silkworm chrysalis protein, enzymatic hydrolysis for 3 hours, the enzymatic hydrolysis temperature is 55°C, and the enzyme is extinguished at 92°C after the enzymatic hydrolysis is completed. Enzyme 13min;
(3) 灭酶后的物料过滤除去不溶物,得淡黄色澄清透明溶液,此多肽溶液过超微滤膜,收集分子量为3000Da以下的滤液; (3) Filtrate the insoluble matter after deactivating the material to obtain a light yellow clear and transparent solution. The polypeptide solution is passed through an ultra-microfiltration membrane to collect the filtrate with a molecular weight below 3000Da;
(4)所得多肽溶液加入4%活性炭吸附脱色,经大孔树脂DA201-C脱盐处理后,真空浓缩,冷冻干燥获得蚕蛹蛋白多肽干粉,备用; (4) Add 4% activated carbon to the obtained polypeptide solution for adsorption and decolorization, after desalination treatment by macroporous resin DA201-C, vacuum concentration, freeze-drying to obtain silkworm chrysalis protein polypeptide dry powder, set aside;
步骤二: 蚕蛹多肽面膜的制备Step 2: Preparation of silkworm chrysalis polypeptide mask
(1) 将蚕蛹蛋白多肽干粉7份、海藻提取物3份置于容器中,加入20份去离子水,加热至45℃溶解,此混合物为组分一; (1) Put 7 parts of silkworm chrysalis protein peptide dry powder and 3 parts of seaweed extract into a container, add 20 parts of deionized water, heat to 45°C to dissolve, and this mixture is component 1;
(2) 将石榴籽提取物2份、橄榄油 3 份、辛酸癸酸甘油三酯3份、对羟基苯甲酸甲酯0.05份,苯氧乙醇0.05份用乙醇溶解,搅拌均匀,然后加入1份吐温-60,加热至42℃,充分混匀,制得组分二; (2) Dissolve 2 parts of pomegranate seed extract, 3 parts of olive oil, 3 parts of caprylic capric triglyceride, 0.05 part of methyl p-hydroxybenzoate, and 0.05 part of phenoxyethanol in ethanol, stir well, and then add 1 part Tween-60, heated to 42°C, mixed thoroughly to obtain component 2;
(3) 将果胶2份,透明质酸钠2份置于容器中,加入20份去离子水,加入珍珠粉 2份,甘油3份,加热至55℃保温8min,搅拌均匀,此为组分三; (3) Put 2 parts of pectin and 2 parts of sodium hyaluronate in a container, add 20 parts of deionized water, add 2 parts of pearl powder, 3 parts of glycerin, heat to 55 ° C for 8 minutes, stir well, this is the composition divided into three;
(4) 将上述组分一、二、三混合,于70℃搅拌混匀,冷却后加入迷迭香精油2份,混合均匀即得蚕蛹多肽面膜。 (4) Mix the above components 1, 2, and 3, stir and mix at 70°C, add 2 parts of rosemary essential oil after cooling, and mix well to get the silkworm chrysalis polypeptide mask.
对比例1Comparative example 1
与实施例1相比,将蚕蛹蛋白多肽干粉替换为市售蚕蛹蛋白粉,其余同实施例1完全一致,制备面膜。 Compared with Example 1, the silkworm chrysalis protein polypeptide dry powder was replaced with commercially available silkworm chrysalis protein powder, and the rest was exactly the same as Example 1 to prepare a facial mask.
对比例2Comparative example 2
与实施例1相比,未加入迷迭香精油,其余同实施例1完全一致,制备面膜。 Compared with Example 1, rosemary essential oil was not added, and all the others were completely consistent with Example 1 to prepare facial mask.
对比例3Comparative example 3
与实施例1相比,将实施例1制备的蚕蛹蛋白多肽干粉替换为其他方法制备的蚕蛹蛋白多肽,其余同实施例1完全一致,制备面膜。 Compared with Example 1, the silkworm chrysalis protein polypeptide dry powder prepared in Example 1 was replaced with silkworm chrysalis protein polypeptide prepared by other methods, and the rest was exactly the same as in Example 1 to prepare a facial mask.
