CN115282096A - 一种新型祛痘印精华液及其制备方法 - Google Patents
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Abstract
本发明公开了一种新型祛痘印精华液及其制备方法。该精华液主要由以下质量百分含量的组分：纳米结构脂质载体12～18％、保湿剂1.5～3％、抗污剂0.5～1.2％、抗敏剂0.1～0.15％、防腐剂0.1～0.5％、pH调节剂0.5～1％、芳香剂0.01～0.02％、余量水。本发明采用纳米载体技术能有效促进植物活性成分的经皮渗透，显着增加皮肤对活性成分的保留。同时，纳米载体可以有效改善不溶性活性成分的溶解性，增强活性成分的稳定性，实现多种活性成分协同抑制酪氨酸酶，以阻止黑色素的形成，同时促进已形成黑色素沉淀的分解代谢，达到淡化痘印的效果。
Description
技术领域
本发明涉及化妆品技术领域，尤其涉及一种新型祛痘印精华液及其制备方法。
背景技术
众所周知，皮肤是身体最脆弱的部位，人体皮肤日常暴露在外会出现许多问题，例如痤疮、痘印、粉刺、色素沉着和晒伤痕迹等等。现在最常见的皮肤病是长痘，如果患者在长痘期间出现用手抠摸患处、不注意饮食、经常熬夜、随意使用功能性产品、暴露于空气污染物和紫外线辐射等情况，就会引发痘印、痘坑、黑色素沉着、炎症、氧化受损和屏障功能受损等一系列肌肤问题，对于整体的面部美观和皮肤状态都有着很大的影响，给患者带来较大的心理压力，甚至产生社交障碍。
目前，针对痘印问题已经研发出了多种具有祛痘印功能的产品。然而，这些产品中可能使用了大量抗生素、激素、重金属等成分，该类成分成本高昂、副作用大且具有毒性。虽然短时间内使用该类产品能有效抑制细菌、抗炎、淡化痘印，但是长期使用可能会出现过敏反应、毒性反应、炎症感染等问题。因此，许多消费者对含有天然成分的护肤产品需求正在迅速增加。但是，植物活性成分在祛痘印产品应用中存在溶解性差、稳定性差、皮肤渗透性低等问题，限制了植物活性成分在祛痘印产品中的应用。幸运的是，纳米载体技术很好地解决了上述问题，极大地拓展了植物活性成分在祛痘印产品的应用，但现有的纳米脂质体仍存在不稳定现象。
发明内容
为解决上述问题，本发明的目的在于提供一种新型祛痘印精华液及其制备方法。
为解决其技术问题，本发明采用的技术方案为：
本发明提供了一种新型祛痘印精华液，其特征在于，包括以下质量百分含量的组分：纳米结构脂质载体12～18％、保湿剂1.5～3％、抗污剂0.5～1.2％、抗敏剂0.1～0.15％、防腐剂0.1～0.5％、pH调节剂0.5～1％、芳香剂0.01～0.02％、余量水。
优选地，所述的一种新型祛痘印精华液，其特征在于，所述纳米结构脂质载体为甘草提取物0.5～3％、洋甘菊提取物1～5％、葡萄籽提取物1～5％；按照质量百分含量，还包括甘油单月桂酸酯3～5％、金盏花油3～5％、水凝胶0.5～1％。
优选地，所述水凝胶由聚乙二醇硬脂酸酯，壳聚糖，丙烯酸及N,N-亚甲基双丙烯酰胺组成；所述水凝胶中壳聚糖：聚乙二醇硬脂酸酯：丙烯酸：N,N-亚甲基双丙烯酰胺的质量比为：1:5:15:2。
优选地，所述的一种新型祛痘印精华液，其特征在于，所述保湿剂为透明质酸0.5～1.5％和银耳多糖0.5～1.2％。
优选地，所述的一种新型祛痘印精华液，其特征在于，所述抗污剂为维生素C 0.03～0.09％、维生素E 0.01～0.08％和阿魏酸0.4～1％。
优选地，所述的一种新型祛痘印精华液，其特征在于，所述抗敏剂为獐芽菜提取物0.05～0.09％和黄连提取物0.02～0.07％。
优选地，所述的一种新型祛痘印精华液，其特征在于，所述防腐剂为羟苯甲脂0.1～0.5％。
优选地，所述的一种新型祛痘印精华液，其特征在于，所述pH调节剂为三乙醇胺0.5～1％。
