CN113304091B - 一种具有祛痘功效的美白保湿面膜及其制备方法 - Google Patents
一种具有祛痘功效的美白保湿面膜及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种具有祛痘功效的美白保湿面膜及其制备方法,包括以下步骤:取祛痘精华液、秦艽叶提取物、海藻糖、γ‑聚谷氨酸、角鲨烷加入到水中混合均匀,均质处理;冷却至室温,得到面膜液;将面膜液灌入到含有面膜载体的面膜袋内,真空封口,即得。本发明的具有祛痘功效的美白保湿面膜具备良好的祛痘、美白保湿功效。
Description
技术领域
本发明属于化妆品技术领域,具体涉及一种具有祛痘功效的美白保湿面膜及其制备方法。
背景技术
皮肤长痘属于常见的皮肤问题,不仅会引起身体的不适还会影响外貌形象。皮肤长痘、痤疮主要是由痤疮丙酸杆菌的大量繁殖使皮肤微环境被破坏,皮脂分解成游离酸,引起皮肤的红肿、疼痛等炎症,一般通过外用抗生素类药物、痤疮局部穿刺引流等治疗缓解,但是外用抗生素易产生耐药性,并且会有红斑、瘙痒等不良反应。采用天然植物活性成分来修复皮肤屏障,达到抗炎抑菌的效果是不错的选择。中国专利CN107184463A公开了一种美白祛痘面膜,配方中包括植物组合物,所述植物组合物由猪苓提取物、紫藤花提取物和长叶地榆提取物组成,其具有很好的祛痘、美白和抗衰老的作用,能够迅速修复祛痘后的损伤皮肤,但存在稳定性不佳,功效不持久的问题还需改善。
发明内容
针对上述现有技术中存在的不足,本发明提供了一种具有祛痘功效的美白保湿面膜及其制备方法。
为解决上述技术问题,本发明采用的技术方案是:
一种具有祛痘功效的美白保湿面膜的制备方法,包括以下步骤:
取祛痘精华液、秦艽叶提取物、海藻糖、γ-聚谷氨酸、角鲨烷加入到水中混合均匀,均质处理;冷却至室温,得到面膜液;将面膜液灌入到含有面膜载体的面膜袋内,真空封口,即得。
一种具有祛痘功效的美白保湿面膜的制备方法,包括以下步骤:
取55-60重量份祛痘精华液、3-5重量份秦艽叶提取物、1-3重量份海藻糖、1-3重量份γ-聚谷氨酸、2-4重量份角鲨烷加入到30-35重量份水中混合均匀,然后高压均质处理15-20min,均质压力为30-35Mpa;冷却至室温,得到面膜液;将面膜液灌入到含有面膜载体的面膜袋内,每袋灌装15-20g,真空封口,即得。
所述秦艽叶提取物的制备方法如下:将晾干的秦艽叶粉碎至50-100目,得到秦艽叶粉;取秦艽叶粉加入水中微波处理0.5-1h,料液比为1kg:(10-15)L,微波功率为600-700W;再加入秦艽叶粉质量10-30wt%的苹果酸,在90-100℃回流提取2-3h;冷却至室温,过滤,将滤液pH调至中性,冻干,即得。
所述祛痘精华液由以下质量百分比的物质组成:1-4%烟酰胺、5-10%沙棘油、1-8%赤藓醇、3-5%芦荟胶、2.0-3.8%甘油、0.25-0.4%山嵛醇、0.15-0.24%1,2-己二醇、0.03-0.06%维生素E、1-4%柠檬酸、0.1-3%聚合杏仁蛋白、0.05-0.2%透明质酸钠、0.07-0.1%乙二胺四乙酸二钠、1-5%凝血酸、0.13-0.25%熊果素、0.08-0.12%水溶性氮酮、0.01%-0.08%O-伞花烃-5-醇、0.15-0.25%尿囊素、0.05-0.2%生育酚乙酸酯、10-35%祛痘组合物、5-20%修复剂、余量为水。
所述祛痘精华液中,烟酰胺是起到保水锁水的作用;熊果素具有杀菌、消炎的作用;以芦荟胶、赤藓醇、甘油、1,2-己二醇作为、透明质酸钠保湿剂;山嵛醇作为乳化剂;凝血酸、维生素E、生育酚乙酸酯作为抗氧化剂、乙二胺四乙酸二钠作为金属螯合剂作为增稠剂;水溶性氮酮为渗透剂、O-伞花烃-5-醇为防腐剂;尿囊素具有促进细胞生长,加快伤口愈合;祛痘组合物作为主要祛痘的活性物质,用于祛除痤疮、青春痘、粉刺等;修复剂可以调节皮肤,促进新成代谢,以达到修复受损皮肤的作用。
人之所以会长痘,是应为皮肤表面和皮脂腺毛囊中存在着多种如痤疮丙酸杆菌、表皮葡萄球菌和糠秕孢子菌等微生物,尤以痤疮丙酸杆菌与痤疮炎症的关联性最强。而本发明中主要的祛痘物质是祛痘组合物,加入了天然、安全、无刺激并且具有祛痘效果的祛痘组合物。
所述祛痘组合物的制备方法如下:
S1、将质量比为(1-10):(1-10):(1-8):(1-8):(1-8)的北苍术、母菊花、三色堇菜、台湾山芙蓉、苦参根混合,粉碎,过10-40目筛,得到混合粉末;
S2、将混合粉末与60-80wt%乙醇水溶液按质量比1:(1-5)混合,置于带有氮气保护的回流装置中,在80-90℃下回流4-8h,冷却至室温后抽滤,保留滤液A,滤饼置于60-80℃下真空干燥4-10h后,备用;