其他方法制备的蚕蛹蛋白多肽,制备方法同《食品科学》2008,Vol 29,No.11,《蚕蛹蛋白多肽液抗肿瘤作用的实验研究》第588-589页中所记载的方法。 Silkworm chrysalis protein polypeptide prepared by other methods, the preparation method is the same as that recorded in "Food Science" 2008, Vol 29, No.11, "Experimental Research on the Anti-tumor Effect of Silkworm Chrysalis Protein Polypeptide Liquid", pp. 588-589.
人体使用实验研究Experimental research on human use
1、受试对象和使用 1. Subjects and use
女性志愿者80名,年龄23-50岁,随机分成四组,实施例1组20人,对比例1、2、3组各20人,试验期间,试验部位停用任何外用物和/或化妆品,受试者分别将受试样品和对比例1、2、3样品分别涂于面部,每天一次,连涂三天,第四次于第6日开始涂,此后,每周涂两次,每次涂20分钟,20分钟后洗去面膜,连续8周,采用硅橡胶复膜方法复制受试者受试的脸颊及眼角部位的皮肤皱纹,编号,肉眼观察,按照规定的评估标准对皱纹程度改善进行评分,评分小组由2人组成,采用双盲法。 80 female volunteers, aged 23-50 years, were randomly divided into four groups, 20 people in Example 1 group, 20 people in each of Comparative Example 1, 2, and 3 groups. During the test, any external use and/or cosmetics were stopped at the test site , the subject applied the test sample and the samples of comparative examples 1, 2, and 3 to the face, once a day for three consecutive days, and the fourth time began to apply on the 6th day, and then applied twice a week. Apply for 20 minutes each time, wash off the mask after 20 minutes, for 8 consecutive weeks, use the silicone rubber lamination method to replicate the skin wrinkles on the cheeks and corners of the eyes of the subjects, number them, observe with the naked eye, and evaluate the wrinkles according to the prescribed evaluation standards The degree of improvement was scored, and the scoring group was composed of 2 people, and a double-blind method was adopted.
2、实验结果 2. Experimental results
结果如下表所示: The results are shown in the table below:
皱纹深度改善人数为使用前后皱纹抚平的使用者; The number of wrinkle depth improvement is the users whose wrinkles were smoothed before and after use;
皱纹深度改善%=(使用前-使用后皱纹深度)/使用前皱纹深度; Wrinkle depth improvement %= (before use - wrinkle depth after use) / wrinkle depth before use;
抚平的平均有效积分高表明配方对皱纹改善作用明显,小于0为无效。 A high average effective score for smoothing indicates that the formula has an obvious effect on improving wrinkles, and less than 0 means it is ineffective.
实施例1中,面膜涂于皮肤后,面膜稠度合适,取少量面膜在手背上以打圈的方式涂抹,搓泥现象少,使用后皮肤不紧绷,舒适; 对比例1中,面膜涂于皮肤后,面膜稠度合适,取少量面膜在手背上以打圈的方式涂抹,有搓泥现象,使用后皮肤有紧绷的感觉;原因可能是蚕蛹蛋白与蚕蛹蛋白肽相比,其渗透效果与吸收效果要差; 对比例2中涂于皮肤后,面膜稠度合适,取少量面膜在手背上以打圈的方式涂抹,搓泥现象少,使用后皮肤不紧绷,舒适,但面膜稍有淡淡的腥味。 对比例3中,面膜涂于皮肤后,面膜稠度合适,取少量面膜在手背上以打圈的方式涂抹,搓泥现象少,使用后皮肤有紧绷感,说明本对比例使用的其他方法制备的蚕蛹多肽分子量分布范围不够合理,吸收和渗透效果要差于实施例1。 In Example 1, after the mask is applied to the skin, the consistency of the mask is suitable. Take a small amount of the mask and apply it in circles on the back of the hand. There is less mud rubbing, and the skin is not tight and comfortable after use; in Comparative Example 1, the mask is applied on After the skin, the consistency of the mask is suitable. Take a small amount of the mask and apply it in circles on the back of your hand. There is a phenomenon of rubbing mud, and the skin feels tight after use. The reason may be that silkworm chrysalis protein has a better penetration effect than silkworm chrysalis protein peptide. The absorption effect is poor; In Comparative Example 2, after applying to the skin, the mask consistency is suitable. Take a small amount of the mask and apply it in circles on the back of the hand. There is less mud rubbing. fishy smell. In Comparative Example 3, after the mask was applied to the skin, the consistency of the mask was suitable. Take a small amount of the mask and apply it in circular motions on the back of the hand. There was less mud rubbing, and the skin felt tight after use, which shows that other preparation methods used in this comparative example The silkworm chrysalis polypeptide molecular weight distribution range is not reasonable enough, and the absorption and penetration effect is worse than that of Example 1.
