CN115300435A - 一种祛斑保湿精华液及其制备方法 - Google Patents
一种祛斑保湿精华液及其制备方法 Download PDFInfo
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- CN115300435A CN115300435A CN202211154156.6A CN202211154156A CN115300435A CN 115300435 A CN115300435 A CN 115300435A CN 202211154156 A CN202211154156 A CN 202211154156A CN 115300435 A CN115300435 A CN 115300435A
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- essence
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- cumin
- freckle
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Abstract
本发明公开了一种祛斑保湿精华液及其制备方法。本发明制备的祛斑精华液包括以下重量份数的原料:乌拉尔甘草‑孜然复合物0.3~0.5份,甘油0.3~0.6份,乙二胺四乙酸二钠0.1~0.15份,透明质酸0.05~0.1份,羧甲基纤维素钠0.1~0.2份,三乙醇胺1.0~1.5份,水杨酸0.1~0.2份,维生素C 0.1~0.2份,水溶性氮酮0.1~0.2份,香精0.0001~0.0005份,防腐剂0.2~0.3份,多元醇8~10份,增稠剂0.1~0.5份,水60~90份。与现有技术相比,本发明所制备的祛斑保湿精华液成分安全,温和无刺激,且稳定性良好,在润泽肌肤的同时还能够达到祛斑效果。
Description
技术领域
本发明涉及化妆品技术领域,尤其涉及一种祛斑保湿精华液及其制备方法。
背景技术
近几年,随着经济与技术不断进步,消费者对功能性化妆品的需求也日渐旺盛,尤其是美白祛斑类化妆品市场增长迅速。皮肤中的色素主要有黑褐色的黑色素、红色的血红素和黄色的胡萝卜素,其中黑色素是决定皮肤颜色最主要的因素。皮肤颜色深浅会受到多种因素的影响,但主要是由于细胞黑色素的量和分泌黑素颗粒的数量、大小、分布、黑色化程度等等。黑色素细胞是位于表皮的基底层,是皮肤里面一种非常特殊的细胞,它约占基底层细胞10%的总含量。由于外界不同外源和内源的因素,会促使黑色素细胞产生黑色素,从而传递给周围的角质形成细胞,一个黑色素细胞周围通常会分布着30~40个角质形成细胞,而黑色素细胞与周围角质形成细胞最终构成了一个黑色素形成单元。通常皮肤中的黑色素细胞会以酪氨酸酶为自有底物,在多种酶的氧化作用下生成黑色素,也就是非常熟悉的转化流程:酪氨酸-多巴-多巴醌-多巴色素-二羟基吲哚-酮式吲哚-黑色素,最终所形成的黑色素颗粒再由黑色素细胞树突转运至皮肤表皮层的基底层细胞,进一步随着细胞新陈代谢而被带到角质层,最终导致皮肤色沉暗淡,或者形成雀斑、晒斑、黑斑等。
参与黑色素形成的生物酶多种多样,其中酪氨酸酶是黑色素合成中的主要核心生物酶,目前主流的美白祛斑作用机制主要包括:抑制酪氨酸酶活性,氧化反应抑制剂及促进黑色素代谢。抑制酪氨酸酶活性的策略通常为合成与酪氨酸酶的底物例如酪氨酸或多巴在化学结构上有许多相似性的化合物,从而在进行化学反应时能够与酪氨酸酶分子进行竞争,使得酪氨酸酶的活性受到抑制,常选用的原料包括氢醌、熊果苷等,但这些成分安全性较差,对人体有刺激;氧化反应抑制剂则是通过将黑色素转换成无色的前体物质而减少黑色素沉着,常选择的成分包括维生素C、维A醇等,但这些原料性质较为活泼,容易变质;而促进黑色素新陈代谢则是采用剥脱、去角质等方式加速老化角质细胞的脱落,实现黑色素代谢加速,典型代表原料有水杨酸、果酸等,值得注意的是这类物质会对皮肤屏障产生一定影响,甚至导致皮肤敏感发红。
