CN113712843B - 一种美白组合物及含其精华液及该精华液的制备方法 - Google Patents
一种美白组合物及含其精华液及该精华液的制备方法 Download PDFInfo
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Abstract
本发明公开了一种美白组合物及含其精华液及该精华液的制备方法，美白组合物包括组分：二葡糖基棓酸、肌肽、乙酰壳糖胺；精华液包括组分：溶剂、多元醇、舒敏剂、增稠剂、美白组合物、螯合剂、pH调节剂、抑菌剂；精华液的制备方法包括步骤：(1)将抑菌剂、多元醇混合，加热搅拌溶解得到第一混合物；(2)将溶剂、螯合剂及增稠剂依次投入主锅中，加热，均质搅拌溶解；(3)主锅降温加入第一混合物，搅拌溶解；(4)主锅降温，加入多元醇、美白组合物及舒敏剂，搅拌溶解；(5)向主锅中加入pH调节剂，搅拌溶解，得到成品。本发明产品在祛黑祛黄作用方面相互协同，效果显著。
Description
技术领域
本发明涉及化妆品技术领域，尤其涉及一种美白组合物及含其精华液及该精华液的制备方法。
背景技术
黑色素形成并大量分布于角质细胞是皮肤变黑的关键因素，所以减少黑色素是美白之路不可缺少的一部分，其原理主要分为两个部分：1、抑制黑色素合成、转移；2、促进皮肤内已合成黑色素的分解和代谢。
黑色素分解和代谢主要有两条途径：一是黑色素在皮肤内被分解、溶解和吸收后穿透基底膜，被真皮层的嗜黑色素细胞吞噬后，通过淋巴液带到淋巴结再经血液循环从肾脏排出体外；二是黑色素通过黑色素细胞树枝状突起，向角质形成细胞转移，然后随表皮细胞上行至角质层，随老化的角质细胞脱落而排出体外。
黑色素由黑色素细胞合成，而外胚层的神经嵴细胞(CNN)通过增值、迁徙、生存、分化为黑素细胞前体，进而演变为成黑素细胞后到达真皮和表皮、内耳血管纹等，然后发育为黑素细胞。
黑色素细胞中的黑素小体内，由苯丙氨基酸和酪氨酸在酪氨酸酶(TYR)的催化作用下氧化生成多巴醌(DQ)开始，DQ在一系列条件下，分两个方向分别合成真黑素和褐色素。最后真黑素与褐色素合成黑色素。黑色素细胞形成树枝状突起，与周围30～40个角质细胞相触，黑色小体经由树枝状突起转运至周围的角质细胞中，由此完成黑色素的转运、分布。
在抑制黑色素合成方面，抑制酪氨酸酶活性是一条有效途径。而除了抑制酪氨酸酶活性，还可以通过抑制小眼畸形相关转录因子(MITF)的转录活性。
MITF基因成特异性表达于黑素细胞和黑素瘤细胞。MITF蛋白不但在CNN分化为黑素细胞过程中起到重要调控作用，而且是调控酪氨酸酶(TYR)基因家族转录最关键的转录因子。
MITF的表达可以调控黑素细胞的增殖和周期，从而影响黑色素合成含量。研究发现缺乏MITF基因的成黑素细胞在2天之内死亡，这也证实了MITF是成黑素细胞生存必不可少的。
MITF主要通过调控TYR基因家族来控制黑素细胞的生存和分化以及黑色素的合成、转运和分布，它在黑素细胞形态构成、生存、迁徙、增殖和分化的发育过程中有重要作用。
而相对于抑制酪氨酸酶活性，抑制MITF相关基因的表达是一条更高效的路径。
皮肤发黄的主要是因为高级糖基化终末产物和脂褐素的不断累积。
(1)胶原蛋白和弹性蛋白分子中的氨基酸容易与细胞外液中葡萄糖发生非酶糖基化反应，反应生成高级糖基化终末产物(AGEs)，AGEs随年龄的增长进行性增加。AGEs发生褐变后会形成棕黄色的生物垃圾，在真皮层堆积，进而导致皮肤泛黄、暗沉，皮肤视觉效果的剔透感下降。非酶糖基化反应过程中产生一些活性羰基化合物会参与羰基氧化应激反应，产生脂褐素导致肤色暗黄。