从以上的比较中可以看出,本发明中以小分子量蚕蛹多肽为原料制备的面膜,皮肤的吸收效果好,见效明显,有效的改善了面部皮肤的皱纹深度。 From the above comparison, it can be seen that the facial mask prepared from silkworm chrysalis polypeptide with small molecular weight in the present invention has good skin absorption effect and obvious effect, and effectively improves the wrinkle depth of facial skin. the
实施例2Example 2
步骤一:双步酶解制备蚕蛹蛋白多肽Step 1: Two-step enzymatic hydrolysis to prepare silkworm chrysalis protein polypeptide
(1)用去离子水配制浓度10%的蚕蛹蛋白溶液,加入木瓜蛋白酶,加酶量8000IU/g蚕蛹蛋白,酶解温度50℃,pH值7.5,酶解时间4h,酶解完成后95℃灭酶10min; (1) Prepare a silkworm chrysalis protein solution with a concentration of 10% with deionized water, add papain, the enzyme amount is 8000IU/g silkworm chrysalis protein, the enzymatic hydrolysis temperature is 50°C, the pH value is 7.5, the enzymatic hydrolysis time is 4h, and the enzymatic hydrolysis is completed at 95°C Inactivate the enzyme for 10 minutes;
(2)第一步酶解完成后,调节酶解液pH至9.5,加入Esperase蛋白酶,加酶量0.075KNPU/g蚕蛹蛋白,酶解4h,酶解温度50℃,酶解完成后95℃灭酶10min; (2) After the first step of enzymatic hydrolysis is completed, adjust the pH of the enzymatic hydrolysis solution to 9.5, add Esperase protease, the amount of enzyme added is 0.075KNPU/g silkworm chrysalis protein, enzymatic hydrolysis for 4 hours, the enzymatic hydrolysis temperature is 50°C, and the enzyme is extinguished at 95°C after the enzymatic hydrolysis is completed. Enzyme 10min;
(3) 灭酶后的物料过滤除去不溶物,得淡黄色澄清透明溶液,此多肽溶液过超微滤膜,收集分子量为3000Da以下的滤液; (3) Filtrate the insoluble matter after deactivating the material to obtain a light yellow clear and transparent solution. The polypeptide solution is passed through an ultra-microfiltration membrane to collect the filtrate with a molecular weight below 3000Da;
(4)所得多肽溶液加入5%活性炭吸附脱色,经大孔树脂DA201-C脱盐处理后,真空浓缩,冷冻干燥获得蚕蛹蛋白多肽干粉,备用; (4) Add 5% activated carbon to the obtained polypeptide solution for adsorption and decolorization, after desalination treatment by macroporous resin DA201-C, vacuum concentration, freeze-drying to obtain silkworm chrysalis protein polypeptide dry powder, set aside;
步骤二: 蚕蛹多肽面膜的制备Step 2: Preparation of silkworm chrysalis polypeptide mask
(1) 将蚕蛹蛋白多肽干粉10份、海藻提取物3份置于容器中,加入15份去离子水,加热至45℃溶解,此混合物为组分一; (1) Put 10 parts of silkworm chrysalis protein peptide dry powder and 3 parts of seaweed extract into a container, add 15 parts of deionized water, and heat to 45°C to dissolve. This mixture is component 1;
(2) 将石榴籽提取物3份、橄榄油 2 份、辛酸癸酸甘油三酯5份、对羟基苯甲酸乙酯0.05份,苯甲酸0.05份用乙醇溶解,搅拌均匀,然后加入1份吐温-60,加热至42℃,充分混匀,制得组分二; (2) Dissolve 3 parts of pomegranate seed extract, 2 parts of olive oil, 5 parts of caprylic capric triglyceride, 0.05 part of ethyl p-hydroxybenzoate, and 0.05 part of benzoic acid in ethanol, stir well, and then add 1 part of spit Temperature -60, heat to 42°C, mix thoroughly to obtain component 2;