优选地，所述的一种新型祛痘印精华液，其特征在于，所述甘草提取物包含槲皮素、甘草类黄酮；所述洋甘菊提取物包含黄酮类活性成分；所述葡萄籽提取物包含原花青素。
本发明还提供一种所述新型祛痘印精华液的制备方法，其特征在于，包括以下步骤：
(1)制备含纳米结构脂质载体(NLC)的溶液：首先将甘油单月桂酸酯和金盏花油加热至50～60℃，然后将甘草提取物、洋甘菊提取物、葡萄籽提取物加入油相中，最后将含水凝胶的水相(水相中的水含量为：40％余量的去离子水)加热到50～60℃，并倒入油相中；进一步将混合物超声处理，冷却至25℃，得到纳米结构脂质载体(NLC)；并将其保存在4℃下备用；
所述水凝胶由聚乙二醇硬脂酸酯，壳聚糖，丙烯酸及N,N-亚甲基双丙烯酰胺组成，所述水凝胶中壳聚糖：聚乙二醇硬脂酸酯：丙烯酸：N,N-亚甲基双丙烯酰胺的质量比为：1:5:15:2，所述水凝胶制备方法为：将壳聚糖的酸性溶液，聚乙二醇硬脂酸酯，丙烯酸加入到三口烧瓶中，在氮气保护下，温度为50～60℃下，搅拌滴加偶氮二异丁腈的乙醇溶液及N,N-亚甲基丙烯酰胺，反应5～8h后，将产物用去离子水浸泡洗涤，烘干，研磨成粉末；所述壳聚糖的酸性溶液为质量分数为1％壳聚糖的甲酸溶液或质量分数为1％壳聚糖的乙酸溶液；所述偶氮二异丁腈的乙醇溶液中偶氮二异丁腈的体积质量分数为0.01g/mL；所述偶氮二异丁腈与丙烯酸的质量比为0.005～0.02:1；
(2)制备祛痘印精华液：先将抗敏剂加入50％余量的去离子水中，在60～90℃下搅拌10～40min，随后，加入保湿剂和抗污剂继续搅拌10～40min，完全溶解后冷却至40～60℃；再取上述(1)中制备得到的NLC加入其中，在60～90℃下搅拌10～40min；降温至35～55℃时，一次加入防腐剂和芳香剂，搅拌均匀将pH调节剂的水溶液与剩余的去离子水一起加入精华液，调节pH值为6～6.5，出料。
本发明提供了以上方案所述祛痘印精华液或上述技术方案所述制备方法制得的精华液在祛痘印中的应用。
与现有技术相比，本发明的有益效果为：
1.本发明制备的一种新型祛痘印精华液，甘草提取物中的槲皮素、甘草类黄酮可通过抑制酪氨酸酶和多巴色素互变酶(TRP-2)的活性、阻碍5,6—二羟基吲哚(DHl)的聚合，以此来阻止黑色素的形成，从而达到美白皮肤的效果。
2.本发明制备的一种新型祛痘印精华液，洋甘菊提取物中富含黄酮类活性成分，可清除自由基，抑制酪氨酸酶活性。同时，该成分还具有抗氧化、消炎、抗变应性、和抗病毒的功效。
3.本发明制备的一种新型祛痘印精华液，葡萄提取物所含的原花青素具有超强抗氧化能力，保护胶原蛋白，改善皮肤弹性与光泽，美白、保湿、祛斑；减少皱纹、保持皮肤的柔润光滑；清除痤疮、愈合疤痕。
4.本发明制备的一种新型祛痘印精华液，提取物中的多糖含有许多亲水性的羟基，可与水分子形成氢键，并相互交联成网状结构而使其表现出良好的吸水性和保湿性。
5.本发明制备的一种新型祛痘印精华液，通过添加天然的祛痘印成分，同时加入抗污剂、渗透促进剂等助剂，制备了一种具有良好祛印效果的精华液。通过纳米载体技术能有效促进植物活性成分的经皮渗透，显着增加皮肤对活性成分的保留。同时，纳米载体可以有效改善不溶性活性成分的溶解性，增强活性成分的稳定性，实现多种活性成分协同抑制酪氨酸酶，以此来阻止黑色素的形成，同时促进已形成黑色素沉淀的分解代谢，从而达到淡化痘印的效果，纳米载体上的水凝胶可增加脂质体稳定性。
6.本发明所制备通过将聚乙二醇硬脂酸酯，壳聚糖，丙烯酸及N,N-亚甲基双丙烯酰胺制备成水凝胶，负载在纳米脂质体外层，其中聚乙二醇硬脂酸酯的疏水性长碳链可嵌入到脂质体间，减少渗漏。壳聚糖所带电荷斥力有利于脂质体的稳定，防止团聚；同时，壳聚糖表面所带电荷有利于与细胞结合，增加吸附能力。同时聚丙烯酸有具有优异的保水性。
说明书附图
图1为实施例1～4与对比例1～5酪氨酸酶活性抑制实验图；
