CN114983914A - 一种美白护肤品的制备方法 - Google Patents
一种美白护肤品的制备方法 Download PDFInfo
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- CN114983914A CN114983914A CN202210713645.4A CN202210713645A CN114983914A CN 114983914 A CN114983914 A CN 114983914A CN 202210713645 A CN202210713645 A CN 202210713645A CN 114983914 A CN114983914 A CN 114983914A
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Abstract
本发明公开了一种美白护肤品的制备方法,该美白护肤品由以下原料组成:去离子水、甘油、烟酰胺、苹果酸、蜂蜜、霍霍巴油、合成角鲨烷、水溶性神经酰胺、维生素E、黄原胶、乙二胺四乙酸二钠、防腐剂、氢化卵磷脂、中药精华提取物、紫外吸收剂,所述中药精华提取物由川芎、甘草、白茯苓、木芙蓉叶以及益母草制得,所述紫外吸收剂为纳米纤维素改性阿魏酸和改性鞣花酸的混合。本发明制备的美白护肤品通过作用于黑色素生成和转移的各个阶段,达到了更好的美白效果,同时将修复,补水,锁水,防晒功能集为一体,能达到长效保湿的目的。
Description
技术领域
本发明涉及化妆品技术领域,尤其涉及一种美白护肤品的制备方法。
背景技术
随着人们生活水平的提高,越来越多的人开始追求幸福和美丽。白皙红润,细腻光滑的皮肤一直是亚洲女性所追求的,美白也一直是化妆品市场的主旋律,因此,在亚洲地区,美白行业具有很大的发展空间。对于一直致力于美白化妆品原料开发的科研人员来说,美白原料的开发是机遇与挑战并存。目前市面上销售的美白化妆品近千种,由于科技水平的限制,许多美白产品的安全性,只有经过长期、广泛的使用才能逐渐被确定,美白产品在给我们带来美的同时,也可能带来许多不安全的隐患。因此,绿色、安全的纯天然植物美白添加剂成为近年来的研究热点。
开发美白剂应建立在对美白机理的深入了解的基础上,而通过抑制皮肤黑色素是美白作用机理的中心。黑色素是酚性物质的酶在氧化过程中形成的高分子色素的总称,存在于所有生物中。人体黑色素为碱性难溶性黑色色素(优黑色素)和碱性易溶性的黄色素(褐黑色素)的复合体。在黑色素形成的过程中,其最初反应被称为黑色素合成的速率控制阶段,而酪氨酸酶是其主要限速酶,因此,通过抑制酪氨酸酶活性,可以减少黑色素的形成而达到美白的功效。
在黑色素的形成过程中,可以通过几种方法达到美白的作用,①抑制酪氨酸酶活性;②螯合铜离子;③清除氧自由基;④加速表皮代谢;⑤抑制黑色素转移。
护肤品保湿的核心原理是:①修复屏障,修复屏障有利于维持角质层水分;②利用吸湿剂,吸湿剂发挥作用需要环境湿度在70%以上,否则反而会从真皮吸水,故一般会在最外层配合封闭剂使用;③利用润肤剂,主要作用是填充胶质细胞间的缝隙,让皮肤更光滑;④利用封闭剂,主要作用是阻止或延缓水分蒸发。
以上为美白保湿的内源机制,但是影响黑色素形成的原因还包括外源因素,如在紫外线的作用下,细胞受到紫外线的刺激,肌肤角质细胞会自然分泌内皮素,会导致黑色素细胞增殖,酪氨酸酶活性增加,促使黑色素生成,同时由于其光热效应也会导致水分的流失以及皮肤细胞的萎缩,是导致色斑、黑色素的主要元凶之一。然而在现有技术中的美白护肤品基本都没考虑过这方面的影响,因此均需要额外使用防晒剂。
专利CN105287341B公开了一种美白保湿精华液及其制备方法,该美白保湿精华液包括以下重量份数的原料:增稠剂0.2~0.5份、多元醇3~12份、中药提取物15~35份、蜂蜜1~2份、珍珠粉0.3~2份、香精0.1~0.3份、水40~70份,所述中药提取物的制备原料包括杜仲、天门冬、薏米以及蓝莓果。其中主要的有效成分是中药提取物、蜂蜜以及珍珠粉,主要是通过清除氧自由基来达到美白的效果,通过蜂蜜的吸湿效果达到保湿的效果,具有一定的美白保湿效果,但是效果有限,有待进一步加强,同时紫外线也是黑色素增加的主要外源因素,该专利并未从这方面进行防护,需要额外使用防晒剂。
专利CN113208968A公开了一种美白保湿精华液及其制备方法,该美白保湿精华液由以下原料组成:甘油、1,3-丙二醇、去离子水、γ-聚谷氨酸、卡波姆、水溶性富勒烯、抗坏血酸葡糖苷、对羟基苯乙酮、甘草酸二钾、透明质酸钠、1,2-戊二醇、烟酰胺、植物精华提取物、皮肤调理剂。其添加了多种保湿剂来达到保湿的效果,同时也添加了多种美白成分,但是其增加皮肤的水合度不够,渗透性较差,不易吸收,且美白保湿效果并不显著,同时对光线照射无保护作用。
发明内容
针对现有技术中存在的上述不足,本发明所要解决的技术问题是提供一种渗透性好,肌肤吸收率高,能美白肌肤改善肌肤状态,并能具有长时间保湿的同时能够防紫外线的美白护肤品。