专利CN108042425 B中公开了一种美白保湿精华液及其制备方法,主要由去离子水、霍霍巴油、熊果苷、壬二酸氨基酸钾盐、羟苯甲酯、辛基聚甲基硅氧烷、甘油、丙二醇、水溶性神经酰胺、透明质酸钠、苯氧乙醇、三乙醇胺、卡波姆、天然植物精华提取物等原料制备而成。专利CN105456109 A中公开了一种美白乳液,包括如下原料:去离子水50-70份、椰子汁15-25份、抗氧化剂1-3份、奇异果萃取物15-25份、水杨酸5-15份、抗菌肽6-8份、甜杏仁油5-15份、果酸1-3份。目前涉及到的美白祛斑保湿产品大多采用的熊果苷或者水杨酸等刺激性较强的成分,长期使用可能导致皮肤屏障受损从而皮肤变得敏感甚至红肿。因此,研发出一种成分温和无刺激,且性质稳定的美白祛斑保湿产品将具有十分广阔的市场前景。
发明内容
有鉴于现有技术的上述缺陷,本发明所要解决的技术问题是目前制备的祛斑保湿精华成分容易失活稳定性较差,以及对皮肤刺激性较强。本发明的目的在于提出一种成分温和,稳定性高,安全有效的祛斑保湿精华的制备方法。
本发明的技术方案:
一种祛斑保湿精华液,由以下原料组成:甘油,乙二胺四乙酸二钠,透明质酸,羧甲基纤维素钠,三乙醇胺,水杨酸,维生素C,水溶性氮酮,香精,防腐剂,多元醇,增稠剂,水。
优选的,所述祛斑保湿精华液,包括以下重量份数的原料:甘油0.3~0.6份,乙二胺四乙酸二钠0.1~0.15份,透明质酸0.05~0.1份,羧甲基纤维素钠0.1~0.2份,三乙醇胺1.0~1.5份,水杨酸0.1~0.2份,维生素C 0.1~0.2份,水溶性氮酮0.1~0.2份,香精0.0001~0.0005份,防腐剂0.2~0.3份,多元醇8~10份,增稠剂0.1~0.5份,水60~90份。
孜然富集多种生物活性成分,相关研究已经证实孜然中有100多种化合物。研究表明,干燥的孜然种子中含有挥发油(5%)、脂肪(22%)、蛋白质(10%)、糖类、纤维(11%)、游离氨基酸和多种微量元素。孜然种子富含黄酮和多酚类物质,其中包括没食子酸,肉桂酸,迷迭香酸,香豆酸和香草酸,木犀草素,儿茶素,香豆素,槲皮素和槲皮素等。孜然非精油组分中主要有萜、倍半萜、芳香族醛、酮醚类物质。主要包括枯茗醛、枯茗醇、对伞花烃、β-蒎烯、α-蒎烯、γ-萜品烯、水芹烯、月桂烯、松油烯、藏花醛、柠檬烯等多种化学物质,其中枯茗醛的含量最高。其中黄酮类及多酚类由于含有丰富的羟基、酚羟基等活性官能团,因而具有强大的抗氧化性,通过对氧自由基或激发态氧的直接清除、抑制氧化酶的活性以及对金属离子的螯合作用均可以达到很好的抗氧化活性。
乌拉尔甘草,甘草中主要含三菇类、黄酮类和多糖类化合物,另外还含有香豆素类、氨基酸类、生物碱、性激素和有机酸等100多种有效化学成分。三菇类化合物主要含甘草甜素、甘草次酸、甘草菇醇、异甘草内脂、齐墩果酸等。黄酮类化合物主要含甘草苷、甘草苷元、异甘草苷、异甘草素(异甘草苷元)、甘草素(甘草苷元)、新异甘草苷、异芒柄花苷、新甘草酚、甘草黄酮A和甘草查尔酮A、B。生物碱类化合物包括四氢喹啉化合物:5,6,7,8-四氢-2,4-二甲基喹啉,5,6,7,3-四氢-4-甲基喹啉。异甘草素作为甘草黄酮中活性最高的成分,由于其结构本身所含有的丰富的酚羟基具有极强的酪氨酸酶抑制活性。