(2)过量的自由基将不饱和脂肪酸氧化成过氧化脂质，其终产物丙二醛有很强的交联性质，它与含游离的氨基的磷脂、蛋白质、核酸等生物大分子交联，形成难溶的脂褐素，脂褐素难溶于水，不易被代谢排出，因此随着年龄的增大，脂褐素在细胞内含量增加且有密集和增大的趋势，使得皮肤愈加暗黄。
即皮肤发黄的关键因素高级糖基化终末产物(AGEs)和脂褐素，而导致两个产物产生的主要原因是非酶糖基化反应和过量的自由基与不饱和脂肪酸的氧化反应。
据研究，随着年龄的增加，中国人的皮肤颜色显著变暗且黄色显著增加，由此可知，中国人的皮肤美白重点在于祛黑和祛黄。另一项研究显示，中国女性中，15-20岁、21-25岁、26-35岁女性受到脸色暗黄的皮肤问题困扰的比率分别为32.58％、44.61％、51.52％。所以，开发针对皮肤暗黄的美白化妆品在现实中具有重要意义。
而现有技术中，却鲜有针对祛黄的，宣称美白功效的化妆品所用功效原料大多数以抑制酪氨酸酶活性为机理。该类机理一般只能抑制黑色素生成，提高L*值，祛黑不祛黄，并不能美白整体肤色，尤其是对亚洲人特征性黄色皮肤。此外，该类机理的原料要起到高效整体美白效果，往往需要复配多种不同机理的原料，导致工艺繁琐，徒增成本，且酪氨酸酶抑制剂一般稳定性差，容易变色，影响产品外观。
发明内容
针对现有技术的不足，本发明所解决的技术问题是提供一种祛黑且祛黄美白产品。
为解决上述技术问题，本发明采用的技术方案是一种美白组合物，按质量份计，包括以下组分：二葡糖基棓酸1-4份、肌肽0.1-0.5份、乙酰壳糖胺1-4份；其制备方法：常温下，将二葡糖基棓酸、肌肽、乙酰壳糖胺逐一添加混合搅拌即得到成品。
本发明解决的另一个技术问题是含上述美白组合物的精华液的制备方法，包括以下步骤：
(1)将抑菌剂、多元醇混合，加热搅拌溶解均匀，得到第一混合物，备用；
(2)将溶剂、螯合剂及增稠剂依次投入主锅中，加热，均质后搅拌溶解至均匀；
(3)主锅降温至65℃～50℃，加入第一混合物，速度为100rmp/min下搅拌5min溶解均匀；
(4)主锅降温至45℃～30℃，加入多元醇、美白组合物及舒敏剂，搅拌速度为100rmp/min下搅拌5min溶解均匀；
(5)向主锅中加入pH调节剂，速度为100rmp/min下搅拌5min溶解均匀，检测合格出料，得到成品。
优选的，步骤(1)中，所述加热温度为50℃～65℃，进一步，加热温度为60℃；所述搅拌速度为50rmp/min～200rmp/min，进一步，搅拌速度为80rmp/min。
优选的，步骤(2)中，所述加热温度为60℃～80℃，进一步的，加热温度为75℃；所述均质速度为500rmp/min～2000rmp/min，均质时间为4min～8min，进一步的，均质速度为800rmp/min，均质时间为5min。所述搅拌速度为80rmp/min～200rmp/min，搅拌时间5min～15min，进一步，搅拌速度为100rmp/min，搅拌时间8min。
优选的，步骤(3)中，降温温度至60℃；
优选的，步骤(4)中，降温温度至40℃。
本发明解决的再一个技术问题提供上述制备方法的精华液，按质量份计，包括以下组分：
溶剂：71.5份－91.43份；
多元醇：5份－15份；
舒敏剂：0.05份－1份；
增稠剂：0.1份－1份；
美白组合物：2.1份－8.5份；
螯合剂：0.01份－0.5份；
pH调节剂：0.01份－1份；
抑菌剂：1.3份－1.5份。
优选的，所述溶剂为去离子水、超纯水、植物纯露中的至少一种。进一步，所述纯露为玫瑰纯露、库拉索芦荟叶水中的至少一种。
优选的，所述多元醇为甘油、1，3－丁二醇、双甘油、1，3－丙二醇，1，2－戊二醇中的至少一种。进一步，所述多元醇为双甘油及1，2－戊二醇。