图2为实施例1～4与对比例1～5在不同时间点角质层内祛印活性物的渗透量图。
具体实施方式
下面通过实施例对本发明进行具体描述，只用于对本发明进行进一步说明，不能理解为对本发明保护范围的限定。对外应理解，在阅读了本发明的内容之后，本领域技术人员对本发明作各种改动或修改，这些等价形式同样落于本申请所附权利要求书所限定的范围。
实施例1～4：
实施例1～4提供了一种新型祛痘印精华液，分别由表1所示重量百分含量的组分组成：
表1祛痘印精华液各例含量配比
注：本发明中，余量是指精华液配方组成中，除去离子水以外的组分有限定的重量百分含量，配方中所有组分含量加和之后，最后用去离子水补足至100％。香精为日用香精。
需要注意的是，本发明所述纳米结构脂质载体为甘草提取物0.5～3％、洋甘菊提取物1～5％、葡萄籽提取物1～5％；按照质量百分含量，还包括甘油单月桂酸酯3～5％、金盏花油3～5％、水凝胶0.5～1％。纳米结构脂质载体在制备过程中，需要加入水相，为余量水质量分数的40％，制得的为纳米结构脂质载体的水溶液。
实施例1～4水凝胶的制备方法为：将1g壳聚糖在三口瓶中搅拌溶于100mL质量分数为1％的乙酸溶液，再加入5g聚乙二醇硬脂酸酯，15g丙烯酸加入到三口烧瓶中，在氮气保护下，温度为50～60℃下，搅拌滴加10mL体积质量分数为0.01g/mL的偶氮二异丁腈乙醇溶液及2g N,N-亚甲基丙烯酰胺，反应5～8h后，将产物用去离子水浸泡洗涤，烘干，研磨成粉末。
实施例1～4的祛痘印精华液的制备方法，包括以下步骤：
(1)制备含纳米结构脂质载体(NLC)的溶液：首先将甘油单月桂酸酯和金盏花油加热至55℃，然后将甘草提取物、洋甘菊提取物、葡萄籽提取物加入油相中，最后将含水凝胶的水相(水相中的水含量为：40％余量的去离子水)加热到55℃，并倒入油相中；进一步将混合物超声处理，冷却至25℃，得到纳米结构脂质载体(NLC)；并将其保存在4℃下备用。
(2)制备祛痘印精华液：先将抗敏剂加入50％余量的去离子水中，在60～90℃下搅拌20min，随后，加入保湿剂和抗污剂继续搅拌20min，完全溶解后冷却至40℃；再取上述(1)中制备得到的NLC加入其中，在70℃下搅拌20min；降温至40℃时，一次加入防腐剂和芳香剂，搅拌均匀，将pH调节剂的水溶液与剩余的去离子水一起加入精华液中，调节pH值为6.5，出料。
对比例1
本对比例一种新型祛痘印精华液，其原料和制备方法类似实施例1，区别在于：未采用所述的银耳多糖、葡萄籽提取物和甘草提取物。
对比例2
本对比例一种新型祛痘印精华液，其原料和制备方法类似实施例1，区别在于：未采用所述的獐芽菜提取物、葡萄籽提取物和洋甘菊提取物。
对比例3
本对比例一种新型祛痘印精华液，其原料及制备方法类似实施例1，区别在于：未采用所述纳米结构脂质载体(NLC)，其制备方法为，将甘草提取物、洋甘菊提取物、葡萄籽提取物，抗敏剂加入水相中，在70℃下搅拌20min，随后，加入保湿剂和抗污剂继续搅拌20min，完全溶解后降温至40℃时，一次加入防腐剂和芳香剂，搅拌均匀将pH调节剂的水溶液与剩余的去离子水一起加入精华液，调节pH值为6.5，出料。
对比例4
本对比例一种新型祛痘印精华液，其原料及制备方法类似实施例1，区别在于：水凝胶的制备过程中不添加聚乙二醇硬脂酸酯。
对比例5
本对比例一种新型祛痘印精华液，其原料及制备方法类似实施例1，区别在于：水凝胶的制备过程中不添加壳聚糖。
理化性能测试：
测试产品的pH值、高低温稳定性和离心稳定性，以评价该产品的理化性能。采用稀释法，使用pH计测定产品的pH值:准确称量所开发的祛痘调理精华乳10.0g，加入经煮沸冷却后的去离子水10.0g进行稀释，加热至40℃，期间不断搅拌使其分散均匀，然后冷却至室温，***校正过的pH计，待读数稳定后读取数值，测量两次取其平均值。高低温稳定性测试:将产品先置于-15℃冰箱中24h，取出后放置在45℃烘箱中24h，重复3次，观察产品的状态。