S3、将步骤S2干燥后的滤饼加入超临界CO2萃取釜,通入液态CO2,流量为1-4mL/min,同时通入50-80wt%乙醇水溶液作为夹带剂,流量为0.1-0.4mL/min,在40-60℃、压力20-40MPa下萃取1-3h,得萃取物,合并萃取物和滤液A,得到滤液B;
S4、将滤液B在50-70℃、-0.01--0.1MPa旋转蒸发至体积为原体积的8%-20%,获得浓缩液;将浓缩液冷却至0-8℃,离心取上清液,将上清液用500-2000目滤布过滤,保留滤液,即祛痘组合物。
北苍术提取物中具有挥发油、苍术醇、苍术酮、茅术醇及桉叶醇等,对多种细菌具有抗菌抑菌作用,可以替代防腐剂,应用于防治粉刺,对酪氨酸酶有抑制作用,结合其抗氧化性,可用作美白和抗衰成分;母菊花提取物中富含挥发油、黄酮类、香豆素等多种成分,其具有消炎、抗敏、舒缓、抑菌和解痉等作用,不仅能均衡油脂分泌,抑脂抗痘,防止粉刺,消除黑斑,美白肌肤,而且对某些皮肤致病性真菌具有抑制及杀菌作用。三色堇菜提取物富含类胡萝卜素、黄酮化合物、酚酸类成分,能够有效抑制黑色素B-16细胞活性,具有杀菌,治疗皮肤上青春痘、粉刺、过敏、减少毛孔等功效。台湾山芙蓉提取物含有木脂素类化合物、酰胺类化合物,萜类化合物,具有祛痘抗炎、抗氧化、抗痤疮丙酸杆菌、控油、减少毛孔等功效。苦参根提取物能够平衡肌肤的油脂分泌,疏通并收敛毛孔,清除皮肤内毒素杂质,对痤疮丙酸杆菌具有良好的抑菌作用,促进受损血管神经细胞的生长和修复,恢复皮下毛细血管细胞活力。
北苍术提取物、母菊花提取物、三色堇菜提取物、台湾山芙蓉提取物以及苦参根提取物可以从调节皮脂分泌、调节表皮过度角质、美白保湿、抑制痤疮丙酸杆菌繁殖、祛痘抗炎这五个维度着手来预防以及清除痤疮,不仅高效,而且非常温和安全。
所述修复剂为苜蓿多糖或改性苜蓿多糖。
所述苜蓿多糖的制备方法如下:
X1、将苜蓿草在90-110℃干燥3-5h,粉碎,过5-30目筛,得到苜蓿粉末,按质量比1:(15-25)将苜蓿粉末与水混合均匀,在80-100℃下提取1-3h,过滤,得到滤液Ⅰ和滤渣Ⅰ,在滤渣Ⅰ中加水,所述滤渣Ⅰ和水的质量比为1:(10-20),在80-100℃下加热0.5-2h,过滤,得二次滤液和滤渣Ⅱ,合并滤液Ⅲ;
X2、将X1中的滤液Ⅲ置于50-80℃、-0.01~-0.1MPa蒸发浓缩至原体积的10-30%,得浓缩液,在浓缩液中加入3-6倍质量的无水乙醇进行醇析,静置8-14h,在4000rpm下离心10min,弃上清液,得粗多糖,加入粗多糖质量5倍的水,得到粗多糖溶液;
X3、将上述粗多糖溶液置于0-8℃环境中,用截留分子量为500-2000Da的透析袋透析20-30h,每隔2-4h更换水,收集透析液A,加入透析液A质量相等的三氯甲烷,置于0-8℃沉淀8-16h,离心,取上清液,在上清液中加入5-8倍质量的无水乙醇进行醇析,静置8-14h,在4000rpm下离心10min,将固体冷冻干燥,得苜蓿多糖。
尽管现有技术中祛痘产品的效果比较好,但是对于祛痘之后皮肤的角质层受损,容易受到大量细菌的感染,导致祛痘之后肌肤恢复较慢,甚至祛痘之后肌肤因没有做好修复而受到感染导致留下痘印甚至是疤痕,本发明的目的在于既要达到祛痘的效果就要在祛痘之后将肌肤得到更好的修复,使得肌肤保持白皙透嫩的效果。
植物多糖中含有大量的羟基,使得亲水性比较好,用于化妆品中能够使得肌肤达到非常好的保湿效果,同时也能使得祛痘之后的肌肤得到很快修复,提高祛痘的效果,但是本发明还发现,植物多糖经改性之后使表面富有修饰基团,有利于减弱植物多糖的羟基氢键作用,增加改性引入的化学基团之间的弱作用力,使得化妆品形成紧密的网络作用,进而具有更好的成膜,以配合角质层锁住水分子,可以进一步提高保水效果。
具体的,苜蓿中提取得到的多糖与改性剂在加热后发生美拉德反应,使改性剂的氨基与多糖的羰基之间发生羰氨反应,形成多糖衍生物,保留了改性剂结构中羧基和羟基的持水作用,进一步增强了多糖的溶解性和保湿能力,同时增强了多糖的抗氧化能力和热稳定性。将其添加到化妆品中,有效减缓了多糖的氧化变质。与北苍术提取物、母菊花提取物、三色堇菜提取物、台湾山芙蓉提取物以及苦参根提取物一起使用,利用其成分的协同作用,可达到调节皮脂分泌、调节表皮过度角质、美白保湿、抑制痤疮丙酸杆菌繁殖、祛痘抗炎、补水保湿、改善肤质,以达到修复受损皮肤的作用。
优选的,所述修复剂为改性苜蓿多糖;所述改性苜蓿多糖的制备方法如下:
X1、将苜蓿草在90-110℃干燥3-5h,粉碎,过5-30目筛,得到苜蓿粉末,按质量比1:(15-25)将苜蓿粉末与水混合均匀,在80-100℃下提取1-3h,过滤,得到滤液Ⅰ和滤渣Ⅰ,在滤渣Ⅰ中加水,所述滤渣Ⅰ和水的质量比为1:(10-20),在80-100℃下加热0.5-2h,过滤,得二次滤液和滤渣Ⅱ,合并滤液Ⅲ;