优选的，所述舒敏剂为甘草酸二钾、尿囊素、甘草根提取物中的至少一种。进一步，所述舒敏剂为甘草酸二钾。
优选的，所述增稠剂为卡波姆、丙烯酰二甲基牛磺酸铵/VP共聚物中至少一种。进一步，所述增稠剂为卡波姆980或卡波姆2020。
优选的，所述螯合剂为乙二胺四乙酸二钠、乙二胺四乙酸四钠中的至少一种。进一步，所述螯合剂为乙二胺四乙酸二钠。
优选的，所述为pH调节剂为三乙醇胺、精氨酸、氢氧化钠、氢氧化钾中的至少一种。进一步，所述pH调节剂为精氨酸。
优选的，所述抑菌剂为1，2－己二醇、对羟基苯乙酮的混合物，优选地质量份比1，2－己二醇：对羟基苯乙酮的＝8:5。
进一步地，上述美白组合物的精华液，还可以再添加着色剂、赋香剂。
二葡糖基棓酸：因皮肤中大多数微生物拥有α－葡萄糖苷酶基因，这是一种高度选择性的酶，可用于将二葡糖基棓酸分解为棓酸，也叫没食子酸(Gallic Acid)，并提高其对皮肤的功效。其功效具体表现为抑制MITF表达，从而调控酪氨酸酶及其相关蛋白酶的合成，降低黑色素的合成，还可以降低前列腺素E2(PEG2)的表达，使黑素小体的角质形成细胞受体饱和，从而限制黑色素的转运，使其未能到达角质形成细胞即被代谢排出体外。捕获紫外线诱导的自由基(ROS)，防止紫外线引起的DNA损伤，即使在紫外线条件下也能阻止黑色素合成；
肌肽：可以阻碍导致皮肤黄化的两个关键反应：自由基与不饱和脂肪酸的氧化反应和非酶糖基化反应，防止AGEs、RCS、脂褐素的产生并促进其代谢去除；还可以保护皮肤细胞受UVB照射后所致DNA损伤。
乙酰壳糖胺：具有优秀的透皮吸收性，能提升皮肤的水合能力，促进成纤维细胞和角质形成细胞中透明质酸的合成，是一种高品质的多功能保湿剂和角质代谢调节剂。除保湿功效外，具有优异的美白靓肤及天然角质代谢调节功效。
与现有技术相比，本发明的美白组合物作用于导致皮肤暗黄的关键路径及其多个交叉点，使得皮肤美白护理能够以一当十，达到少量高效、以点带面改善肤色的效果，且三个组合物二葡糖基棓酸、肌肽及乙酰壳糖胺在祛黑祛黄作用方面相互协同，表现出显著效果。
具体实施方式
下面结合实施例对本发明的具体实施方式做进一步的说明，但不是对本发明的限定。
实施例1：
一种美白组合物，按质量份计，包括以下组分：二葡糖基棓酸1份、肌肽0.5份、乙酰壳糖胺1份；其制备方法：常温下，将二葡糖基棓酸、肌肽、乙酰壳糖胺逐一添加混合搅拌即得到成品。
实施例2：
一种美白组合物，按质量份计，包括以下组分：二葡糖基棓酸2份、肌肽0.3份、乙酰壳糖胺2份；其制备方法：常温下，将二葡糖基棓酸、肌肽、乙酰壳糖胺逐一添加混合搅拌即得到成品。
实施例3：
一种美白组合物，按质量份计，包括以下组分：二葡糖基棓酸4份、肌肽0.1份、乙酰壳糖胺4份；其制备方法：常温下，将二葡糖基棓酸、肌肽、乙酰壳糖胺逐一添加混合搅拌即得到成品。
实施例4至9：
一种含上述美白组合物的精华液，其中，溶剂优选定玫瑰纯露，多元醇优选定双甘油与1，2－戊二醇的混合物，舒敏剂优选定甘草酸二钾，增稠剂优选定卡波姆980，美白组合物为二葡糖基棓酸、肌肽、乙酰壳糖胺的混合物，螯合剂优选定乙二胺四乙酸二钠，pH调节剂优选定精氨酸，抑菌剂优选定1，2－己二醇与对羟基苯乙酮混合物。各组分按质量份计如下表所示得到实施例6至9，且对比例为实施例9的改变例，如下表1：
上述实施6至9例的精华液的制备方法，包括以下步骤：
(1)将1，2己二醇、对羟基苯乙酮、双甘油混合，加热温度为60℃，搅拌速度为80rmp/min，搅拌溶解均匀，得到第一混合物，备用；
(2)将玫瑰纯露、甘草酸二钾、乙二胺四乙酸二钠、卡波姆980依次投入主锅中，加热温度为75℃，均质速度为800rmp/min，搅拌时间为8min，搅拌速度为100rmp/min，均质搅拌溶解至均匀；