为了实现上述的发明目的,本发明是通过如下技术方案实现的:
一种美白护肤品,由以下原料组成:水、甘油、烟酰胺、苹果酸、蜂蜜、霍霍巴油、合成角鲨烷、水溶性神经酰胺、维生素E、黄原胶、乙二胺四乙酸二钠、防腐剂、氢化卵磷脂、中药精华提取物、紫外吸收剂。
本发明中采用多种有效成分协同作用达到美白保湿的效果,所述烟酰胺是维生素家族中的一员,具体来说是烟酸(微生物B3)的酰胺,其分子较小且有一定脂溶性,容易穿过角质层被细胞吸收,其除了能抑制黑素小体向角质细胞移动这种防御性美白措施以外,烟酰胺还可以加快已经含有黑色素的角质细胞脱落从而达到美白的效果。
苹果酸是一种有机酸,其可以通过加速角质细胞的代谢来达到美白的目的。维生素E是一种脂溶性的维生素,容易通过角质层被细胞吸收,其可以不可逆的还原黑色素,同时通过清除自由基来抑制黑色素的合成达到美白的效果。乙二胺四乙酸二钠是一种螯合剂,其可以通过螯合酪氨酸酶中的金属离子,通过使酪氨酸酶失去催化活性,从而阻断黑色素的合成途径达到美白效果。
氢化卵磷脂使卵磷脂的部分水解物,氢化卵磷脂提高了它的亲水能力,有着一定的保湿效果,可以被人的皮肤吸收并能促进其他营养物质的渗透,加强护肤品中有效成分的作用效果,并且其乳化性能强,能稳定乳状液,同时具有一定的抗氧化功能,保证护肤品中的有效成分不因氧化而失效。
水溶性神经酰胺有别于其他的神经酰胺,其他的不是水溶的,只是增强皮肤屏障功能的一种油脂,其具有更强的渗透作用,神经氨酸使角质层脂质的主要成分,在角质层脂质中占到的比例达到40~50%,其可以加强网状结构来锁住角质层的水分,同时修复角质层屏障,达到长效保湿的目的。蜂蜜是一种天然的吸湿剂,可以吸收空气中的水分达到保湿的效果。霍霍巴油是从霍霍巴所结种子中提取得到的油,具有良好的渗透性,这是因为霍霍巴油的化学分子排列和人类的皮脂十分类似,极容易被皮肤类化和吸收,同时含有丰富的维生素D及蛋白质,是很好的滋润及保湿油,可增加皮肤水分,预防皱纹和老化。合成角鲨烷是有异戊二烯合成的,具有和角鲨烷类似的性质,角鲨烷是最为接近人体皮脂的一种脂类,亲和力强,能够和人体自身的皮脂膜融为一体,在皮肤表面形成一层天然的屏障,还能抑制皮肤脂质的过氧化,能够有效渗透入肌肤,并促进皮肤基底细胞的增值,对延缓皮肤老化有显著效果,能够起到长效的封闭保湿效果。
黄原胶是由野油菜黄单胞杆菌(Xanthomnas campestris)以碳水化合物为主要原料(如玉米淀粉)经发酵工程生产的一种作用广泛的微生物胞外多糖,是目前国际上集增稠、悬浮、乳化、稳定于一体,性能最优越的生物胶,能够有效的提升护肤品的稳定性和使用质感。
优选的,所述防腐剂为苯甲酸钠或山梨酸钾。
优选的,所述中药精华提取物的制备原料由川芎、甘草、白茯苓、木芙蓉叶、益母草按照(2~6):(1~3):(2~6):(2~6):(2~6)的质量比提取得到。
优选的,所述中药精华提取物由以下步骤制得:
S1将中药精华提取物的制备原料按比例混合,用粉碎机粉碎,过30~40目筛,得到粉碎后的原料密封在塑料袋中,放在阴凉干燥处备用;
S2将粉碎后的原料与水按用量比1g:(8~12)mL充分混合得到混合液1,混合液1在10~25℃下超声提取20~30min,超声功率为250~400W,超声频率为20~40kHz;提取完成后将混合液1过滤,滤渣重复上述操作2~3次,收集最后一次过滤的滤渣,合并每次过滤得到的滤液为水提液备用;
S3将步骤S2中最后一次过滤的滤渣与体积分数为70~75%的乙醇水溶液按用量比1g:(8~12)mL充分混合得到混合液2,混合液2在10~25℃下超声提取20~30min,超声功率为250~300W,超声频率为20~40kHz;提取完成后将混合液2过滤,滤渣重复上述操作2~3次,合并每次过滤得到的滤液为醇提液备用;
S4将步骤S2和S3得到的水提液和醇提液合并得到提取液;将提取液减压浓缩至原滤液体积的1/6~1/4得到浓缩滤液;
S5将步骤S4得到的浓缩滤液在-40~-45℃下冷冻干燥24~48h即得到中药精华提取物。
川芎为伞形科藁本属植物川芎Ligusticum chuanxiong的干燥根茎,始载于《神农本草经》,是常用的中草药。传统中医学认为川芎具有美白功效,古代已有使用川芎美白的记录。《古今医鉴》用川芎、旱墨莲、当归、牙皂、白芷等每早擦牙,有固齿乌须之效。《圣济总录》用川芎、白芷、甘草、桂枝(去粗皮)、杜蘅等日服,三十日体皆香。《广济方》用单味川芎,水煎含之,香口除臭。从以上的本草记载可以看出,川芎在古代就用于美齿、美发、香口香身。
甘草为双子叶植物豆科Leguminosae甘草Glycyrrhiza uralensis的根及根茎。古代中医学记载甘草有着补脾益气,清热解毒,祛痰止咳,缓急止痛,调和诸药的作用。