X2、将X1中的滤液Ⅲ置于50-80℃、-0.01~-0.1MPa蒸发浓缩至原体积的10-30%,得浓缩液,在浓缩液中加入3-6倍质量的无水乙醇进行醇析,静置8-14h,在4000rpm下离心10min,弃上清液,得粗多糖,加入粗多糖质量5倍的水,得到粗多糖溶液;
X3、将上述粗多糖溶液置于0-8℃环境中,用截留分子量为500-2000Da的透析袋透析20-30h,每隔2-4h更换水,收集透析液A,加入透析液A质量相等的三氯甲烷,置于0-8℃沉淀8-16h,离心,取上清液,在上清液中加入5-8倍质量的无水乙醇进行醇析,静置8-14h,在4000rpm下离心10min,将固体冷冻干燥,得苜蓿多糖;
X4、将X3中的苜蓿多糖与改性剂按质量比(4-10):1混合均匀,加入苜蓿多糖质量的4-10倍的水,在60-80℃回流加热4-7h,得改性多糖水溶液;再用截留分子量为500-2000Da的透析袋透析20-30h,收集透析液B,冷冻干燥,得改性苜蓿多糖。
所述改性剂为苏氨酸和/或谷氨酸;优选的,所述改性剂由苏氨酸和谷氨酸按照质量比(1-3):(1-5)组成的混合物。
所述的祛痘精华液的制备方法如下:
(1)按配方将烟酰胺、赤藓醇、芦荟胶、1,2-己二醇、甘油、维生素E、柠檬酸、透明质酸钠、乙二胺四乙酸二钠、凝血酸、熊果素、水溶性氮酮、水混合,在50-60℃、300-500rpm下搅拌10-30min,得混合液A;
(2)将沙棘油、山嵛醇、聚合杏仁蛋白、尿囊素、O-伞花烃-5-醇、生育酚乙酸酯混合,在70-80℃、300-500rpm下搅拌10-20min,加入所述步骤(1)中的混合液A,继续搅拌10-20min;再加入祛痘组合物和修复剂,在室温、300-500rpm下搅拌10-20min,即得祛痘精华液。
一种具有祛痘功效的美白保湿面膜,采用上述方法制备而成。
本发明的有益效果:本发明的具有祛痘功效的美白保湿面膜具有良好的祛痘、美白保湿功效。在祛痘精华液中加入祛痘组合物,具有控制油脂分泌,疏通毛孔,抑菌消毒,祛痘的功效;能够软化角质层,促进角质层更新,软化角质层,有利于活性成分渗透进入皮肤深层,还有消炎抗敏作用,北苍术提取物、母菊花提取物、三色堇菜提取物、台湾山芙蓉提取物以及苦参根提取物可以从调节皮脂分泌、调节表皮过度角质、美白保湿、抑制痤疮丙酸杆菌繁殖、祛痘抗炎这五个维度着手来预防以及清除痤疮,不仅高效,而且非常温和安全。
具体实施方式
下面结合具体实施方式对本发明的上述发明内容作进一步的详细描述,但不应将此理解为本发明上述主题的范围仅限于下述实施例。
本申请中部分原料的介绍:
实施例中沙棘油购于甘肃艾康沙棘制品有限公司,货号:sj-03。
实施例中芦荟胶购于广州尚研生物科技有限公司,货号:NO.BQY2850。
实施例中聚合杏仁蛋白购于广州市腾源生物化工有限公司,货号:02213。
实施例中水溶性氮酮购于湖北鑫润德化工有限公司,水溶性氮酮有效含量:≥30.0%。
实施例中苜蓿草来源兰考田园牧歌草业有限公司。
对照组中市售祛痘精华液购于广州市颜婷化妆品有限公司,货号:YT0028。主要植物精华成分:连翘、金银花、茶树油、蒲公英、紫花地丁。
北苍术:以北苍术(Rhizoma Atractylodis)的茎为原料。主要成分为挥发油、苍术醇、苍术酮、茅术醇及桉叶醇等;苍术挥发油具有新鲜而强烈的木香、辛香、奶油香等混合气息;对多种细菌具有抗菌抑菌作用,可以替代防腐剂,应用于防治粉刺;对酪氨酸酶有抑制作用,结合其抗氧化性,可用作美白和抗衰成分。
母菊花:以母菊花(Matricaria recutita L)的花为原料。富含挥发油、黄酮类、香豆素等多种成分,其具有消炎、抗敏、舒缓、抑菌和解痉等作用,不仅能均衡油脂分泌,抑脂抗痘,防止粉刺,消除黑斑,美白肌肤,而且对某些皮肤致病性真菌具有抑制及杀菌作用。添加于化妆品中的洗面奶、护肤霜、按摩膏、面膜中具有良好的护肤、美肤治疗作用。
三色堇菜:以三色堇菜(Viola tricolor L.)的叶为原料。富含类胡萝卜素、黄酮化合物、酚酸类成分,能够有效抑制黑色素B-16细胞活性,同时能够促进水通道蛋白和透明质酸的生成,具有杀菌,治疗皮肤上青春痘、粉刺、过敏、减少毛孔等功效。
台湾山芙蓉:以台湾山芙蓉(Hibiscus taiwanensis S.Y.Hu)的叶为原料。主要成分为木脂素类化合物,酰胺类化合物,萜类化合物,甾醇类化合物以及萘醌类等化合物,具有抗炎、抗氧化、抗痤疮丙酸杆菌、控油、减少毛孔等功效。
苦参根:是苦参(Sophora flavescens Alt.)的根。能够平衡肌肤的油脂分泌,疏通并收敛毛孔,清除皮肤内毒素杂质,对痤疮丙酸杆菌具有良好的抑菌作用,促进受损血管神经细胞的生长和修复,恢复皮下毛细血管细胞活力。
实施例1