(3)主锅降温至60℃，加入第一混合物，速度为100rmp/min下搅拌5min溶解均匀；
(4)主锅降温至40℃，加入1，2－戊二醇、美白组合物，搅拌速度为100rmp/min下搅拌5min溶解均匀；
(5)向主锅中加入精氨酸，速度为100rmp/min下搅拌5min溶解均匀，检测合格出料，得到成品。
为体现本发明的美白功效的效果，设置了以下测试方法：
(1)定义
人类皮肤颜色主要根据国际照明委员会(CIE)的L*a*b*颜色空间系统来表征：
L*值代表被测皮肤表面的黑白亮度，等于0时为黑，等于100时为白。
a*值代表红绿色之间的平衡，大于0表示红色，小于0表示绿色；
b*值代表皮肤蓝黄色度的变化，大于0表示黄色，小于0表示蓝色。
个体类型角(individual type angle，ITA°)：通过皮肤色度计或反射分光光度计测量皮肤L*a*b*颜色空间数据来表征人体皮肤颜色的参数，计算公式如下：
(2)试验方法
(2.1)受试者的选择
按受试者入选和排除标准选择合格的受试者，并按随机表分为试验组和对照组，在受试部位左右两侧色斑对称的情况下，可分为试验产品侧和对照产品侧，征集390人，分13组，30人/组，无脱访者。
(2.2)入选标准
30～50岁，健康女性，从事室内工作，无长时间或经常暴露于紫外线的活动；无过敏性疾病，无化妆品及其他外用制剂过敏史；既往无光感性疾病史，近期内未使用影响光感性的药物；受试部位皮肤应无胎记、炎症、瘢痕、多毛等现象；能够理解试验过程，自愿参加试验并签署书面知情同意书者。
(2.3)排除标准
妊娠或哺乳期妇女，或近期有备孕计划者；
患有银屑病、湿疹、异位性皮炎、严重痤疮等皮肤病史者；或患有其他慢性系统性疾病者；
近1个月内口服或外用过皮质类固醇激素等抗炎药物者；
近2个月内使用过果酸、水杨酸等任何影响皮肤颜色的产品或药物(如氢醌类制剂)者；
近3个月内试验部位使用过维A酸类制剂或进行过化学剥脱、激光、脉冲光等医美治疗者；
不可避免长时间日光暴露者；
近2月内参加过其他临床试验者；
其他临床评估认为不适合参加试验者。
(2.4)受试者限制
1)在试验期间受试部位必须使用试验机构提供的试验产品，不能使用其他任何具有祛斑美白功效或者可能对测试结果产生影响的产品；
2)在试验期间不能有暴晒情况，并应做好试验部位的防晒工作。
(2.5)受试物
1)试验产品：本发明实施例、对比例及对照化妆品。
2)阴性对照产品：不含本发明美白组合物成分的相应试验产品基质配方产品。
(2.6)使用方法：由工作人员按照随机表发放试验产品和阴性对照产品(双盲测试)，并根据使用说明对受试者进行使用指导，确保受试者正确、连续使用产品8周。受试者记录使用时间及使用过程中的任何不适感和不良反应症状。
(2.7)试验部位：受试者面部。
(2.8)环境条件
试验结果测试在温度为21±1℃.相对湿度为50±10％RH、色温5500～6500K的日光灯管或LED光照的恒定环境下进行，并且所有受试者应在此环境条件下适应30分钟后进行测试。
(2.9)试验流程
1)按照要求招募入组志愿受试者，签署书面知情同意书。入组前根据入选和排除标准等询问受试者一系列关于疾病史、健康状况等问题，同时对面部肤色进行测试筛选，ITA°值在25°～35°者入选，并记录。
2)符合条件者按要求使用发放的产品；产品使用后2周、4周、8周再次于相同各部位进行测试并记录。
皮肤色度仪测量
在各访视时点，用皮肤色度仪分别测量试验组及对照组试验部固定部位皮肤的L*、a*、b*数值，每个测试区测试三次，取平均值，记录并计算ITA°值。测试皮肤区域ITA°值越大，肤色越浅，反之越深。