进一步的,所述祛斑保湿精华液,包括以下重量份数的原料:孜然提取物0.3~0.5份,乌拉尔甘草提取物0.4~0.6份,甘油0.3~0.6份,乙二胺四乙酸二钠0.1~0.15份,透明质酸0.05~0.1份,羧甲基纤维素钠0.1~0.2份,三乙醇胺1.0~1.5份,水杨酸0.1~0.2份,维生素C 0.1~0.2份,水溶性氮酮0.1~0.2份,香精0.0001~0.0005份,防腐剂0.2~0.3份,多元醇8~10份,增稠剂0.1~0.5份,水60~90份。
优选的,所述祛斑保湿精华液,包括以下重量份数的原料:孜然-乌拉尔甘草复合物0.4~0.6份,甘油0.3~0.6份,乙二胺四乙酸二钠0.1~0.15份,透明质酸0.05~0.1份,羧甲基纤维素钠0.1~0.2份,三乙醇胺1.0~1.5份,维生素C 0.1~0.2份,水溶性氮酮0.1~0.2份,香精0.0001~0.0005份,防腐剂0.2~0.3份,多元醇8~10份,增稠剂0.1~0.5份,水60~90份。
所述孜然提取物由如下方法制备得到:称取孜然种子200~400g粉碎,过50~60目筛,按照料液比1:(10~15)g/mL加入体积分数为60~70%的乙醇水溶液,于70~80℃下提取2~3h,提取液经4000~5000rpm转速离心10~20min,上清液于40~50℃下旋转蒸发浓缩至干,得孜然提取物。
所述乌拉尔甘草提取物由如下方法制备得到:将500~600g乌拉尔甘草根洗净后粉碎,过60~80目筛,加入0.5~1mol/L的HCl水溶液,料液比为1:(5~10)g/mL,在90~100℃下水解2~3h,用0.5~1mol/L的NaOH水溶液调节pH至中性,过滤,滤渣加入5~6L体积分数70~80%的乙醇水溶液进行超声提取20~30min,超声功率400~500W,频率30~40Hz,提取液经于45~50℃旋转蒸发浓缩至干,得乌拉尔甘草提取物。
所述孜然-乌拉尔甘草复合物由如下方法制备得到:取30~50g孜然提取物,40~60g乌拉尔甘草提取物加入到1~2L体积分数70~80%的乙醇水溶液中,加入5~10g水杨酸,在20~30℃下搅拌1~2h,经乙酸乙酯萃取2~4次后,合并萃取液,于40~50℃下旋转蒸发浓缩至干,得孜然-乌拉尔甘草复合物。
优选的,所述多元醇为1,2-丙二醇和/或丁二醇。更优选的,所述1,2-丙二醇及丁二醇的重量比为(0.75~1):1。
优选的,所述增稠剂为卡波姆和/或聚乙烯醇。
优选的,所述防腐剂为尼泊金乙酯,卡松,苯氧乙醇中的至少一种。更优选的,所述尼泊金乙酯和卡松的重量比为(0.1~0.15):0.1。
优选的,所述香精为香豆素。
尼泊本发明还提供了上述祛斑保湿精华液的制备方法,包括如下步骤:
S1取配方量的卡波姆加入20~30重量份水中溶胀,再加入多元醇,甘油,透明质酸,羧甲基纤维素钠,于80~90℃下搅拌1~2h;取配方量的尼泊金乙酯,卡松,乙二胺四乙酸二钠和乌拉尔甘草-孜然提取复合物加入20~30重量份水中,于80~90℃下搅拌溶解后加入到卡波姆的水溶液中,于80~90℃下搅拌10~30min;
S2取配方量的水杨酸、维生素C溶于20~30重量份水中并混合均匀;
S3将步骤S1与S2中的最终混合溶液混合均匀,于60~70℃下加入三乙醇胺;
S4将步骤S3得到的混合溶液降温至40~50℃后加入配方量的水溶性氮酮和香豆素,充分混合即得祛斑保湿精华。
本发明提供了一种祛斑保湿精华的制备方法。与现有技术相比,本发明解决了现有技术中遇到的困难,具有如下有益效果:
(1)本发明制备的祛斑保湿精华配方简单,原料成本低,且制备方法简单,条件易控,工艺稳定,可工业化生产,能够推广应用;
(2)本发明中的祛斑保湿精华可很好地润养肌肤,保持肌肤的水分,且pH值为弱酸性,能够温和地护理皮肤,不会产生刺激性反应;