白茯苓为多孔菌科真菌茯苓Poria cocos的干燥菌核内部白色致密的部分,古人称茯苓为“四时神药”,因为它功效非常广泛,不分四季,将它与各种药物配伍,不管寒、温、风、湿诸疾,都能发挥其独特功效。
木芙蓉叶为锦葵科植物木芙蓉Hibiscus mutabilis的叶片,具有凉血,解毒,消肿,止痛。治痈疽焮肿,缠身蛇丹,烫伤,目赤肿痛,跌打损伤。《本草纲目》记载有清肺凉血,散热解毒。治一切大小痈疽肿毒恶疮,消肿排脓止痛。
益母草为唇形科植物益母草Leonurus japonicus的新鲜或干燥地上部分。具有活血、法瘀、调经、消水的功效。治疗妇女月经不调,胎漏难产,胞衣不下,产后血晕,瘀血腹痛,崩中漏下,尿血、泻血,痈肿疮疡。
优选的,所述紫外吸收剂为阿魏酸、纳米纤维素改性阿魏酸、鞣花酸、改性鞣花酸中的一种或两种及两种以上的混合。
所述纳米纤维素改性阿魏酸的制备方法包括以下步骤:
M1将1~4g阿魏酸、0.1~0.5g 1-乙基-(3-二甲基氨基丙基)碳酰二亚胺(EDC)、0.01~0.05g N-羟基丁二酰亚胺(NHS)加入到100~200mL水中,超声分散15~30min,在30~50℃下反应2~5h,反应结束后即得到羧基活化的阿魏酸水溶液;
M2向步骤M1得到的羧基活化的阿魏酸水溶液中加入2~5g纳米纤维素,超声分散10~20min,在30~50℃下反应3~6h,反应结束后离心10~20min,倒掉上清液,即得到产物,将产物先用水洗2~3次,再用乙醇洗2~3次,将最后一次洗涤得到的产物在40~60℃下真空干燥即得到纳米纤维素改性阿魏酸。
所述改性鞣花酸的制备方法为:将10~20g羟丙基-β-环糊精溶解在25~50mL水中得到羟丙基-β-环糊精溶液,另将5~10g鞣花酸分散在20~30mL无水乙醇中得到鞣花酸乙醇溶液,将其加入到羟丙基-β-环糊精溶液中,超声处理20~30min,再在20~30℃下搅拌12~20h,反应结束后将反应液在60~80℃下干燥12~24h得到改性鞣花酸。
进一步优选的,所述紫外吸收剂为质量比为1~3:1~3的纳米纤维素改性阿魏酸和改性鞣花酸的混合。
阿魏酸是广泛存在于植物界中的一种酚酸,具有超强的抗氧化能力、清除自由基作用以及紫外吸收能力,由此有着美白、祛斑以及防晒效果,但是其在水中溶解性较差,导致阿魏酸不易被吸收,因此在水基护肤品的使用受到限制。本发明使用的纳米纤维素改性阿魏酸,由于纳米纤维素优秀的水分散性,使阿魏酸在水中具有良好的分散性,使其更加稳定的存在于护肤品中,与此同时,由于纳米纤维素良好的生物相容性以及亲水性,使得阿魏酸更易被皮肤吸收从而发挥作用,阿魏酸除了具有较好紫外吸收能力外,还具有抑制黑素细胞和酪氨酸酶活性的效果。
阿魏酸对波段为UVA和UVB的紫外线吸收较好,但是对波段为UVC的紫外线吸收能力较差,为了赋予护肤品防全波段紫外线的能力,本发明还加入了鞣花酸,鞣花酸是一种多酚二内酯,是没食子酸的二聚衍生物,具有很强的紫外吸收能力,同时也具有美白抗氧化的功效,但是其几乎不溶于水,影响了其应用。本发明将鞣花酸用羟丙基-β-环糊精进行包合,极大的提高了其水溶性、理化稳定性以及生物利用度,使其更易被皮肤吸收,与添加的纳米纤维素改性阿魏酸进行协同作用,达到全波段紫外吸收的效果;两者复配除了增加了紫外吸收能力外,纳米纤维素改性阿魏酸还能增强鞣花酸的抗氧化美白效果,并且提高了其在体系中的化学稳定性,达到更好的美白效果。
优选的,一种美白护肤品,由以下重量份原料组成:60~75份水、4~10份甘油、1~2份烟酰胺、0.1~1份苹果酸、1~2份蜂蜜、2~6份霍霍巴油、1~4份合成角鲨烷、2~6份水溶性神经酰胺、0.5~2份维生素E、0.1~0.5份黄原胶、0.1~0.5份乙二胺四乙酸二钠、0.1~0.5份防腐剂、2~5份氢化卵磷脂、5~10份中药精华提取物、1~3份紫外吸收剂。
本发明还提供了所述美白护肤品的制备方法,包括以下步骤:
N1将水、苹果酸、蜂蜜、黄原胶、乙二胺四乙酸二钠、防腐剂、氢化卵磷脂加入搅拌器中,在50~70℃下,搅拌25~40min,得到混合物A;
N2将甘油、烟酰胺、霍霍巴油、合成角鲨烷、水溶液神经酰胺、维生素E、紫外吸收剂加入搅拌器中,在50~70℃下,搅拌25~40min,得到混合物B;
N3将混合物A和混合物B放入乳化均质装置中,均质15~30s,冷却后,再向其中加入中药精华提取物,搅拌10~20min,得到乳化物C;
N4将乳化物C放入超高压均质机中,在压力为150~200MPa,均质3~5min,得到美白护肤品。
与现有技术相比,本发明的有益效果:
1、本发明通过作用于黑色素生成和转移的各个阶段,达到了更好的美白效果,同时将修复、补水、锁水、防晒功能集为一体,能达到长效保湿的目的。
2、本发明中添加多种中药的精华提取物,通过其中的各种活性成分与其他各种添加剂协同增效,进一步增强护肤品的美白保湿效果,同时本发明中药精华提取物采用低温超声萃取的方法,避免在提取过程中有效成分的损失,从而取得更好的效果。