效果评测数据表现为均值±标准差，如下表2：
使用SPSS软件分别对各实施例和阴性对照L*、b*、ITA°值的第0周和第8周数据进行配对样本T检验，得到阴性对照组使用产品8周后b*值数据均显著性提高(P<0.05)，L*值数据显著性降低(P<0.05)，皮肤ITA°值相对比未使用前显著性变低(P<0.05)，即使用未添加美白组合物样品的受试者在8周后变得更暗黄。各组实施例b*值的第0周和第8周数据均显著性降低(P<0.05)，L*值数据显著性升高(P<0.05)，ITA°值显著性升高(P<0.05)，其中以实施例9最为显著(P<0.01)，即本次发明组合物具有优异的祛黄祛黑功能，可以达到去除暗黄的整体美白效果。
本发明组合物协同效果的评测，使用文献《Enhanced identification ofsynergistic and antagonistic emergent interactions among three or more drugs》(DOI:10.1098/rsif.2016.0332)中记载的公式和原理，具体如下：
式中：
E表示组合物相互作用的度量值，当E<-0.5时，相互作用为协同作用，E>0.5时为拮抗作用，-0.5≤E≤0.5时为简单叠加。
ωD表示各组对比例或实施例中加入D后L*、ITA°值的降低程度，b*值的升高程度，其中D＝(X,Y,Z,XY,XZ,YZ,XYZ)，即单个原料或几种原料的混合物。
X＝二葡糖基棓酸，对应对比例1；
Y＝肌肽，对应对比例2；
Z＝乙酰壳糖胺，对应对比例3；
XY＝二葡糖基棓酸+肌肽，对应对比例4；
XZ＝二葡糖基棓酸+乙酰壳糖胺，对应对比例5；
YZ＝肌肽+乙酰壳糖胺，对应对比例6；
XYZ＝二葡糖基棓酸+肌肽+乙酰壳糖胺，对应实施例9；
min(A,B,C)表示A，B,C中变化程度最小的一个。
根据以上原理，对前述实施例9和各组对比例中使用0周和8周的数据进行处理，得下表3：
| ωX | ωY | ωZ | ωXY | ωXZ | ωYZ | ωXYZ | E值 | |
| ΔL* | -1.11 | -0.22 | -0.5 | -1.92 | -2.18 | -0.93 | -2.78 | -1.12 |
| Δb* | -0.1 | -1.13 | -0.1 | -1.52 | -0.17 | -1.18 | -2.17 | -4.54 |
| ΔITA° | -2.48 | -1.98 | -1.18 | -6.2 | -4.85 | -4.29 | -8.97 | -1.19 |
如上表3：表现在L*、b*、ITA°值上本发明组合物相互作用的度量值E均小于－0.5，即该组合物在祛黑、祛黄和整体美白上均表现出协同效果。
综上所述，与现有技术相比，本发明的美白组合物作用于导致皮肤暗黄的关键路径及其多个交叉点，使得皮肤美白护理能够以一当十，达到少量高效、以点带面改善肤色的效果，且三个组合物二葡糖基棓酸、肌肽及乙酰壳糖胺在祛黑祛黄作用方面相互协同，表现出显著效果。
以上结合实施例对本发明的实施方式作出了详细说明，但本发明不局限于所描述的实施方式。对于本领域技术人员而言，在不脱离本发明的原理和精神的情况下，对这些实施方式进行各种变化、修改、替换和变型仍落入本发明保护范围内。
Claims (1)
1.一种美白组合物用于祛黑、祛黄的用途，其特征在于，按质量份计，由以下组分组成：二葡糖基棓酸4份、肌肽0.5份、乙酰壳糖胺4份；其制备方法：常温下，将二葡糖基棓酸、肌肽、乙酰壳糖胺逐一添加混合搅拌即得到成品。
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