(3)本发明中的祛斑保湿精华使用了乌拉尔甘草提取物与孜然提取物进行混合,孜然提取物中的枯茗醛与甘草中酸水解后产生的异甘草素进行结合,增加了黄酮类化合物的含量,结合后形成共轭烯烃结构且酚羟基不会受到影响,结构稳定的同时活性更强,在抑制酪氨酸酶活性及黑色素合成方面具有很好的效果,能够很好地焕亮肌肤,同时由于其保湿和祛斑效果俱佳,成分温和刺激性低,因此将具有良好的市场前景和推广价值。
具体实施方式
下面对本发明实施例中的技术方案进行清楚、完整地描述。以下实施例用于说明本发明,但不用来限制本发明的范围。实施例中涉及的操作如无特殊说明,均为本领域常规技术操作。
本发明实施例中部分原料参数如下:
卡波姆-940,CAS号:9007-20-9,来源于固安希星药业有限公司。
水溶性氮酮,CAS号:59227-89-3,来源于西安交大科创药业有限责任公司。
卡松,CAS号:26172-55-4,来源于湖北齐飞医药化工有限公司。
对比例1
一种祛斑保湿精华液的制备,包括如下步骤:
S1取卡波姆0.3g加入20mL水溶胀,再加入1,2-丙二醇3g,丁二醇5g,甘油0.5g,透明质酸0.1g,羧甲基纤维素钠0.1g于90℃下搅拌2h;取尼泊金乙酯0.15g,卡松0.1g,乙二胺四乙酸二钠0.1g加入到20mL水中,于90℃下搅拌溶解后加入到上述卡波姆与水的混合物中,于90℃下搅拌10min;
S2取维生素C 0.2g,水杨酸0.2g溶于30mL水中混合均匀;
S3将步骤S1与S2中的最终混合溶液混合均匀,于60℃下加入1.0g的三乙醇胺;
S4将步骤S3得到的混合溶液降温至40℃下加入水溶性氮酮0.1g和香豆素0.0005g,充分混合即得祛斑保湿精华液。
对比例2
一种祛斑保湿精华液的制备,包括如下步骤:
S1取卡波姆0.3g加入20mL水溶胀,再加入1,2-丙二醇3g,丁二醇5g,甘油0.5g,透明质酸0.1g,羧甲基纤维素钠0.1g,于90℃下搅拌2h;取尼泊金乙酯0.15g,卡松0.1g,乙二胺四乙酸二钠0.1g和乌拉尔甘草-孜然复合物0.4g加入到20mL水中,于90℃下搅拌溶解后加入到上述卡波姆与水的混合物中,于90℃下搅拌10min;
S2取维生素C 0.2g,水杨酸0.2g溶于30mL水中混合均匀;
S3将步骤S1与S2中的最终混合溶液混合均匀,于60℃下加入1.0g的三乙醇胺;
S4将步骤S3得到的混合溶液降温至40℃下加入水溶性氮酮0.1g、卡松0.1g和香豆素0.0005g,充分混合即得祛斑保湿精华液。
所述乌拉尔甘草-孜然复合物采用如下方法制备:
(1)称取孜然种子200g粉碎,过60目筛,加入3L体积分数为70%的乙醇水溶液,于70℃下提取2h,提取液经4000rpm转速离心10min,上清液于50℃下浓缩至干,得孜然提取物;
(2)将500g乌拉尔甘草根洗净后粉碎,过60目筛,加入3L 0.5mol/L的HCl溶液,在90℃下水解2h,用0.5mol/L的NaOH溶液调节pH至中性,过滤,滤渣加入5L体积分数80%的乙醇溶液进行超声提取20min,超声功率400W,频率40Hz,提取液在50℃浓缩至干得乌拉尔甘草提取物;
(3)取30g孜然提取物,40g乌拉尔甘草提取物加入到1L体积分数80%的乙醇溶液中,加入5g水杨酸,在20℃下搅拌2h,用500mL*3乙酸乙酯萃取,合并萃取液,于45℃下浓缩至干,得孜然-乌拉尔甘草复合物。
实施例1
一种祛斑保湿精华液的制备,包括如下步骤:
S1取卡波姆0.3g加入20mL水溶胀,再加入1,2-丙二醇3g,丁二醇5g,甘油0.5g,透明质酸0.1g,羧甲基纤维素钠0.1g于90℃下搅拌2h;取尼泊金乙酯0.15g,卡松0.1g,乙二胺四乙酸二钠0.1g和孜然提取物0.4g加入到20mL水中,于90℃下搅拌溶解后加入到上述卡波姆与水的混合物中,于90℃下搅拌10min;
S2取维生素C 0.2g,水杨酸0.2g溶于30mL水中混合均匀;