(3) 将汉生胶1份,小麦胚芽氨基丙基氧化胺3份置于容器中,加入15份去离子水溶解,加入珍珠粉 3份,甘油5份,加热至60℃保温10min,搅拌均匀,此为组分三; (3) Put 1 part of xanthan gum and 3 parts of wheat germ aminopropylamine oxide in a container, add 15 parts of deionized water to dissolve, add 3 parts of pearl powder, 5 parts of glycerin, heat to 60 ° C for 10 minutes, stir Uniform, this is component three;
(4) 将上述组分一、二、三混合,于75℃搅拌混匀,冷却后加入迷迭香精油1份,混合均匀即得蚕蛹多肽面膜。 (4) Mix the above components 1, 2, and 3, stir and mix at 75°C, add 1 part of rosemary essential oil after cooling, and mix well to get the silkworm chrysalis polypeptide mask.
实施例3Example 3
步骤一:双步酶解制备蚕蛹蛋白多肽Step 1: Two-step enzymatic hydrolysis to prepare silkworm chrysalis protein polypeptide
(1)用去离子水配制浓度10%的蚕蛹蛋白溶液,加入木瓜蛋白酶,加酶量60000IU/g蚕蛹蛋白,3%,酶解温度45℃,pH值6.5,酶解时间2h,酶解完成后90℃灭酶15min; (1) Prepare a silkworm chrysalis protein solution with a concentration of 10% in deionized water, add papain, the amount of enzyme added is 60000IU/g silkworm chrysalis protein, 3%, the enzymatic hydrolysis temperature is 45°C, the pH value is 6.5, the enzymatic hydrolysis time is 2h, and the enzymatic hydrolysis is completed Then inactivate the enzyme at 90°C for 15 minutes;
(2)第一步酶解完成后,调节酶解液pH至10.0,加入Esperase蛋白酶,加酶量0.225KNPU/g蚕蛹蛋白,酶解4h,酶解温度45℃,酶解完成后90℃灭酶15min; (2) After the first step of enzymatic hydrolysis is completed, adjust the pH of the enzymatic hydrolysis solution to 10.0, add Esperase protease, the amount of enzyme added is 0.225KNPU/g silkworm chrysalis protein, enzymatic hydrolysis for 4 hours, the enzymatic hydrolysis temperature is 45°C, and the enzymatic hydrolysis is extinguished at 90°C Enzyme 15min;
(3) 灭酶后的物料过滤除去不溶物,得淡黄色澄清透明溶液,此多肽溶液过超微滤膜,收集分子量为3000Da以下的滤液; (3) Filtrate the insoluble matter after deactivating the material to obtain a light yellow clear and transparent solution. The polypeptide solution is passed through an ultra-microfiltration membrane to collect the filtrate with a molecular weight below 3000Da;
(4)所得多肽溶液加入3%活性炭吸附脱色,经大孔树脂DA201-C脱盐处理后,真空浓缩,冷冻干燥获得蚕蛹蛋白多肽干粉,备用; (4) Add 3% activated carbon to the obtained polypeptide solution for adsorption and decolorization, after desalination treatment by macroporous resin DA201-C, vacuum concentration, freeze-drying to obtain silkworm chrysalis protein polypeptide dry powder, set aside;
步骤二: 蚕蛹多肽面膜的制备Step 2: Preparation of silkworm chrysalis polypeptide mask
(1) 将蚕蛹蛋白多肽干粉5份、海藻提取物6份置于容器中,加入16份去离子水,加热至50℃溶解,此混合物为组分一; (1) Put 5 parts of silkworm chrysalis protein peptide dry powder and 6 parts of seaweed extract into a container, add 16 parts of deionized water, heat to 50°C to dissolve, and this mixture is component 1;