3、本发明制备的纳米纤维素改性阿魏酸和改性鞣花酸,提高了阿魏酸和鞣花酸在护肤品中的分散性、理化稳定性以及生物利用度,同时两者的协同作用得到了防全波段紫外线的能力,阿魏酸也是护肤品中鞣花酸、维生素E以及中药精华提取物中抗氧化美白成分的活性助剂,通过协同作用达到更好的美白保湿效果。
具体实施方式
本发明实施例中部分物质和仪器的具体参数如下:
川芎:伞形科植物川芎Ligusticum chuanxiong的干燥根茎,味辛、温,归肝、胆、心包经,主要功能为活血行气,祛风止痛,产地四川。
甘草:双子叶植物豆科Leguminosae甘草Glycyrrhiza uralensis的根及根茎。味甘,归胃、肺、脾经,主要功能为补脾益气,清热解毒,祛痰止咳,缓急止痛,调和诸药,产地甘肃。
白茯苓:多孔菌科真菌茯苓Poria coco的干燥菌核内部白色致密的部分,味淡、平,归心、脾、肺、肾经,主要功能为渗湿利水,健脾和胃,宁心安神,产地湖北。
木芙蓉叶:锦葵科植物木芙蓉Hibiscus mutabilis的叶片,味辛、平,归肺、肝经,主要功能为凉血,解毒,消肿,止痛,产地湖北。
益母草:唇形科植物益母草Leonurus japonicus的新鲜或干燥地上部分,味幸、苦,归肝、心包经,具有活血、法瘀、调经、消水的功效,产地甘肃。
纳米纤维素,宽10~50nm,长0.5~3μm,购自于武汉华翔科洁生物技术有限公司。
阿魏酸,纯度≥98%,购自于上海源叶生物科技有限公司。
鞣花酸,纯度≥96%,购自于上海源叶生物科技有限公司。
实施例1
一种美白护肤品的制备方法,包括以下步骤:
N1将75份去离子水、0.5份苹果酸、2份蜂蜜、0.4黄原胶、0.2份乙二胺四乙酸二钠、0.2份山梨酸钾、4份氢化卵磷脂加入放入搅拌器中,在60℃下,搅拌30min,得到混合物A;
N2将8份甘油、2份烟酰胺、5份霍霍巴油、3份合成角鲨烷、5份水溶液神经酰胺、1份维生素E、3份紫外吸收剂加入放入搅拌器中,在60℃下,搅拌30min,得到混合物B;
N3将混合物A和混合物B放入乳化均质装置中,用均质15s,冷却后,再向其中加入8份中药精华提取物,搅拌15min,得到乳化物C;
N4将乳化物C放入超高压均质机中,在压力为180Mpa,均质4min,得到美白护肤品。
所述中药精华提取物由以下步骤制得:
S1将川芎、甘草、白茯苓、木芙蓉叶以及益母草按照2:1:1.5:2:2的质量比混合,用粉碎机粉碎,过40目筛,得到粉碎后的原料密封在塑料袋中,放在阴凉干燥处备用;
S2将粉碎后的原料与水按用量比1g:10mL充分混合得到混合液1,混合液1在15℃下超声提取30min,超声功率为300W,超声频率为20kHz;提取完成后将混合液1过滤,滤渣重复上述操作3次,收集最后一次过滤的滤渣,合并每次过滤得到的滤液为水提液备用;
S3将所述步骤S2中最后一次过滤的滤渣与体积分数为75%的乙醇水溶液按用量比1g:10mL充分混合得到混合液2,混合液2在15℃下超声提取30min,超声功率为300W,超声频率为20kHz;提取完成后将混合液2过滤,滤渣重复上述操作3次,合并每次过滤得到的滤液为醇提液备用;
S4将所述步骤S2和S3得到的水提液和醇提液合并得到提取液;将提取液减压浓缩至原滤液体积的1/6得到浓缩滤液;
S5将所述步骤S4得到的浓缩滤液在-45℃下冷冻干燥48h即得到中药精华提取物;
所述紫外吸收剂为质量比为3:1的纳米纤维素改性阿魏酸和改性鞣花酸的混合;
所述纳米纤维素改性阿魏酸的制备方法包括以下步骤:
M1将2g阿魏酸、0.6g 1-乙基-(3-二甲基氨基丙基)碳酰二亚胺、0.02g N-羟基丁二酰亚胺加入到150mL水中,超声分散15min,在40℃下反应5h,反应结束后即得到羧基活化的阿魏酸水溶液;
M2向步骤M1得到的羧基活化的阿魏酸水溶液中加入4g纳米纤维素,超声分散20min,在4℃下反应6h,反应结束后离心20min,倒掉上清液,即得到产物,将产物先用水洗3次,再用乙醇洗3次,将最后一次洗涤得到的产物在40℃下真空干燥即得到纳米纤维素改性阿魏酸;
所述改性鞣花酸的制备方法为:将16g羟丙基-β-环糊精溶解在50mL水中得到羟丙基-β-环糊精溶液,另将8g鞣花酸分散在30mL无水乙醇中得到鞣花酸乙醇溶液,将其加入到羟丙基-β-环糊精溶液中,超声处理30min,再在25℃下搅拌16h,反应结束后将反应液在60℃下干燥24h得到改性鞣花酸。
实施例2
一种美白护肤品的制备方法,包括以下步骤:
N1将75份去离子水、0.5份苹果酸、2份蜂蜜、0.4黄原胶、0.2份乙二胺四乙酸二钠、0.2份山梨酸钾、4份氢化卵磷脂加入放入搅拌器中,在60℃下,搅拌30min,得到混合物A;
N2将8份甘油、2份烟酰胺、5份霍霍巴油、3份合成角鲨烷、5份水溶液神经酰胺、1份维生素E、3份紫外吸收剂加入放入搅拌器中,在60℃下,搅拌30min,得到混合物B;
N3将混合物A和混合物B放入乳化均质装置中,用均质15s,冷却后,再向其中加入8份中药精华提取物,搅拌15min,得到乳化物C;