S3将步骤S1与S2中的最终混合溶液混合均匀,于60℃下加入1.0g的三乙醇胺;
S4将步骤S3得到的混合溶液降温至40℃下加入水溶性氮酮0.1g和香豆素0.0005g,充分混合即得祛斑保湿精华液。
所述孜然提取物采用如下方法制备:称取孜然种子200g粉碎,过60目筛,加入3L体积分数为70%的乙醇水溶液,于70℃下提取2h,提取液经4000rpm转速离心10min,上清液于50℃下浓缩至干,得孜然提取物。
实施例2
一种祛斑保湿精华液的制备,包括如下步骤:
S1取卡波姆0.3g加入20mL水溶胀,再加入1,2-丙二醇3g,丁二醇5g,甘油0.5g,透明质酸0.1g,羧甲基纤维素钠0.1g于90℃下搅拌2h;取尼泊金乙酯0.15g,卡松0.1g,乙二胺四乙酸二钠0.1g和乌拉尔甘草-孜然复合物0.4g加入到20mL水中,于90℃下搅拌溶解后加入到上述卡波姆与水的混合物中,于90℃下搅拌10min;
S2取维生素C 0.2g,水杨酸0.2g溶于30mL水中混合均匀;
S3将步骤S1与S2中的最终混合溶液混合均匀,于60℃下加入1.0g的三乙醇胺;
S4将步骤S3得到的混合溶液降温至40℃下加入水溶性氮酮0.1g、和香豆素0.0005g,充分混合即得祛斑保湿精华液。
所述乌拉尔甘草-孜然复合物采用如下方法制备:
(1)称取孜然种子200g粉碎,过60目筛,加入3L体积分数为70%的乙醇水溶液,于70℃下提取2h,提取液经4000rpm转速离心10min,上清液于50℃下浓缩至干,得孜然提取物;
(2)将500g乌拉尔甘草根洗净后粉碎,过60目筛,加入3L 0.5mol/L的HCl水溶液,在90℃下水解2h,用0.5mol/L的NaOH水溶液调节pH至中性,过滤,滤渣加入5L体积分数80%的乙醇水溶液进行超声提取20min,超声功率400W,频率40Hz,提取液在50℃下浓缩至干,得乌拉尔甘草提取物;
(3)取30g孜然提取物,40g乌拉尔甘草提取物加入到1L无水甲醇中,再加入25wt%的NaOH水溶液100mL,避光,在50℃下搅拌50h,静置10min,加入2mol/L HCl水溶液调节pH至中性,再加入500mL乙酸乙酯萃取,萃取液再用400mL*3水洗三次,于45℃下除去乙酸乙酯后得到粗产物,进一步加入100mL甲苯洗涤,100mL*3水洗3次除去甲苯,经60℃真空干燥得乌拉尔甘草-孜然提取复合物。
在弱碱性条件下,孜然提取物中的醛类如枯茗醛可与甘草提取物酸水解后的异甘草素进行偶联,形成不饱和的共轭双键,所形成的黄酮类化合物结构更为稳定,且由于共轭双键的加持活性更高。同时本发明将孜然提取物中无抗氧化活性的醛类利用起来,增强了复配物的抗氧化活性,将其运用到化妆品中可显著提升产品的抗氧化活性,祛斑功效也将得到显著提升。
实施例3
一种祛斑保湿精华液的制备,包括如下步骤:
S1取卡波姆0.3g加入20mL水溶胀,再加入1,2-丙二醇3g,丁二醇5g,甘油0.5g,透明质酸0.1g,羧甲基纤维素钠0.1g于90℃下搅拌2h;取尼泊金乙酯0.15g,卡松0.1g,乙二胺四乙酸二钠0.1g和乌拉尔甘草提取物0.4g加入到20mL水中,于90℃下搅拌溶解后加入到上述卡波姆与水的混合物中,于90℃下搅拌10min;
S2取维生素C 0.2g,水杨酸0.2g溶于30mL水中混合均匀;
S3将步骤S1与S2中的最终混合溶液混合均匀,于60℃下加入1.0g的三乙醇胺;
S4将步骤S3得到的混合溶液降温至40℃下加入水溶性氮酮0.1g和香豆素0.0005g,充分混合即得祛斑保湿精华液。