一种祛痘精华液,由以下质量百分比的物质组成:2%烟酰胺、6%沙棘油、4%赤藓醇、4%芦荟胶、3%甘油、0.3%山嵛醇、0.2%1,2-己二醇、0.05%维生素E、2%柠檬酸、1%聚合杏仁蛋白、0.1%透明质酸钠、0.08%乙二胺四乙酸二钠、3%凝血酸、0.2%熊果素、0.1%水溶性氮酮、0.05%O-伞花烃-5-醇、0.1%尿囊素、0.1%生育酚乙酸酯、余量为水。
祛痘精华液的制备方法如下:
(1)按配方将烟酰胺、赤藓醇、芦荟胶、1,2-己二醇、甘油、维生素E、柠檬酸、透明质酸钠、乙二胺四乙酸二钠、凝血酸、熊果素、水溶性氮酮、水混合,在60℃、400rpm下搅拌20min,得混合液A;
(2)将沙棘油、山嵛醇、聚合杏仁蛋白、尿囊素、O-伞花烃-5-醇、生育酚乙酸酯混合,在70℃、400rpm下搅拌20min,加入所述步骤(1)中的混合液A,继续搅拌15min;再加入祛痘组合物和修复剂,在室温、400rpm搅拌10min,即得祛痘精华液。
实施例2
一种祛痘精华液,由以下质量百分比的物质组成:2%烟酰胺、6%沙棘油、4%赤藓醇、4%芦荟胶、3%甘油、0.3%山嵛醇、0.2%1,2-己二醇、0.05%维生素E、2%柠檬酸、1%聚合杏仁蛋白、0.1%透明质酸钠、0.08%乙二胺四乙酸二钠、3%凝血酸、0.2%熊果素、0.1%水溶性氮酮、0.05%O-伞花烃-5-醇、0.1%尿囊素、0.1%生育酚乙酸酯、20%祛痘组合物、余量为水。
所述祛痘组合物的制备方法如下:S1、将质量比为7:7:5:5:5的北苍术、母菊花、三色堇菜、台湾山芙蓉、苦参根混合,粉碎,过20目筛,得到混合粉末;
S2、将混合粉末与75wt%的乙醇水溶液按质量比1:3混合,置于带有氮气保护的回流装置中,在80℃下回流6h,冷却至室温后抽滤,保留滤液A,滤饼置于70℃下真空干燥6h后,备用;
S3、将步骤S2干燥后的滤饼加入超临界CO2萃取釜中,通入液态CO2,流量为2mL/min,同时通入60wt%乙醇水溶液做夹带剂,流量为0.2mL/min,在50℃、压力30MPa下萃取1.5h,得萃取物,合并萃取物和滤液A,得到滤液B;
S4、将滤液B在60℃、-0.05MPa旋转蒸发至原体积的10%获得浓缩液;将浓缩液冷却至4℃,离心取上清液,将上清液用1000目滤布过滤,保留滤液,即祛痘组合物。
祛痘精华液的制备方法如下:
(1)按配方将烟酰胺、赤藓醇、芦荟胶、1,2-己二醇、甘油、维生素E、柠檬酸、透明质酸钠、乙二胺四乙酸二钠、凝血酸、熊果素、水溶性氮酮、水混合,在60℃、400rpm下搅拌20min,得混合液A;
(2)将沙棘油、山嵛醇、聚合杏仁蛋白、尿囊素、O-伞花烃-5-醇、生育酚乙酸酯混合,在70℃、400rpm下搅拌20min,加入所述步骤(1)中的混合液A,继续搅拌15min;再加入祛痘组合物和修复剂,在室温、400rpm搅拌10min,即得祛痘精华液。
对比例1
与实施例2基本相同,其区别仅在于,所述祛痘组合物的制备方法如下:
S1、将质量比为7:7:5:5:5的北苍术、母菊花、三色堇菜、台湾山芙蓉、苦参根混合,粉碎,过20目筛,得到混合粉末;
S2、将混合粉末与75wt%的乙醇水溶液按质量比1:3混合,置于带有氮气保护的回流装置中,在80℃下回流6h,冷却至室温后抽滤,保留滤液A;
S3、将滤液A在60℃、-0.05MPa旋转蒸发至原体积的10%获得浓缩液;将浓缩液冷却至4℃,离心取上清液,将上清液用1000目滤布过滤,保留滤液,即祛痘组合物。
实施例3
一种祛痘精华液,由以下质量百分比的物质组成:2%烟酰胺、6%沙棘油、4%赤藓醇、4%芦荟胶、3%甘油、0.3%山嵛醇、0.2%1,2-己二醇、0.05%维生素E、2%柠檬酸、1%聚合杏仁蛋白、0.1%透明质酸钠、0.08%乙二胺四乙酸二钠、3%凝血酸、0.2%熊果素、0.1%水溶性氮酮、0.02%O-伞花烃-5-醇、0.1%尿囊素、0.1%生育酚乙酸酯、20%祛痘组合物、10%修复剂、余量为水。
所述祛痘组合物的制备方法如下:
S1、将质量比为7:7:5:5:5的北苍术、母菊花、三色堇菜、台湾山芙蓉、苦参根混合,粉碎,过20目筛,得到混合粉末;
S2、将混合粉末与75wt%的乙醇水溶液按质量比1:3混合,置于带有氮气保护的回流装置中,在80℃下回流6h,冷却至室温后抽滤,保留滤液A,滤饼置于70℃下真空干燥6h后,备用;
S3、将步骤S2干燥后的滤饼加入超临界CO2萃取釜中,通入液态CO2,流量为2mL/min,同时通入60wt%乙醇水溶液做夹带剂,流量为0.2mL/min,在50℃、压力30MPa下萃取1.5h,得萃取物,合并萃取物和滤液A,得到滤液B;
S4、将滤液B在60℃、-0.05MPa旋转蒸发至原体积的10%获得浓缩液;将浓缩液冷却至4℃,离心取上清液,将上清液用1000目滤布过滤,保留滤液,即祛痘组合物。
所述修复剂为苜蓿多糖;所述苜蓿多糖的制备方法如下:
X1、将苜蓿草在100℃干燥4h,粉碎,过10目筛,得到苜蓿粉末,按质量比1:20将苜蓿粉末与水混合均匀,在90℃下提取1.5h,过滤,得到滤液Ⅰ和滤渣Ⅰ,在滤渣Ⅰ中加水,所述滤渣Ⅰ和水的质量比为1:15,在90℃下加热1h,过滤,得二次滤液和滤渣Ⅱ,合并滤液Ⅲ;
X2、将X1中的滤液Ⅲ置于70℃、-0.05MPa蒸发浓缩至原体积的15%,得浓缩液,在浓缩液中加入4倍质量的无水乙醇进行醇析,静置12h,在4000rpm下离心10min,得粗多糖,加入粗多糖质量5倍的水,得到粗多糖溶液;
X3、将上述粗多糖溶液置于4℃环境中,用截留分子量为1000Da的透析袋透析24h,每隔3h更换水,收集透析液A,加入透析液A质量相等的三氯甲烷,置于4℃沉淀12h,离心,取上清液,在上清液中加入6倍质量的无水乙醇进行醇析,静置12h,在4000rpm下离心10min,将固体冷冻干燥,得苜蓿多糖;
祛痘精华液的制备方法如下:
(1)按配方将烟酰胺、赤藓醇、芦荟胶、1,2-己二醇、甘油、维生素E、柠檬酸、透明质酸钠、乙二胺四乙酸二钠、凝血酸、熊果素、水溶性氮酮、水混合,在60℃、400rpm下搅拌20min,得混合液A;
(2)将沙棘油、山嵛醇、聚合杏仁蛋白、尿囊素、O-伞花烃-5-醇、生育酚乙酸酯混合,在70℃、400rpm下搅拌20min,加入步骤(1)的混合液A,继续搅拌15min;再加入祛痘组合物和修复剂,在室温、400rpm搅拌10min,即得祛痘精华液。
实施例4
与实施例3基本相同,其区别仅在于,所述修复剂为改性苜蓿多糖;
所述改性苜蓿多糖的制备方法如下:
X1、将苜蓿草在100℃干燥4h,粉碎,过10目筛,得到苜蓿粉末,按质量比1:20将苜蓿粉末与水混合均匀,在90℃下提取1.5h,过滤,得到滤液Ⅰ和滤渣Ⅰ,在滤渣Ⅰ中加水,所述滤渣Ⅰ和水的质量比为1:15,在90℃下加热1h,过滤,得二次滤液和滤渣Ⅱ,合并滤液Ⅲ;
X2、将X1中的滤液Ⅲ置于70℃、-0.05MPa蒸发浓缩至原体积的15%,得浓缩液,在浓缩液中加入4倍质量的无水乙醇进行醇析,静置12h,在4000rpm下离心10min,得粗多糖,加入粗多糖质量5倍的水,得到粗多糖溶液;
X3、将上述粗多糖溶液置于4℃环境中,用截留分子量为1000Da的透析袋透析24h,每隔3h更换水,收集透析液A,加入透析液A质量相等的三氯甲烷,置于4℃沉淀12h,离心,取上清液,在上清液中加入6倍质量的无水乙醇进行醇析,静置12h,在4000rpm下离心10min,将固体冷冻干燥,得苜蓿多糖;
X4、将X3中的苜蓿多糖与改性剂按质量比6:1混合均匀,加入苜蓿多糖质量6倍的水,在70℃回流加热5h,得改性多糖水溶液;再用截留分子量为1000Da的透析袋透析24h,每隔3h更换水,收集透析液B,冷冻干燥,得改性苜蓿多糖。
所述改性剂为苏氨酸。
实施例5
与实施例4基本相同,其区别仅在于,所述改性剂为谷氨酸。
实施例6
与实施例4基本相同,其区别仅在于,所述改性剂由苏氨酸和谷氨酸按照质量比2:3组成。
测试例1
抑菌试验:参照国家标准GB 15979-2002《一次性使用卫生用品卫生标准》中附录C4“溶出性抗(抑)菌产品抑菌性能试验方法”进行本发明实施例1-6和对比例1的祛痘精华液的抑菌性能测定。
试验菌种:痤疮丙酸杆菌ATCC6919、大肠杆菌ATCC25922、金黄色葡萄球菌ATCC6538和白色念珠菌ATCC10231。
培养条件:大肠杆菌、金黄色葡萄球菌采用普通营养琼脂培养基培养,37℃条件下培养48h;痤疮丙酸杆菌在葡萄糖营养液中37℃厌氧培养48h;白色念珠菌在沙氏琼脂培养基中30℃培养3天。
测试:①菌悬液的制备:试验菌24h(细菌)培养物用0.03mol/L磷酸盐缓冲液洗下,制成106efu/mL菌悬液;②分别取被试样品1g,加人上述菌悬液0.1mL均匀涂布混合,开始计时20min后,加入9mL 0.03mol/L磷酸盐缓冲液充分混匀,作适当稀释后,取其中3个稀释度,分别取1mL置于两个平行平皿内,再加入相应培养基分别混菌培养,作菌落计数。以上试验重复4次,取其平均数,同时设空白对照。计算公式:X(%)=(A-B)/A×100,其中X为抑菌率,A为对照样品平均回收菌落数;B为试验样品平均回收菌落数。结果见表1。
表1抑菌试验结果
表1结果表明,在祛痘精华液中添加祛痘组合物能够明显抑制细菌的生成,进而抑制青春痘的产生,达到祛痘的效果。主要是因为苍术提取物中具有挥发油、苍术醇、苍术酮、茅术醇及桉叶醇等,对多种细菌具有抗菌抑菌作用,应用于防治粉刺;母菊花提取物中富含挥发油、黄酮类、香豆素等多种成分,其具有消炎、抗敏、舒缓、抑菌和解痉等作用,不仅能均衡油脂分泌,抑脂抗痘,防止粉刺,消除黑斑,美白肌肤,而且对某些皮肤致病性真菌具有抑制及杀菌作用;三色堇菜提取物富含类胡萝卜素、黄酮化合物、酚酸类成分,能够有效抑制黑色素B-16细胞活性,具有杀菌,治疗皮肤上青春痘、粉刺、过敏、减少毛孔等功效。台湾山芙蓉提取物含有木脂素类化合物、酰胺类化合物,萜类化合物,具有祛痘抗炎、抗氧化、抗痤疮丙酸杆菌、控油、减少毛孔等功效。苦参根提取物能够平衡肌肤的油脂分泌,疏通并收敛毛孔,清除皮肤内毒素杂质,对痤疮丙酸杆菌具有良好的抑菌作用,促进受损血管神经细胞的生长和修复,恢复皮下毛细血管细胞活力。