N4将乳化物C放入超高压均质机中,在压力为180Mpa,均质4min,得到美白护肤品。
所述中药精华提取物由以下步骤制得:
S1将川芎、甘草、白茯苓、木芙蓉叶以及益母草按照2:1:1.5:2:2的质量比混合,用粉碎机粉碎,过40目筛,得到粉碎后的原料密封在塑料袋中,放在阴凉干燥处备用;
S2将粉碎后的原料与水按用量比1g:10mL充分混合得到混合液1,混合液1在15℃下超声提取30min,超声功率为300W,超声频率为20kHz;提取完成后将混合液1过滤,滤渣重复上述操作3次,收集最后一次过滤的滤渣,合并每次过滤得到的滤液为水提液备用;
S3将所述步骤S2中最后一次过滤的滤渣与体积分数为75%的乙醇水溶液按用量比1g:10mL充分混合得到混合液2,混合液2在15℃下超声提取30min,超声功率为300W,超声频率为20kHz;提取完成后将混合液2过滤,滤渣重复上述操作3次,合并每次过滤得到的滤液为醇提液备用;
S4将所述步骤S2和S3得到的水提液和醇提液合并得到提取液;将提取液减压浓缩至原滤液体积的1/6得到浓缩滤液;
S5将所述步骤S4得到的浓缩滤液在-45℃下冷冻干燥48h即得到中药精华提取物;
所述紫外吸收剂为阿魏酸。
实施例3
一种美白护肤品的制备方法,包括以下步骤:
N1将75份去离子水、0.5份苹果酸、2份蜂蜜、0.4黄原胶、0.2份乙二胺四乙酸二钠、0.2份山梨酸钾、4份氢化卵磷脂加入放入搅拌器中,在60℃下,搅拌30min,得到混合物A;
N2将8份甘油、2份烟酰胺、5份霍霍巴油、3份合成角鲨烷、5份水溶液神经酰胺、1份维生素E、3份紫外吸收剂加入放入搅拌器中,在60℃下,搅拌30min,得到混合物B;
N3将混合物A和混合物B放入乳化均质装置中,用均质15s,冷却后,再向其中加入8份中药精华提取物,搅拌15min,得到乳化物C;
N4将乳化物C放入超高压均质机中,在压力为180Mpa,均质4min,得到美白护肤品。
所述中药精华提取物由以下步骤制得:
S1将川芎、甘草、白茯苓、木芙蓉叶以及益母草按照2:1:1.5:2:2的质量比混合,用粉碎机粉碎,过40目筛,得到粉碎后的原料密封在塑料袋中,放在阴凉干燥处备用;
S2将粉碎后的原料与水按用量比1g:10mL充分混合得到混合液1,混合液1在15℃下超声提取30min,超声功率为300W,超声频率为20kHz;提取完成后将混合液1过滤,滤渣重复上述操作3次,收集最后一次过滤的滤渣,合并每次过滤得到的滤液为水提液备用;
S3将所述步骤S2中最后一次过滤的滤渣与体积分数为75%的乙醇水溶液按用量比1g:10mL充分混合得到混合液2,混合液2在15℃下超声提取30min,超声功率为300W,超声频率为20kHz;提取完成后将混合液2过滤,滤渣重复上述操作3次,合并每次过滤得到的滤液为醇提液备用;
S4将所述步骤S2和S3得到的水提液和醇提液合并得到提取液;将提取液减压浓缩至原滤液体积的1/6得到浓缩滤液;
S5将所述步骤S4得到的浓缩滤液在-45℃下冷冻干燥48h即得到中药精华提取物;
所述紫外吸收剂为纳米纤维素改性阿魏酸;
所述纳米纤维素改性阿魏酸的制备方法包括以下步骤:
M1将2g阿魏酸、0.6g 1-乙基-(3-二甲基氨基丙基)碳酰二亚胺、0.02g N-羟基丁二酰亚胺加入到150mL水中,超声分散15min,在40℃下反应5h,反应结束后即得到羧基活化的阿魏酸水溶液;
M2向步骤M1得到的羧基活化的阿魏酸水溶液中加入4g纳米纤维素,超声分散20min,在4℃下反应6h,反应结束后离心20min,倒掉上清液,即得到产物,将产物先用水洗3次,再用乙醇洗3次,将最后一次洗涤得到的产物在40℃下真空干燥即得到纳米纤维素改性阿魏酸。
实施例4
一种美白护肤品的制备方法,包括以下步骤:
N1将75份去离子水、0.5份苹果酸、2份蜂蜜、0.4黄原胶、0.2份乙二胺四乙酸二钠、0.2份山梨酸钾、4份氢化卵磷脂加入放入搅拌器中,在60℃下,搅拌30min,得到混合物A;
N2将8份甘油、2份烟酰胺、5份霍霍巴油、3份合成角鲨烷、5份水溶液神经酰胺、1份维生素E、3份紫外吸收剂加入放入搅拌器中,在60℃下,搅拌30min,得到混合物B;
N3将混合物A和混合物B放入乳化均质装置中,用均质15s,冷却后,再向其中加入8份中药精华提取物,搅拌15min,得到乳化物C;
N4将乳化物C放入超高压均质机中,在压力为180Mpa,均质4min,得到美白护肤品。
所述中药精华提取物由以下步骤制得:
S1将川芎、甘草、白茯苓、木芙蓉叶以及益母草按照2:1:1.5:2:2的质量比混合,用粉碎机粉碎,过40目筛,得到粉碎后的原料密封在塑料袋中,放在阴凉干燥处备用;
S2将粉碎后的原料与水按用量比1g:10mL充分混合得到混合液1,混合液1在15℃下超声提取30min,超声功率为300W,超声频率为20kHz;提取完成后将混合液1过滤,滤渣重复上述操作3次,收集最后一次过滤的滤渣,合并每次过滤得到的滤液为水提液备用;