所述乌拉尔甘草提取物采用如下方法制备:将500g乌拉尔甘草根洗净后粉碎,过60目筛,加入3L 0.5mol/L的HCl水溶液,在90℃下水解2h,用0.5mol/L的NaOH水溶液调节pH至中性,过滤,滤渣加入5L体积分数80%的乙醇溶液进行超声提取20min,超声功率400W,频率40Hz,提取液在50℃浓缩至干,得乌拉尔甘草提取物。
测试例1
对对比例1,2及实施例1,2,3进行了抑制酪氨酸酶活性测试,参考(上海日用化学品行业协会团体标准T/SHRH 015-2018)中的测试方法进行测试。具体步骤为:设立样品管(T)、样品本底(T0)、酶反应管(C)和溶剂本底(C0),每组设立三支平行管。在样品管(T)和样品本底(T0)中各加入1mL相同浓度的样品溶液,酶反应管(C)和溶剂本底(C0)则分别加入1mL磷酸盐缓冲溶液,在样品管和酶反应管中各加入0.5mL酪氨酸酶溶液,样品本底和溶剂本底则以0.5mL磷酸盐缓冲溶液代替,混匀,在35℃下孵育10min,依次在各管中加入2mL的左旋多巴溶液,控制没管反应时间为5min,迅速转移至比色皿中,立即用紫外可见分光光度计于475nm处测定各样品的反应溶液的吸光度,再计算出抑制率。
抑制率(%)=(1-(T-T0)/(C-C0))*100%
T—样品管吸光值,即样品与酪氨酸酶反应后溶液吸光值;
T0—样品本底吸光值;
C—未加样品时酪氨酸酶和多巴反应的吸光值;
C0—溶剂本底吸光值。
表1-抑制酪氨酸酶活性的抑制率结果表
实验方案 | 抑制率/% |
对比例1 | 47.95% |
对比例2 | 75.31% |
实施例1 | 53.67% |
实施例2 | 85.43% |
实施例3 | 56.31% |
由表1可知,乌拉尔甘草及孜然提取物均可提高精华液对于酪氨酸酶的活性,然而二者复合后抑制效果更为明显,实施例2相对于对比例2而言孜然-乌拉尔甘草提取物复配采用的是碱性条件下发生C-C偶联反应,这种结合更为紧密,所生成的复合物具有黄酮类结构,共轭双键和丰富的酚羟基使得其的抗氧化能力更强,因此对于酪氨酸酶催化活性有更好的抑制效果,酪氨酸酶是黑色素生物合成过程中的第一限速酶,对其的抑制效果越好即可以越好地抑制黑色素的合成从而达到祛斑,提亮肤色的功效。
测试例2
对对比例1,2及实施例1,2,3进行了抑制黑色素合成的活性测试,黑色素是由黑色素细胞产生的一种生物色素,广泛存在于人的皮肤,头发和视网膜等,正常含量的黑色素能够帮助皮肤免受紫外线的伤害,但黑色素分泌过多,会导致皮肤色素沉着过度,容易引起雀斑、黄褐斑和皮肤癌等。因此,抑制黑色素的生成或是加速已有黑色素的分解对改善肤色问题是至关重要的。测试方法参考T/ZHCA012-2020《化妆品美白功效测试斑马鱼胚胎黑色素抑制功效测试方法》团体标准,“水中小白鼠”斑马鱼,作为一种与人类基因相似度高达87%的模式生物,以斑马鱼胚胎为基础的实验结果一般情况下均适用于人体,斑马鱼在发育初期全身透明,胚胎发育至24h事黑色素开始从视网膜上皮生长。色素细胞起源于背部外胚层分化的神经嵴细胞,然后增值、迁徙、分化成色素母细胞。用受试物干预斑马鱼的黑色素形成过程,可抑制黑色素的形成,通过与正常对照组的比较可以计算受试物对于黑色素的抑制效率。选取发育正常的6hpf的斑马鱼胚胎,放入六孔板中,每孔15枚,在不伤害胚胎的情况下除去六孔板中的标准稀释水,向每孔中迅速加入3mL受试物溶液。孵育结束后,从表型和行为正常的斑马鱼中随机选取至少12尾斑马鱼,用3#甲基纤维素固定,在体视显微镜下观察并拍照,所有斑马鱼拍照时体位保持一致。照片使用图像分析软件进行分析,选取定量区域为斑马鱼头部边缘(除眼睛部分)至与卵黄囊相切部分。将分析参数校准为OD值,以此来计算斑马鱼头部黑色素信号强度,每组的有效数据不少于10个。将黑色素信号强度记为S,计算受试物的祛斑作用即黑色素抑制率,公式如下:
黑色素抑制率%=(S(正常对照组)-S(供试品组))/S(正常对照组)