(2) 将石榴籽提取物1份、橄榄油4 份、辛酸癸酸甘油三酯2份、对羟基苯甲酸丙酯0.05份用乙醇溶解,搅拌均匀,然后加入1份吐温-80,加热至45℃,充分混匀,制得组分二; (2) Dissolve 1 part of pomegranate seed extract, 4 parts of olive oil, 2 parts of caprylic capric triglyceride, and 0.05 part of propyl p-hydroxybenzoate in ethanol, stir well, then add 1 part of Tween-80, heat To 45°C, mix thoroughly to obtain component 2;
(3) 将瓜尔胶2份,阳离子瓜尔胶3份置于容器中,加入16份去离子水溶解,加入珍珠粉 1份,甘油6份,加热至50℃保温5min,搅拌均匀,此为组分三; (3) Put 2 parts of guar gum and 3 parts of cationic guar gum in a container, add 16 parts of deionized water to dissolve, add 1 part of pearl powder, 6 parts of glycerin, heat to 50°C for 5 minutes, stir well, then is component three;
(4) 将上述组分一、二、三混合,于60℃搅拌混匀,冷却后加入迷迭香精油2份,混合均匀即得蚕蛹多肽面膜。 (4) Mix the above components 1, 2, and 3, stir and mix at 60°C, add 2 parts of rosemary essential oil after cooling, and mix well to get the silkworm chrysalis polypeptide mask.
实施例4Example 4
步骤一:双步酶解制备蚕蛹蛋白多肽Step 1: Two-step enzymatic hydrolysis to prepare silkworm chrysalis protein polypeptide
(1)用去离子水配制浓度15%的蚕蛹蛋白溶液,加入木瓜蛋白酶,加酶量30000IU/g蚕蛹蛋白,酶解温度60℃,pH值6.5,酶解时间4h,酶解完成后95℃灭酶10min; (1) Prepare a silkworm chrysalis protein solution with a concentration of 15% in deionized water, add papain, the enzyme amount is 30000IU/g silkworm chrysalis protein, the enzymatic hydrolysis temperature is 60°C, the pH value is 6.5, the enzymatic hydrolysis time is 4h, and the enzymatic hydrolysis is completed at 95°C Inactivate the enzyme for 10 minutes;
(2)第一步酶解完成后,调节酶解液pH至11.0,加入Esperase蛋白酶,加酶量0.2KNPU/g蚕蛹蛋白,酶解4h,酶解温度60℃,酶解完成后95℃灭酶10min; (2) After the first step of enzymatic hydrolysis is completed, adjust the pH of the enzymatic hydrolysis solution to 11.0, add Esperase protease, the amount of enzyme added is 0.2KNPU/g silkworm chrysalis protein, enzymatic hydrolysis for 4 hours, the enzymatic hydrolysis temperature is 60°C, and the enzymatic hydrolysis is extinguished at 95°C Enzyme 10min;
(3) 灭酶后的物料过滤除去不溶物,得淡黄色澄清透明溶液,此多肽溶液过超微滤膜,收集分子量为3000Da以下的滤液; (3) Filtrate the insoluble matter after deactivating the material to obtain a light yellow clear and transparent solution. The polypeptide solution is passed through an ultra-microfiltration membrane to collect the filtrate with a molecular weight below 3000Da;
(4)所得多肽溶液加入5%活性炭吸附脱色,经大孔树脂DA201-C脱盐处理后,真空浓缩,冷冻干燥获得蚕蛹蛋白多肽干粉,备用; (4) Add 5% activated carbon to the obtained polypeptide solution for adsorption and decolorization, after desalination treatment by macroporous resin DA201-C, vacuum concentration, freeze-drying to obtain silkworm chrysalis protein polypeptide dry powder, set aside;