S3将所述步骤S2中最后一次过滤的滤渣与体积分数为75%的乙醇水溶液按用量比1g:10mL充分混合得到混合液2,混合液2在15℃下超声提取30min,超声功率为300W,超声频率为20kHz;提取完成后将混合液2过滤,滤渣重复上述操作3次,合并每次过滤得到的滤液为醇提液备用;
S4将所述步骤S2和S3得到的水提液和醇提液合并得到提取液;将提取液减压浓缩至原滤液体积的1/6得到浓缩滤液;
S5将所述步骤S4得到的浓缩滤液在-45℃下冷冻干燥48h即得到中药精华提取物;
所述紫外吸收剂为改性鞣花酸;
所述改性鞣花酸的制备方法为:将16g羟丙基-β-环糊精溶解在50mL水中得到羟丙基-β-环糊精溶液,另将8g鞣花酸分散在30mL无水乙醇中得到鞣花酸乙醇溶液,将其加入到羟丙基-β-环糊精溶液中,超声处理30min,再在25℃下搅拌16h,反应结束后将反应液在60℃下干燥24h得到改性鞣花酸。
实施例5
一种美白护肤品的制备方法,包括以下步骤:
N1将75份去离子水、0.5份苹果酸、2份蜂蜜、0.4黄原胶、0.2份乙二胺四乙酸二钠、0.2份山梨酸钾、4份氢化卵磷脂加入放入搅拌器中,在60℃下,搅拌30min,得到混合物A;
N2将8份甘油、2份烟酰胺、5份霍霍巴油、3份合成角鲨烷、5份水溶液神经酰胺、1份维生素E、3份紫外吸收剂加入放入搅拌器中,在60℃下,搅拌30min,得到混合物B;
N3将混合物A和混合物B放入乳化均质装置中,用均质15s,冷却后,搅拌15min,得到乳化物C;
N4将乳化物C放入超高压均质机中,在压力为180Mpa,均质4min,得到美白护肤品。
所述紫外吸收剂为质量比为3:1的纳米纤维素改性阿魏酸和改性鞣花酸的混合;
所述纳米纤维素改性阿魏酸的制备方法包括以下步骤:
M1将2g阿魏酸、0.6g 1-乙基-(3-二甲基氨基丙基)碳酰二亚胺、0.02g N-羟基丁二酰亚胺加入到150mL水中,超声分散15min,在40℃下反应5h,反应结束后即得到羧基活化的阿魏酸水溶液;
M2向步骤M1得到的羧基活化的阿魏酸水溶液中加入4g纳米纤维素,超声分散20min,在4℃下反应6h,反应结束后离心20min,倒掉上清液,即得到产物,将产物先用水洗3次,再用乙醇洗3次,将最后一次洗涤得到的产物在40℃下真空干燥即得到纳米纤维素改性阿魏酸;
所述改性鞣花酸的制备方法为:将16g羟丙基-β-环糊精溶解在50mL水中得到羟丙基-β-环糊精溶液,另将8g鞣花酸分散在30mL无水乙醇中得到鞣花酸乙醇溶液,将其加入到羟丙基-β-环糊精溶液中,超声处理30min,再在25℃下搅拌16h,反应结束后将反应液在60℃下干燥24h得到改性鞣花酸。
测试例1
美白功效测试:通过测试护肤品对酪氨酸酶的抑制率以及对DPPH(1,1-二苯基-2-三硝基苯肼)自由基的清除率作为其美白功效的指标。
酪氨酸酶的抑制率测试:先称取8.0g NaCl、0.2g KCl、1.44gNa2HPO4、0.24gKH2PO4溶于800mL蒸馏水中,用HCl水溶液调节溶液至7.4,最后加蒸馏水定容至1L即可得0.01M PBS缓冲液备用;精确称取酪氨酸酶,用所述PBS缓冲液配成200U/mL的酪氨酸酶水溶液,-20℃冷冻保存,用前4℃解冻;将3,4-二羟基苯丙氨酸溶解在所述PBS缓冲液配置1.5mg/mL的3,4-二羟基苯丙氨酸水溶液。按表1中各反应组,用移液枪移取反应液于5mL带盖塑料离心管中,混合均匀,37℃水浴恒温反应10min,再加入1mL 1.5mg/mL 3,4-二羟基苯丙氨酸水溶液,混合均匀,再在37℃水浴恒温反应4min,将混合液倒入比色皿,在第5min时在475nm处测定吸光度(上述PBS缓冲液做空白对照),得到A1、A2、A3、A4。平行实验三次。按公式:
抑制率(%)=[1-(A3-A4)/(A1-A2)]×100%
计算供试护肤品对酪氨酸酶的抑制率。
表1抑酶反应液的组成
DPPH自由基清除率测试:精确称取DPPH,用无水乙醇配成0.04mg/mL的溶液,4℃避光冷藏保存备用。按表2中各反应组,用移液枪移取反应液于5mL带盖塑料离心管中,混合均匀,避光静置反应30min,于517nm处测定吸光度(无水乙醇作为空白对照),得到A1、A2、A3。平行实验3次。按公式:
清除率(%)=[1-(A2-A3)/A1]×100%
计算供试护肤品对DPPH自由基的清除率。
表2抑酶反应液的组成
反应组 | DPPH自由基溶液/mL | 护肤品/mL | 无水乙醇/mL |
1 | 2 | 0 | 2 |
2 | 2 | 2 | 0 |
3 | 0 | 2 | 2 |
所得到的结果如表3所示。
表3美白功效测试结果
酪氨酸酶的抑制率(%) | DPPH自由基的清除率(%) | |
实施例1 | 97.2 | 98.6 |
实施例2 | 72.6 | 78.8 |
实施例3 | 89.2 | 76.2 |