表2-黑色素抑制功效测试结果表
实验方案 | 黑色素抑制率/% |
对比例1 | 51.34% |
对比例2 | 76.71% |
实施例1 | 61.54% |
实施例2 | 87.15% |
实施例3 | 68.95% |
酪氨酸酶是黑色素合成过程中的关键酶,抑制酪氨酸酶活性,可以直接抑制黑色素的合成,然而黑色素是由黑色素细胞分泌产生的,抑制黑色素细胞的增殖,能直接减少黑色素的生成,因此,抑制黑色素的生成或是加速已有黑色素的分解对改善肤色问题的效果更为直接。由表可知,在孜然提取物和乌拉尔提取物进行复合后,由于黄酮类化合物含量的增加,其清除自由基和抑制酪氨酸酶的活性能力均有提升,自由基可以上调酪氨酸酶mRNA的表达,使酪氨酸酶的活性增强,因此,清除氧自由基,也会间接抑制酪氨酸酶的催化活性,抑制黑色素的生成,实施例2中的复合物中形成的黄酮类物质由于其独特的结构,与酪氨酸酶活性中心的金属离子的螯合能力也大大增强,可以与底物竞争结合酪氨酸酶,因此会阻止酪氨酸酶催化氧化酪氨酸的过程,减少黑色素的生成。
测试例3
邀请健康志愿者30人,在手臂上试用对比例1,2及实施例1,2,3中的精华液,对比使用28天前后的皮肤状况,测试方法参考文献(王鹏,一款美白产品的功效与研究,科技广场,2020(43):36-43)中的标准进行测试。具体步骤为在志愿者前臂曲侧随机选定产品涂抹区和空白对照区,在涂抹区使用美白化妆品,要求产品涂抹均匀。志愿者按2mg/cm2的使用量于每日早晚各涂1次,使用周期为8周。在测试周期内,受试部位不使用其他任何化妆品。采用皮肤测试仪测试志愿者使用产品前后皮肤的对比情况。具体数据见表3:
表3-人体试验结果表
皮肤黑色素含量MI值,表征黑素指数,MI值越大皮肤黑色素含量越高;皮肤亮度L*值,表征皮肤亮度,其变化表示皮肤黑白色度的变化,其值越大,颜色越偏向白色;ITA值(个体类型角)表征皮肤明亮度,ITA值越大,皮肤越明亮,反之,皮肤越晦暗。测量皮肤角质层的电容量来反映人体皮肤角质层的水分含量,测得的值越大表征皮肤角质层水分含量越高,保湿效果越好。样品组在实验周期内皮肤黑色素含量MI值、皮肤亮度L值、ITA值和角质层水分含量均有不同程度的改善,表现出了祛斑和保湿的效果。由表可知,实施例2,对比例2相较于其他例中的精华液表现出了良好的祛斑效果,实施例2由于所生成的活性物质有更为优异的抑制酪氨酸酶活性及清除自由基的功效,因此对于皮肤的整体提亮效果更为卓越,且本发明制备的精华液保湿效果良好,能适应更多地区及人群的使用。
测试例4
对对比例1,2及实施例1,2,3进行稳定性实验,测试标准参考(化妆品稳定性试验指导原则T/SHFCA 002-2021)中的标准进行测试。具体步骤为样品分别在温度54℃、相对湿度75%、避光条件及﹣5℃左右、避光的条件下循环放置7天,进行耐热耐寒交替实验,分别检测样品的色泽、香味、状态、pH值和是否有分层现象。具体结果见表4:
表4-稳定性实验结果
色泽 | 香味 | 状态 | pH | 是否分层 | |
对比例1 | 无色透明 | 没有明显香味 | 粘稠状,底部有沉淀 | 4.1 | 是 |
对比例2 | 无色透明 | 特殊香味,香气宜人 | 流动状 | 6.5 | 否 |
实施例1 | 淡黄色 | 具有孜然辛香 | 粘稠状,底部无沉淀 | 5.5 | 是 |
实施例2 | 淡黄色 | 特殊香味,香气宜人 | 流动状 | 6.5 | 否 |
实施例3 | 淡黄色 | 气味甘甜 | 粘稠状,底部无沉淀 | 5.7 | 是 |