比较实施例2和对比例1可看出,实施例2采用醇水提和超临界联合提取能够有效提高提取物中的活性物质的含量,从而提高对细菌的抑制率,进而提到祛痘的效果。
因此将北苍术提取物、母菊花提取物、三色堇菜提取物、台湾山芙蓉提取物以及苦参根提取物结合起来其实可以从调节皮脂分泌、调节表皮过度角质、美白保湿、抑制痤疮丙酸杆菌繁殖、祛痘抗炎这五个维度着手来预防以及清除痤疮,不仅高效,而且非常温和安全。
而舒缓剂保留了羟基改性剂结构中羟基的持水作用,进一步增强了多糖的溶解性和保湿能力。将其添加到化妆品中,有效减缓了多糖的氧化变质。与本发明的祛痘组合物一起使用,利用其成分的协同作用,可达到调节皮脂分泌、调节表皮过度角质、抑制痤疮丙酸杆菌繁殖、祛痘抗炎、补水保湿、改善肤质,以达到修复受损皮肤的作用。
测试例2
试验人员:320名年龄在15-30岁的脸部有青春痘、丘疹、痤疮、粉刺等的患者,将其分成8组,每组40人,每组男女均分。
使用方法:试验人员的面部用水清洗干净,试验组取(1.0±0.1)mg/cm2本发明实施例1-6和对比例1中的祛痘精华液均匀涂抹于患处,对照组同样取等量的市售祛痘精华液均匀涂抹于患处。每天早、晚各使用一次,试验周期28天。
1、祛痘测试:
效果评价标准:
(1)痊愈:祛痘率90%以上消退,皮肤有光泽,炎症基本消失;
(2)显效:祛痘率60%以上消退,皮肤较有光泽,炎症明显变淡;
(3)好转:祛痘率30%以上消退,皮肤略有光泽,部分炎症变淡;
(4)无效:祛痘率小于30%,皮肤暗黄,炎症有所改善。
表2祛痘测试结果
痊愈(人) | 显效(人) | 好转(人) | 无效(人) | |
实施例1 | 6 | 10 | 20 | 4 |
实施例2 | 30 | 9 | 1 | 0 |
对比例1 | 21 | 9 | 10 | 0 |
实施例3 | 33 | 5 | 2 | 0 |
实施例4 | 35 | 5 | 0 | 0 |
实施例5 | 36 | 4 | 0 | 0 |
实施例6 | 39 | 1 | 0 | 0 |
对照组 | 5 | 15 | 13 | 7 |
从上述表2结果可知,本发明采用北苍术提取物、母菊花提取物、三色堇菜提取物、台湾山芙蓉提取物以及苦参根提取物制备得到的祛痘精华液具有显著的祛痘优势,采用科学的配方,利用各物质的有效物质之间的协同作用,且对青春痘、丘疹、粉刺等类型的痤疮有显著效果,使用本发明的祛痘精华液具有见效快,天然安全无刺激,且具有恢复痘印的功效,使得肌肤红润光泽。
2、修复性能测试:
试验人员使用本产品28天后,进入恒温恒湿评测室静待30分钟后测试使用前面部油脂含量和水分变化率以及回访后皮肤油脂含量和水分变化率,然后统计油脂变化率和水分变化率。水分变化率使用Tewameter探头连续测试5次取平均值,测试结果越高,表皮水分流失越少,水分含量越高,修复效果越好;油脂含量使用Sebumeter探头连续测试5次取平均值,测试结果越低,表皮油脂越少,祛痘和修复效果越好;使用多功能皮肤测试仪进行测试,测试环境温度为20℃,湿度为55%。计算公式:Y(%)=(Q-P)/P×100,其中Y为水分或者油脂变化率,P为使用祛痘精华液前的水分或者油脂含量;Q为使用祛痘精华液后的水分或者油脂含量。水分变化率和油脂变化率见表3。
表3修复性能测试结果
水分变化率(%) | 油脂变化率(%) | |
实施例2 | 20.5 | -21.9 |
实施例3 | 24.7 | -25.3 |
实施例4 | 27.9 | -28.6 |
实施例5 | 28.1 | -29.4 |
实施例6 | 31.4 | -33.9 |
对照组 | 8.43 | -9.57 |
表3结果可知,实施例2-6的水分流失率变化率和油脂变化率均好于对照组,说明使用本发明配方制备的祛痘精华液具有良好的修复作用,苜蓿多糖经改性之后使表面富有修饰基团,有利于减弱植物多糖的羟基氢键作用,增加改性引入的化学基团之间的弱作用力,采用谷氨酸和苏氨酸进行改性,能够起到协同增效的作用,使得化妆品形成紧密的网络作用,进而具有更好的成膜,以配合角质层锁住水分子,可以进一步提高保水效果,同时可以改善肤质,以达到修复受损皮肤的作用,可提高皮肤的湿润性,并且可减少产生痤疮的几率。
实施例7
一种具有祛痘功效的美白保湿面膜,由以下方法制备而成:
取58重量份实施例4所得祛痘精华液、4.5重量份秦艽叶提取物、3重量份海藻糖、3重量份γ-聚谷氨酸、2.5重量份角鲨烷加入到32重量份水中混合均匀,然后高压均质处理18min,均质压力为30Mpa;冷却至室温,得到面膜液;将面膜液灌入到含有面膜载体的面膜袋内,每袋灌装20g,真空封口,即得。
所述秦艽叶提取物的制备方法如下:将晾干的秦艽叶粉碎至80目,得到秦艽叶粉;取秦艽叶粉加入水中微波处理0.5h,料液比为1kg:12L,微波功率为650W;再加入秦艽叶粉质量25wt%的苹果酸,在100℃回流提取2.5h;冷却至室温,过滤,将滤液pH调至中性,冻干,即得。其中秦艽叶,是秦艽(Gentiana macrophylla)的叶;γ-聚谷氨酸购于云南力莲生物有限公司,CAS:25513-46-6,分子量700000。
实施例8
一种具有祛痘功效的美白保湿面膜,由以下方法制备而成:
取58重量份实施例5所得祛痘精华液、4.5重量份秦艽叶提取物、3重量份海藻糖、3重量份γ-聚谷氨酸、2.5重量份角鲨烷加入到32重量份水中混合均匀,然后高压均质处理18min,均质压力为30Mpa;冷却至室温,得到面膜液;将面膜液灌入到含有面膜载体的面膜袋内,每袋灌装20g,真空封口,即得。
所述秦艽叶提取物的制备方法如下:将晾干的秦艽叶粉碎至80目,得到秦艽叶粉;取秦艽叶粉加入水中微波处理0.5h,料液比为1kg:12L,微波功率为650W;再加入秦艽叶粉质量25wt%的苹果酸,在100℃回流提取2.5h;冷却至室温,过滤,将滤液pH调至中性,冻干,即得。其中秦艽叶,是秦艽(Gentiana macrophylla)的叶;γ-聚谷氨酸购于云南力莲生物有限公司,CAS:25513-46-6,分子量700000。
实施例9
一种具有祛痘功效的美白保湿面膜,由以下方法制备而成:
取58重量份实施例6所得祛痘精华液、4.5重量份秦艽叶提取物、3重量份海藻糖、3重量份γ-聚谷氨酸、2.5重量份角鲨烷加入到32重量份水中混合均匀,然后高压均质处理18min,均质压力为30Mpa;冷却至室温,得到面膜液;将面膜液灌入到含有面膜载体的面膜袋内,每袋灌装20g,真空封口,即得。
所述秦艽叶提取物的制备方法如下:将晾干的秦艽叶粉碎至80目,得到秦艽叶粉;取秦艽叶粉加入水中微波处理0.5h,料液比为1kg:12L,微波功率为650W;再加入秦艽叶粉质量25wt%的苹果酸,在100℃回流提取2.5h;冷却至室温,过滤,将滤液pH调至中性,冻干,即得。其中秦艽叶,是秦艽(Gentiana macrophylla)的叶;γ-聚谷氨酸购于云南力莲生物有限公司,CAS:25513-46-6,分子量700000。
测试例3
具有祛痘功效的美白保湿面膜的性能测试:取实施例7-9制得的面膜液配制0.6mg/mL待测溶液,以及配制105U/mL的酪氨酸酶溶液、0.02mol/L的L-酪氨酸溶液备用,上述均采用磷酸盐缓冲液配制。取1mL的待测溶液、1mL的L-酪氨酸溶液、1mL的酪氨酸酶溶液、2mL的磷酸盐缓冲溶液混合均匀,在37℃静置15min后测定475nm处吸光度,平行五组,取平均值,计算酪氨酸酶抑制率。
酪氨酸酶抑制率=[1-(D3-D4)/(D1-D2)]×100%;其中,D1不添加待测溶液;D2不添加待测溶液及酪氨酸酶溶液;D3添加待测溶液、L-酪氨酸溶液及酪氨酸酶溶液;D4不添加酪氨酸酶溶液;加入磷酸盐缓冲液至反应体系5mL。
表4酪氨酸酶抑制率测试结果
酪氨酸酶抑制率(%) | |
实施例7 | 78.35 |
实施例8 | 79.01 |
实施例9 | 81.60 |
表4结果可知,本发明的面膜可以有效抑制酪氨酸酶活性,达到美白肌肤的效果。本发明具有祛痘功效的美白保湿面膜具有良好的祛痘与美白保湿功效。
Claims (6)
1.一种具有祛痘功效的美白保湿面膜的制备方法,其特征在于,包括以下步骤:取祛痘精华液、秦艽叶提取物、海藻糖、γ-聚谷氨酸、角鲨烷加入到水中混合均匀,均质处理;冷却至室温,得到面膜液;将面膜液灌入到含有面膜载体的面膜袋内,真空封口,即得;
所述祛痘精华液由以下质量百分比的物质组成:1-4%烟酰胺、5-10%沙棘油、1-8%赤藓醇、3-5%芦荟胶、2.0-3.8%甘油、0.25-0.4%山嵛醇、0.15-0.24% 1,2-己二醇、0.03-0.06%维生素E、1-4%柠檬酸、0.1-3%聚合杏仁蛋白、0.05-0.2%透明质酸钠、0.07-0.1%乙二胺四乙酸二钠、1-5%凝血酸、0.13-0.25%熊果素、0.08-0.12%水溶性氮酮、0.01%-0.08% O-伞花烃-5-醇、0.15-0.25%尿囊素、0.05-0.2%生育酚乙酸酯、10-35%祛痘组合物、5-20%修复剂、余量为水;
所述祛痘组合物的制备方法如下:
S1、将质量比为(1-10):(1-10):(1-8):(1-8):(1-8)的北苍术、母菊花、三色堇菜、台湾山芙蓉、苦参根混合,粉碎,过10-40目筛,得到混合粉末;