实施例4 | 78.6 | 90.5 |
实施例5 | 70.7 | 81.2 |
通过分析表3的结果可知,实施例1对酪氨酸酶的抑制率以及对DPPH自由基的清除率都显著高于其他实施例,实施例2中直接添加阿魏酸,其溶解性较低,不易在护肤品中很好的分散,导致其在护肤品中分布得不均一,较难发挥自身效果以及与其他活性成分得协同作用;实施例3中将阿魏酸进行纳米纤维素化改性,利用纳米纤维素良好的水分散性,可以使其在护肤品中均匀分散,更好的与护肤品其他活性成分接触,起到良好得作用,其抑制酪氨酸酶抑制率相比实施例2显著提高,但是抗氧化能力反而降低,可能的原因是在改性过程中,阿魏酸主要起抗氧化作用的酚羟基可能部分与纳米纤维素反应形成醚键,导致其抗氧化活性减弱;实施例4中添加的紫外吸收剂为改性鞣花酸,其具有很强的抗氧化作用,使护肤品的抗氧化能力显著提高,但其对酪氨酸酶抑制率相对较弱;实施例5相比实施例1没有添加中药精华提取物,其效果均显著降低,这可能的原因是中药精华提取物中含有多种抑制酪氨酸酶活性以及抗氧化活性成分,如川芎中的阿魏酸,甘草中的黄酮类化合物,其中异甘草苷、异甘草素-葡萄糖芹菜苷和甘草查尔酮甲均对于酪氨酸酶存在竞争性抑制,白茯苓、木芙蓉叶和益母草提取物中除富含黄酮类化合物外,还含有多酚类等抗氧化物质,因此实施例5的功效显著降低。实施例1中既添加有中药精华提取物,又添加有纳米纤维素改性阿魏酸和改性鞣花酸复配的紫外添加剂,纳米纤维素改性阿魏酸均匀分散在护肤品中,与护肤品中其他活性成分通过协同作用起到良好的抑制酪氨酸酶活的作用,同时改性鞣花酸也很好的补足了由于改性阿魏酸抗氧化活性减弱的缺点,协同增效达到更好的美白效果。
测试例2
保湿功效测试:测试环境条件:环境温度为(22±1)℃,湿度为(50±5)%;受试者要求:人数30人,年龄16~45岁,无严重过敏性皮肤病;试验前,受试者需要清洗双手前臂内侧。清洗后,用记号笔在双手前臂内测标记将要测试的区域。正式测试开始前,应在恒温恒湿的测试房内放松状态逗留15min以上。测试过程中不能喝水,不能上厕所。
先将双手手臂内测标记多个3cm×3cm试验区域,区域间间隔1cm。测试产品随机分布在各个区域。然后按2.0mg护肤品/cm2的用量,用乳胶指套将实施例1~5制备的护肤品按序号依次均匀涂布于试验区内。分别测量涂抹前及涂抹后1,2,3和4h受试区域的皮肤含水量。同一个受试者的测试由同一个测量人员完成。
使用Corneometer 825型皮肤水分含量测试仪(MMV)测量皮肤含水量,MMV时基于电容的原理,水和其它物质的介电常数存在显著差异造成电容差,这种电容差产生仪器信号,在转换成水分含量显示出来。皮肤的含水量不同,所测得的电容值不同,其测定数值可代表皮肤水分值。通过计算水合变化率来表征测试周期内皮肤角质层水分含量的变化情况。按公式:
水合变化率(%)=(测试时水合度-初始水合度)/初始水合度×100%
所得结果如表4所示。
表4保湿功效测试结果
通过表4的结果可知,各实施例均有一定的保湿效果,可以看到使用完护肤品后,皮肤的即时水合度均达到最大,之后迅速降低,这是应为护肤品中的水分快速从皮肤表面蒸发的缘故,在1h之后水分基本蒸发完毕,保湿成分作用开始显现,2h时水合度有一定的上升,是吸收了空气中的水分,然后3h、4h水合度平稳降低。实施例1具有最好的长效保湿效果,这可能的原因是纳米纤维素改性阿魏酸其中的纳米纤维素具有较大的比表面积、良好的化学稳定性以及纤维之间彼此交错连接,同时表面具有大量羟基、羧基等亲水性官能团,具有良好的保湿能力,改性鞣花酸中的羟丙基-β-环糊精具有良好的亲水性,具有一定的吸湿能力,且鞣花酸由于其多酚结构,可以使毛孔收缩,防止水分的流失,多羟基的结构又能在空气中吸潮,保持皮肤表面的水分,中药精华提取物中的含有多种植物多糖成分,也具有优良的保水锁水功能,同时这些成分也能促进护肤品中其他保湿成分的吸收,增加皮肤的水合度,因此通过多种物质的协同作用使实施例具有良好的保湿效果。而实施例2~5均只有其中一项或几项物质,导致保湿效果不如实施例1。
测试例3
紫外吸收测试:使用QB/T 2410-98《防晒化妆品UVB区防晒效果的评价方法紫外吸光度法》测试实施例1~5制备精护肤品的紫外吸收能力,结果如表5所示。
表5紫外吸收测试结果
吸光度A | |
实施例1 | 2.05 |
实施例2 | 1.54 |
实施例3 | 1.73 |
实施例4 | 1.76 |
实施例5 | 1.87 |
通过表5的结果可知,各实施例均有不错的紫外吸收效果,其中实施例1的紫外吸收效果最好,阿魏酸具有良好的紫外吸收能力,但是其自身在水中溶解性不好,通过纳米纤维素对其改性,提高了其水溶性以及稳定性,因此实施例3的紫外吸收能力相比实施例2有显著提升,阿魏酸虽然有着较强的紫外吸收能力,但是其遇到紫外线不够稳定,容易分解,因此需要与其他紫外吸收剂配合应用;改性鞣花酸具有良好的全波段紫外吸收能力,同时具有很强的抗氧化能力,将其与纳米纤维素改性阿魏酸配合使用,可以产生显著的协同作用来对抗皮肤的光氧化应急,并将有助于抵抗光老化及皮肤问题,鞣花酸具有很高的氧化活性,可以延缓纳米纤维素改性阿魏酸的分解,显著提高其稳定性,延长紫外吸收时效;中药精华提取物中的黄酮类、多糖、有机酸类化合物也具有一定的紫外吸收能力,因此实施例1的紫外吸收效果显著由于其他实施例。