由表可知,乌拉尔甘草的添加可赋予精华液宜人的香气,孜然的辛香和其结合,则使得香味更为浓烈,且相较于对比例1中普通的祛斑产品,本发明中的祛斑保湿精华液呈弱酸性,对于肌肤刺激性小。在稳定性实验中,由于产物本身的性质导致在极端条件下产品出现性状变化或分层等现象,这可能导致祛斑精华失效甚至变质。然而,实施例2中由于孜然提取物和乌拉尔甘草提取物的复合采用的是更为紧密的化学键结合方式,因此稳定性强,不会轻易发生失效甚至变质的情况。本发明所制备的祛斑保湿精华液pH符合国家化妆品行业标准要求范围,温和不刺激,安全无毒无副作用,且耐寒、耐热,稳定性较好。
Claims (10)
1.一种祛斑保湿精华液,其特征在于,包括以下原料组成:甘油,乙二胺四乙酸二钠,透明质酸,羧甲基纤维素钠,三乙醇胺,水杨酸,维生素C,水溶性氮酮,香精,防腐剂,多元醇,增稠剂,水。
2.如权利要求1所述的一种祛斑保湿精华液,其特征在于,由以下原料组成:乌拉尔甘草-孜然复合物,甘油,乙二胺四乙酸二钠,透明质酸,羧甲基纤维素钠,三乙醇胺,水杨酸,维生素C,水溶性氮酮,香精,防腐剂,多元醇,增稠剂,水。
3.如权利要求2所述的一种祛斑保湿精华液,其特征在于,由以下重量份原料组成:乌拉尔甘草-孜然复合物0.3~0.5份,甘油0.3~0.6份,乙二胺四乙酸二钠0.1~0.15份,透明质酸0.05~0.1份,羧甲基纤维素钠0.1~0.2份,三乙醇胺1.0~1.5份,水杨酸0.1~0.2份,维生素C 0.1~0.2份,水溶性氮酮0.1~0.2份,香精0.0001~0.0005份,防腐剂0.2~0.3份,多元醇8~10份,增稠剂0.1~0.5份,水60~90份。
4.如权利要求2或3所述的一种祛斑保湿精华液,其特征在于,所述乌拉尔甘草-孜然复合物的制备方法如下:取孜然提取物,乌拉尔甘草提取物加入到体积分数70~80%的乙醇水溶液中,加入水杨酸,在20~30℃下搅拌1~2h,经乙酸乙酯萃取2~4次,合并萃取液,浓缩至干,得孜然-乌拉尔甘草复合物。
5.如权利要求4所述的一种祛斑保湿精华液,其特征在于,所述孜然提取物的制备方法如下:称取孜然种子,粉碎,过筛,加入体积分数为60~70%的乙醇水溶液,于70~80℃下提取2~3h,提取液经4000~5000rpm转速离心10~20min,上清液浓缩至干,60~70℃烘干得孜然提取物。
6.如权利要求4所述的一种祛斑保湿精华液,其特征在于,所述乌拉尔甘草提取物的制备方法如下:将乌拉尔甘草根洗净后粉碎,过筛,加入0.5~1mol/L的HCl水溶液水解2~3h,用0.5~1mol/L的NaOH水溶液调节pH至中性,过滤,滤渣加入体积分数70~80%的乙醇水溶液进行超声提取,提取液浓缩得乌拉尔甘草提取物。
7.如权利要求1~3任一项所述的一种祛斑保湿精华液,其特征在于:所述多元醇为1,2-丙二醇,丁二醇中的至少一种。
8.如权利要求1~3任一项所述的祛斑保湿精华液,其特征在于:所述增稠剂为卡波姆,聚乙烯醇中的至少一种。
9.如权利要求1~3任一项所述的一种祛斑保湿精华液,其特征在于:所述防腐剂为尼泊金乙酯,卡松,苯氧乙醇中的至少一种。
10.如权利要求2~9任一项所述的一种祛斑保湿精华液的制备方法,其特征在于,包括以下步骤:
S1取配方量的增稠剂加入水中溶胀,再加入多元醇,甘油,透明质酸,羧甲基纤维素钠,于80~90℃下搅拌1~2h;取配方量的防腐剂尼泊,乙二胺四乙酸二钠和乌拉尔甘草-孜然复合物加入水中,于80~90℃下搅拌溶解后加入到增稠剂的水溶液中,于80~90℃下搅拌10~30min;
S2取配方量的维生素C、水杨酸溶于水中并混合均匀;
S3将步骤S1与S2中的最终混合溶液混合均匀,于60~70℃下加入配方量的三乙醇胺;
S4将步骤S3得到的混合溶液降温至40~50℃后加入配方量的水溶性氮酮、香豆素,充分混合即得祛斑保湿精华。
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