步骤二: 蚕蛹多肽面膜的制备Step 2: Preparation of silkworm chrysalis polypeptide mask
(1) 将蚕蛹蛋白多肽干粉10份、海藻提取物6份置于容器中,加入去离子水17份,加热至50℃溶解,此混合物为组分一; (1) Put 10 parts of silkworm chrysalis protein peptide dry powder and 6 parts of seaweed extract into a container, add 17 parts of deionized water, heat to 50°C to dissolve, and this mixture is component 1;
(2) 将石榴籽提取物3份、橄榄油 4 份、辛酸癸酸甘油三酯5份、对羟基苯甲酸乙酯0.05份,羟基苯甲酸丙酯0.05份用乙醇溶解,搅拌均匀,然后加入1份吐温-60,加热至42℃,充分混匀,制得组分二; (2) Dissolve 3 parts of pomegranate seed extract, 4 parts of olive oil, 5 parts of caprylic capric triglyceride, 0.05 part of ethyl p-hydroxybenzoate, and 0.05 part of propyl paraben in ethanol, stir well, and then add 1 part of Tween-60, heated to 42°C, mixed thoroughly to obtain component 2;
(3) 将羧甲基纤维素3份,大豆氨基丙基氧化胺3份置于容器中,加入17份去离子水溶解,加入珍珠粉 3份,甘油5份,加热至60℃保温10min,搅拌均匀,此为组分三; (3) Put 3 parts of carboxymethyl cellulose and 3 parts of soybean aminopropylamine oxide in a container, add 17 parts of deionized water to dissolve, add 3 parts of pearl powder, 5 parts of glycerin, heat to 60 ° C for 10 minutes, Stir evenly, this is component three;
(4) 将上述组分一、二、三混合,于75℃搅拌混匀,冷却后加入迷迭香精油2份,混合均匀即得蚕蛹多肽面膜。 (4) Mix the above components 1, 2, and 3, stir and mix at 75°C, add 2 parts of rosemary essential oil after cooling, and mix well to get the silkworm chrysalis polypeptide mask.
实施例5Example 5
步骤一:双步酶解制备蚕蛹蛋白多肽Step 1: Two-step enzymatic hydrolysis to prepare silkworm chrysalis protein polypeptide
(1)用去离子水配制浓度15%的蚕蛹蛋白溶液,加入木瓜蛋白酶,加酶量45000IU/g蚕蛹蛋白,酶解温度60℃,pH值6.5,酶解时间4h,酶解完成后95℃灭酶10min; (1) Prepare a silkworm chrysalis protein solution with a concentration of 15% in deionized water, add papain, the enzyme amount is 45000IU/g silkworm chrysalis protein, the enzymatic hydrolysis temperature is 60°C, the pH value is 6.5, the enzymatic hydrolysis time is 4h, and the enzymatic hydrolysis is completed at 95°C Inactivate the enzyme for 10 minutes;
(2)第一步酶解完成后,调节酶解液pH至11.0,加入Esperase蛋白酶,加酶量0.125KNPU/g蚕蛹蛋白,酶解4h,酶解温度60℃,酶解完成后95℃灭酶10min; (2) After the first step of enzymatic hydrolysis is completed, adjust the pH of the enzymatic hydrolysis solution to 11.0, add Esperase protease, the amount of enzyme added is 0.125KNPU/g silkworm chrysalis protein, enzymatic hydrolysis for 4 hours, the enzymatic hydrolysis temperature is 60°C, and the enzyme is extinguished at 95°C after the enzymatic hydrolysis is completed. Enzyme 10min;
(3) 灭酶后的物料过滤除去不溶物,得淡黄色澄清透明溶液,此多肽溶液过超微滤膜,收集分子量为3000Da以下的滤液; (3) Filtrate the insoluble matter after deactivating the material to obtain a light yellow clear and transparent solution. The polypeptide solution is passed through an ultra-microfiltration membrane to collect the filtrate with a molecular weight below 3000Da;