理化性能测试结果：
对按照最终配方制备的祛痘调理精华乳进行理化性能测试，其pH值为6.0～6.5，经高低温和离心实验后，其稳定性较好，未观察到油水分离现象。
刺激性试验、过敏性实验：
小白鼠背部剪去毛，分别涂抹按实施例1～4和对比例1～5制备的精华液于剪去毛的部位，和没涂部位进行比较，结果没有刺激性和过敏反应。取实施例1～4和对比例1～5所得的精华液1克涂于志愿手面上，过30分钟后观察，均未出现发红，发疹，起泡现象。
祛痘印精华液效果测试
测试人群：受试者均为患有痘印问题的在校大学生志愿者，包括一至四年级的男女生共135名。
测前准备：受试者被试部位在试验前3天内不允许使用任何产品(化妆品或外用药物)。正式测试前，对志愿者进行基础测试，取适量本品涂抹于志愿者耳后，观察是否有过敏或其他不良反应。只有在一切顺利的情况下，他们才能签署一份知情同意继续参加测试。
测试方法：随机分为8组，试用期限为28天，左侧面颊涂抹对照组样品，右侧面颊涂抹试验组样品，各组早晚各涂抹一次，分别在第7天、第14天、第21天和第28天各随访一次，随访日为同一时间，采集受试者的主观评价数据。
评判标准：请每组15名受试者结合自身使用情况，用肉眼对实施例1～4和对比例1～5产品的祛痘印效果进行评分，分无效、效果不明显、效果一般和效果明显共4个等级，此结果见表2：
表2祛痘印精华液试用效果
| 无效(人) | 效果不明显(人) | 效果一般(人) | 效果明显(人) | 总有效率(％) | |
| 实例1 | 1 | 1 | 3 | 10 | 93.3 |
| 实例2 | 2 | 2 | 2 | 9 | 86.7 |
| 实例3 | 2 | 1 | 4 | 8 | 86.7 |
| 实例4 | 1 | 1 | 3 | 10 | 93.3 |
| 对比例1 | 4 | 1 | 4 | 6 | 73.3 |
| 对比例2 | 3 | 3 | 3 | 6 | 80.0 |
| 对比例3 | 5 | 2 | 3 | 5 | 66.7 |
| 对比例4 | 3 | 1 | 4 | 7 | 80.0 |
| 对比例5 | 2 | 3 | 4 | 6 | 86.7 |
酪氨酸酶活性抑制实验方法为：T/SHRH 015，实验结果见图1。可知，对比例1和对比例2中祛痘印成分单一，对比例3中无脂质体，对比例4和对比例5中脂质体不如实施例1～4稳定。对比例1～5酪氨酸酶活性抑制效果不如实施例。
体外透皮试验：利用共聚焦拉曼技术，在受试者测试区域分别对单次使用精华液15min、1h和2h后皮肤进行渗透性检测，得到不同时间点角质层内精华液中祛印活性物的渗透量，结果见图2。可知，随着精华液单次使用时间的延长，渗透量逐渐增加。对比例3由于无纳米脂质载体，渗透量低。对比例4无聚乙二醇硬脂酸酯，对比例5无壳聚糖，脂质体稳定性效果不如实施例，渗透低。
本发明精华液综合效果考察
通过利用试用感觉来评价实施例1～4和对比例1～5制备出的祛痘印精华液的功效。采用民意调查评分法，招募90名大学生志愿者作为试用对象，分成9组，分别用实施例1～4和对比例1～5制备的精华液涂抹在痘印处。每天使用两次，使用时间一个月。各项使用效果总分为10分：10分为最高分，表示很好，非常满意；8分为较好；6分为可以接受；6分以下为不好，不能接受。将每组评分数据取平均值，结果见表3：
表3综合使用效果
综上所述，本发明所制备的精华液能有效促进植物活性成分的经皮渗透，显着增加皮肤对活性成分的保留。同时有效改善不溶性活性成分的溶解性，增强活性成分的稳定性，实现多种活性成分协同抑制酪氨酸酶，以此来阻止黑色素的形成、促进已形成黑色素沉淀的分解代谢，从而达到淡化痘印的效果。