综上所述,本发明制备的美白护肤品通过作用于黑色素生成和转移的各个阶段,达到了更好的美白效果,同时将修复,补水,锁水,防晒功能集为一体,能达到长效保湿的目的,因此具有良好的美白保湿防晒功效。
Claims (8)
1.一种美白护肤品的制备方法,其特征在于,包括以下步骤:
N1将水、苹果酸、蜂蜜、黄原胶、乙二胺四乙酸二钠、防腐剂、氢化卵磷脂加入搅拌器中,在50~70℃下,搅拌25~40min,得到混合物A;
N2将甘油、烟酰胺、霍霍巴油、合成角鲨烷、水溶性神经酰胺、维生素E、紫外吸收剂加入搅拌器中,在50~70℃下,搅拌25~40min,得到混合物B;
N3将混合物A和混合物B放入乳化均质装置中,均质15~30s,冷却后,再向其中加入中药精华提取物,搅拌10~20min,得到乳化物C;
N4将乳化物C放入超高压均质机中,在压力为150~200MPa,均质3~5min,得到所述美白护肤品。
2.如权利要求1所述的美白护肤品的制备方法,其特征在于:所述美白护肤品的各原料的重量份为:60~75份水、4~10份甘油、1~2份烟酰胺、0.1~1份苹果酸、1~2份蜂蜜、2~6份霍霍巴油、1~4份合成角鲨烷、2~6份水溶性神经酰胺、0.5~2份维生素E、0.1~0.5份黄原胶、0.1~0.5份乙二胺四乙酸二钠、0.1~0.5份防腐剂、2~5份氢化卵磷脂、5~10份中药精华提取物、1~3份紫外吸收剂。
3.如权利要求1或2所述的美白护肤品的制备方法,其特征在于:所述防腐剂为苯甲酸钠或山梨酸钾。
4.如权利要求1或2所述的美白护肤品的制备方法,其特征在于:所述中药精华提取物由川芎、甘草、白茯苓、木芙蓉叶、益母草按照(2~6):(1~3):(2~6):(2~6):(2~6)的质量比提取而成。
5.如权利要求4所述的美白护肤品的制备方法,其特征在于,所述中药精华提取物由以下步骤制得:
S1将中药精华提取物的制备原料按比例混合,用粉碎机粉碎,过30~40目筛,得到粉碎后的原料密封在塑料袋中,放在阴凉干燥处备用;
S2将粉碎后的原料与水按用量比1g:(8~12)mL充分混合得到混合液1,混合液1在10~25℃下超声提取20~30min,超声功率为250~400W,超声频率为20~40kHz;提取完成后将混合液1过滤,滤渣重复上述操作2~3次,收集最后一次过滤的滤渣,合并每次过滤得到的滤液为水提液备用;
S3将步骤S2中最后一次过滤的滤渣与体积分数为70~75%的乙醇水溶液按用量比1g:(8~12)mL充分混合得到混合液2,混合液2在10~25℃下超声提取20~30min,超声功率为250~300W,超声频率为20~40kHz;提取完成后将混合液2过滤,滤渣重复上述操作2~3次,合并每次过滤得到的滤液为醇提液备用;
S4将步骤S2和S3得到的水提液和醇提液合并得到提取液;将提取液减压浓缩至原滤液体积的1/6~1/4得到浓缩滤液;
S5将步骤S4得到的浓缩滤液在-40~-45℃下冷冻干燥24~48h即得到中药精华提取物。
6.如权利要求1或2所述的美白护肤品的制备方法,其特征在于:所述紫外吸收剂为阿魏酸、纳米纤维素改性阿魏酸、鞣花酸、改性鞣花酸中的一种或两种及两种以上的混合。
7.如权利要求6所述的美白护肤品的制备方法,其特征在于,所述纳米纤维素改性阿魏酸的制备方法包括以下步骤:
M1将1~4g阿魏酸、0.1~1g 1-乙基-(3-二甲基氨基丙基)碳酰二亚胺、0.01~0.05gN-羟基丁二酰亚胺加入到100~200mL水中,超声分散15~30min,在30~50℃下反应2~5h,反应结束即得到羧基活化的阿魏酸水溶液;
M2向步骤M1得到的羧基活化的阿魏酸水溶液中加入2~5g纳米纤维素,超声分散10~20min,在30~50℃下反应3~6h,反应结束后离心10~20min,倒掉上清液,即得到产物,将产物先用水洗2~3次,再用乙醇洗2~3次,将最后一次洗涤得到的产物在40~60℃下真空干燥即得到纳米纤维素改性阿魏酸。
8.如权利要求6所述的美白护肤品的制备方法,其特征在于,所述改性鞣花酸的制备方法为:将10~20g羟丙基-β-环糊精溶解在25~50mL水中得到羟丙基-β-环糊精溶液,另将5~10g鞣花酸分散在20~30mL无水乙醇中得到鞣花酸乙醇溶液,将其加入到羟丙基-β-环糊精溶液中,超声处理20~30min,再在20~30℃下搅拌12~20h,反应结束后将反应液在60~80℃下干燥12~24h得到改性鞣花酸。
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