(4)所得多肽溶液加入5%活性炭吸附脱色,经大孔树脂DA201-C脱盐处理后,真空浓缩,冷冻干燥获得蚕蛹蛋白多肽干粉,备用; (4) Add 5% activated carbon to the obtained polypeptide solution for adsorption and decolorization, after desalination treatment by macroporous resin DA201-C, vacuum concentration, freeze-drying to obtain silkworm chrysalis protein polypeptide dry powder, set aside;
步骤二: 蚕蛹多肽面膜的制备Step 2: Preparation of silkworm chrysalis polypeptide mask
(1) 将蚕蛹蛋白多肽干粉8份、海藻提取物5份置于容器中,加入去离子水15份,加热至45℃溶解,此混合物为组分一; (1) Put 8 parts of silkworm chrysalis protein peptide dry powder and 5 parts of seaweed extract into a container, add 15 parts of deionized water, heat to 45°C to dissolve, and this mixture is component 1;
(2) 将石榴籽提取物3份、橄榄油 4 份、辛酸癸酸甘油三酯3份、对羟基苯甲酸甲酯0.05份用乙醇溶解,搅拌均匀,然后加入1份吐温-20,1份吐温-60,加热至45℃,充分混匀,制得组分二; (2) Dissolve 3 parts of pomegranate seed extract, 4 parts of olive oil, 3 parts of caprylic capric triglyceride, and 0.05 part of methyl p-hydroxybenzoate in ethanol, stir well, then add 1 part of Tween-20, 1 One part of Tween-60, heated to 45°C, and thoroughly mixed to obtain component 2;
(3) 将十六烷基乙氧基(20)衣康酸酯共聚物3份置于容器中,加入15份去离子水溶解,加入珍珠粉 3份,甘油3份,加热至60℃保温10min,搅拌均匀,此为组分三; (3) Put 3 parts of hexadecyl ethoxy (20) itaconate copolymer in a container, add 15 parts of deionized water to dissolve, add 3 parts of pearl powder, 3 parts of glycerin, heat to 60°C and keep warm 10min, stir evenly, this is component 3;
(4) 将上述组分一、二、三混合,于75℃搅拌混匀,冷却后加入迷迭香精油2份,混合均匀即得蚕蛹多肽面膜。 (4) Mix the above components 1, 2, and 3, stir and mix at 75°C, add 2 parts of rosemary essential oil after cooling, and mix well to get the silkworm chrysalis polypeptide mask.
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CN106902004A (en) * | 2015-12-22 | 2017-06-30 | 江南大学 | Preservative free preserving moisture and protecting skin emulsion formulations |
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CN108324663A (en) * | 2018-03-23 | 2018-07-27 | 杨巧 | A kind of white orchid silkworm chrysalis facial mask and preparation method thereof |
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CN108478454A (en) * | 2018-03-23 | 2018-09-04 | 杨巧 | A kind of cordate telosma silkworm chrysalis facial mask and preparation method thereof |
CN108524409A (en) * | 2018-03-23 | 2018-09-14 | 杨巧 | A kind of sweet osmanthus silkworm chrysalis facial mask and preparation method thereof |
CN108524410A (en) * | 2018-03-23 | 2018-09-14 | 杨巧 | A kind of Jasmine silkworm chrysalis facial mask and preparation method thereof |
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