以上仅为本发明的具体实施例，但本发明的技术特征并不局限于此。任何以本发明为基础，为解决基本相同的技术问题，实现基本相同的技术效果，所做出的简单变化、等同替换或者修饰等，皆涵盖于本发明的保护范围之中。
Claims (10)
1.一种新型祛痘印精华液，其特征在于，包括以下质量百分含量的组分：纳米结构脂质载体12～18％、保湿剂1.5～3％、抗污剂0.5～1.2％、抗敏剂0.1～0.15％、防腐剂0.1～0.5％、pH调节剂0.5～1％、芳香剂0.01～0.02％、余量水。
2.根据权利要求1所述的一种新型祛痘印精华液，其特征在于，所述纳米结构脂质载体按照质量百分含量含甘草提取物0.5～3％、洋甘菊提取物1～5％、葡萄籽提取物1～5％，甘油单月桂酸酯3～5％、金盏花油3～5％、水凝胶0.5～1％。
3.根据权利要求2所述的一种新型祛痘印精华液，其特征在于，所述水凝胶由聚乙二醇硬脂酸酯，壳聚糖，丙烯酸及N,N-亚甲基双丙烯酰胺组成；所述水凝胶中壳聚糖：聚乙二醇硬脂酸酯：丙烯酸：N,N-亚甲基双丙烯酰胺的质量比为：1：5：15：2。
4.根据权利要求1所述的一种新型祛痘印精华液，其特征在于，所述保湿剂为透明质酸0.5～1.5％和银耳多糖0.5～1.2％。
5.根据权利要求1所述的一种新型祛痘印精华液，其特征在于，所述抗污剂维生素C0.03～0.09％、维生素E 0.01～0.08％和阿魏酸0.4～1％。
6.根据权利要求1所述的一种新型祛痘印精华液，其特征在于，所述抗敏剂为獐芽菜提取物0.05～0.09％和黄连提取物0.02～0.07％。
7.根据权利要求1所述的一种新型祛痘印精华液，其特征在于，所述防腐剂为羟苯甲脂0.1～0.5％。
8.根据权利要求1所述的一种新型祛痘印精华液，其特征在于，所述pH调节剂为三乙醇胺0.5～1％。
9.一种根据权利要求1-8任意一项所述的新型祛痘印精华液的制备方法，其特征在于，包括以下步骤：
(1)制备含纳米结构脂质载体(NLC)的溶液：首先将甘油单月桂酸酯和金盏花油加热至50～60℃，然后将甘草提取物、洋甘菊提取物、葡萄籽提取物加入油相中，最后将含水凝胶的水相(水相中的水含量为：40％余量的去离子水)加热到50～60℃，并倒入油相中；进一步将混合物超声处理，冷却至25℃，得到含纳米结构脂质载体(NLC)的溶液；并将其保存在4℃下备用；
所述水凝胶由聚乙二醇硬脂酸酯，壳聚糖，丙烯酸及N,N-亚甲基双丙烯酰胺组成；
所述水凝胶中壳聚糖：聚乙二醇硬脂酸酯：丙烯酸：N,N-亚甲基双丙烯酰胺的质量比为：1:5:15:2；
所述水凝胶制备方法为：将壳聚糖的酸性溶液，聚乙二醇硬脂酸酯，丙烯酸加入到三口烧瓶中，在氮气保护下，温度为50～60℃下，搅拌滴加偶氮二异丁腈的乙醇溶液及N,N-亚甲基丙烯酰胺，反应5～8h后，将产物用去离子水浸泡洗涤，烘干，研磨成粉末；所述壳聚糖的酸性溶液为质量分数为1％壳聚糖的甲酸溶液或质量分数为1％壳聚糖的乙酸溶液；所述偶氮二异丁腈的乙醇溶液中偶氮二异丁腈的体积质量分数为0.01g/mL；所述偶氮二异丁腈与丙烯酸的质量比为0.005～0.02:1；
(2)制备祛痘印精华液：先将抗敏剂加入50％余量的去离子水中，在60～90℃下搅拌10～40min，随后，加入保湿剂和抗污剂继续搅拌10～40min，完全溶解后冷却至40～60℃；再取上述(1)中制备得到的NLC加入其中，在60～90℃下搅拌10～40min；降温至35～55℃时，一次加入防腐剂和芳香剂，搅拌均匀，将pH调节剂的水溶液与剩余的去离子水一起加入精华液，调节pH值为6～6.5，出料。
10.权利要求1～8任意一项所述祛痘印精华液或由权利要求9所述制备方法制得的精华液在祛痘印中的应用。
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