S2、将混合粉末与60-80wt%乙醇水溶液按质量比1:(1-5)混合,置于带有氮气保护的回流装置中,在80-90℃下回流4-8h,冷却至室温后抽滤,保留滤液A,滤饼置于60-80℃下真空干燥4-10h后,备用;
S3、将步骤S2干燥后的滤饼加入超临界CO2萃取釜,通入液态CO2,
流量为1-4mL/min,同时通入50-80wt%乙醇水溶液作为夹带剂,流量为0.1-0.4mL/min,在40-60℃、压力20-40MPa下萃取1-3h,得萃取物,合并萃取物和滤液A,得到滤液B;
S4、将滤液B在50-70℃、-0.01--0.1MPa旋转蒸发至体积为原体积的8%-20%,获得浓缩液;将浓缩液冷却至0-8℃,离心取上清液,将上清液用500-2000目滤布过滤,保留滤液,即祛痘组合物;
所述修复剂为苜蓿多糖或改性苜蓿多糖;所述改性苜蓿多糖中采用的改性剂为苏氨酸和/或谷氨酸。
2.如权利要求1所述的具有祛痘功效的美白保湿面膜的制备方法,其特征在于,包括以下步骤:取55-60重量份祛痘精华液、3-5重量份秦艽叶提取物、1-3重量份海藻糖、1-3重量份γ-聚谷氨酸、2-4重量份角鲨烷加入到30-35重量份水中混合均匀,然后高压均质处理15-20min,冷却至室温,得到面膜液;将面膜液灌入到含有面膜载体的面膜袋内,每袋灌装15-20g,真空封口,即得。
3.如权利要求1或2所述的具有祛痘功效的美白保湿面膜的制备方法,其特征在于,所述秦艽叶提取物的制备方法如下:将晾干的秦艽叶粉碎,得到秦艽叶粉;取秦艽叶粉加入水中微波处理0.5-1h,料液比为1kg:(10-15)L,微波功率为600-700W;再加入秦艽叶粉质量10-30wt%的苹果酸,在90-100℃回流提取2-3h;冷却至室温,过滤,将滤液pH调至中性,冻干,即得。
4.如权利要求1所述的具有祛痘功效的美白保湿面膜的制备方法,其特征在于,所述苜蓿多糖的制备方法如下:
X1、将苜蓿草在90-110℃干燥3-5h,粉碎,过5-30目筛,得到苜蓿粉末,按质量比1:(15-25)将苜蓿粉末与水混合均匀,在80-100℃下提取1-3h,过滤,得到滤液Ⅰ和滤渣Ⅰ,在滤渣Ⅰ中加水,所述滤渣Ⅰ和水的质量比为1:(10-20),在80-100℃下加热0.5-2h,过滤,得二次滤液和滤渣Ⅱ,合并滤液Ⅲ;
X2、将X1中的滤液Ⅲ置于50-80℃、-0.01~-0.1MPa蒸发浓缩至原体积的10-30%,得浓缩液,在浓缩液中加入3-6倍质量的无水乙醇进行醇析,静置8-14h,在4000rpm下离心10min,弃上清液,得粗多糖,加入粗多糖质量5倍的水,得到粗多糖溶液;
X3、将上述粗多糖溶液置于0-8℃环境中,用截留分子量为500-2000Da的透析袋透析20-30h,每隔2-4h更换水,收集透析液A,加入透析液A质量相等的三氯甲烷,置于0-8℃沉淀8-16h,离心,取上清液,在上清液中加入5-8倍质量的无水乙醇进行醇析,静置8-14h,在4000rpm下离心10min,将固体冷冻干燥,得苜蓿多糖。
5.如权利要求1所述的具有祛痘功效的美白保湿面膜的制备方法,其特征在于,所述改性苜蓿多糖的制备方法如下:
X1、将苜蓿草在90-110℃干燥3-5h,粉碎,过5-30目筛,得到苜蓿粉末,按质量比1:(15-25)将苜蓿粉末与水混合均匀,在80-100℃下提取1-3h,过滤,得到滤液Ⅰ和滤渣Ⅰ,在滤渣Ⅰ中加水,所述滤渣Ⅰ和水的质量比为1:(10-20),在80-100℃下加热0.5-2h,过滤,得二次滤液和滤渣Ⅱ,合并滤液Ⅲ;
X2、将X1中的滤液Ⅲ置于50-80℃、-0.01~-0.1MPa蒸发浓缩至原体积的10-30%,得浓缩液,在浓缩液中加入3-6倍质量的无水乙醇进行醇析,静置8-14h,在4000rpm下离心10min,弃上清液,得粗多糖,加入粗多糖质量5倍的水,得到粗多糖溶液;
X3、将上述粗多糖溶液置于0-8℃环境中,用截留分子量为500-2000Da的透析袋透析20-30h,每隔2-4h更换水,收集透析液A,加入透析液A质量相等的三氯甲烷,置于0-8℃沉淀8-16h,离心,取上清液,在上清液中加入5-8倍质量的无水乙醇进行醇析,静置8-14h,在4000rpm下离心10min,将固体冷冻干燥,得苜蓿多糖;
X4、将X3中的苜蓿多糖与改性剂按质量比(4-10):1混合均匀,加入苜蓿多糖质量的4-10倍的水,在60-80℃回流加热4-7h,得改性多糖水溶液;再用截留分子量为500-2000Da的透析袋透析20-30h,收集透析液B,冷冻干燥,得改性苜蓿多糖。
6.一种具有祛痘功效的美白保湿面膜,采用如权利要求1-5任一项所述方法制备而成。
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