CN113557002A - 包含油连续纳米乳液的多重乳液及使用该乳液的方法 - Google Patents
包含油连续纳米乳液的多重乳液及使用该乳液的方法 Download PDFInfo
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- CN113557002A CN113557002A CN202080020300.XA CN202080020300A CN113557002A CN 113557002 A CN113557002 A CN 113557002A CN 202080020300 A CN202080020300 A CN 202080020300A CN 113557002 A CN113557002 A CN 113557002A
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Abstract
描述了包含内相的多重乳液，所述内相是油连续纳米乳液。所述多重乳液是水连续的、稳定的，提供保湿的益处和可以包含高浓度的水溶性活性物质。
Description
技术领域
本发明涉及包含油连续纳米乳液的多重乳液及使用该乳液的方法。更特别地，本发明涉及水连续但包含油连续纳米乳液作为内相的多重乳液。
背景技术
纳米乳液的用途在美容和个人护理组合物中变得越来越流行。纳米乳液通常是稳定的，并且鉴于其单位体积而具有高的表面积。纳米乳液可以在其水和油相中携带活性物质，并且因为其尺寸有助于增强活性物质穿透皮肤，所以它是理想的。尽管与乳液(尤其是纳米乳液)相关的优点，但乳液的一般问题通常涉及无法包含多种活性物质以及高含量的保湿剂，如甘油，这通常妨碍重要活性物质在水中的溶解性。此外，在含水量高的组合物中，需要大量的防腐剂用于微生物稳定性。
出乎意料地发现，当油连续纳米乳液作为内相存在于水连续多重乳液中时，可以分离出亲水性活性物质，并且可以制备具有高含水量的最终用途组合物，以提供良好的感官和保湿益处。还发现，当制备具有油连续纳米乳液的多重乳液作为内相时，所得多重乳液需要更少的防腐剂用于微生物稳定性。
为消费者提供具有活性物质和保湿益处且不含高含量防腐剂的组合物的兴趣日益增加。
因此，本发明涉及包含油连续纳米乳液的多重乳液及使用该乳液的方法。令人惊讶的是，本发明的多重乳液在其水相中可以具有高浓度的亲水性有益剂，提供优异的保湿益处，并且不需要高含量的防腐剂用于微生物稳定性。该多重乳液是稳定的，具有良好的感官性质(与传统的不含甘油的水包油乳液一致)，即使存在甘油也是不粘的。本发明还涉及使用该多重乳液的方法。
附加信息
已经公开了制备乳液的努力。在美国公开专利申请号2017/0112764A1中，描述了具有可逆连续相和分散相的纳米乳液。
甚至已经公开了用于制备乳液的其他努力。在世界申请WO 03/039724 A1中，描述了包含纳米尺寸的颗粒的多重乳液。
还公开了用于制备乳液的其他努力。在美国专利号5,589,177中描述了可冲洗掉的油包水多重乳液组合物。
上述附加信息均未描述本权利要求中所述的多重乳液和使用多重乳液的方法。
发明概述
在第一方面，本发明涉及多重乳液，其包括：
(a)包含油包水纳米乳液的内相；和
(b)包含水和保湿剂的外水相，
所述外水相中的水和保湿剂的重量比为95:5至50:50，并且所述油包水乳液包含具有小于8的HLB的乳化剂，并且所述外相包含具有8或更大的HLB的乳化剂，其中所述外水相占所述多重乳液的25至70重量％。
在第二方面，本发明涉及包含多重乳液的化妆品组合物，所述多重乳液包括：
(a)内相，其包括包含乳化剂的油包水纳米乳液，所述纳米乳液具有100至850nm的颗粒尺寸，并且进一步包含基于所述纳米乳液总重量的0.0至15重量％的油溶性有益剂、0.0至15重量％的水溶性有益剂和0.0至20重量％的保湿剂；和
(b)外水相，其包含水、基于所述外水相总重量的0.0至20重量％的保湿剂和0.0至15重量％的水溶性有益剂，
所述化妆品组合物包含基于所述化妆品组合物总重量的20至65重量％(优选地40至60重量％)的纳米乳液，前提是所述纳米乳液和外水相不同时含有0.0重量％的保湿剂。
在第三方面，本发明涉及本发明第一和第二方面的所述多重乳液和化妆品组合物用于改进化妆品皮肤特性的用途。
通过以下描述和示例，本发明的所有其他方面更容易变得明白。
如本文所用，皮肤意指包括臂部(包括腋下)、脸部、脚部、颈部、胸部、手部、腿部、臀部和头皮(包括头发)上的皮肤。对于所述多重乳状和纳米乳液而言，颗粒尺寸指水滴的体积平均直径，单位分别为微米或纳米。可使用市售的Malvern Mastersizer测量水滴尺寸。化妆品组合物是一种用于局部施用的组合物，并且包括霜剂、乳液、香膏、精华液、凝胶、摩丝、气雾剂、除臭剂、止汗剂、洗发水、护发素、化妆品或个人洗涤用品，包括条和液体。这类组合物可以是本发明的多重乳液或具有其中添加了额外成分的多重乳液，所述额外成分如油(如硅油、鱼油或矿物油)、香味剂、有益剂(如维生素B3、间苯二酚和类视黄醇)和/或着色剂。有益剂(或活性物质)，如本文所定义，是水溶性或不溶性组分，其在局部施用后对皮肤产生益处。水不溶性是指在25℃、大气压和中性pH，在水中的溶解性不超过0.05重量％。对于不溶性有益剂如某些氨基酸(如胱氨酸)，可以调整水的pH以诱导该溶质在水中的溶解性。如本文所用，中性pH是指6.0至7.5的pH。除非另有说明，如本文所用的粘度通过使用Brookfield helipath TD，转速为4rpm，持续1分钟进行测量。如本文所用，多重乳液是指包含本发明的纳米乳液的水连续(在水中油包水)乳液。这类多重乳液通常在其内相内具有1至35微米的油滴尺寸，包括其中包含的所有范围。在另一个实施方案中，本发明的化妆品组合物是免洗皮肤乳液、霜剂或液体个人洗涤组合物。在另一个实施方案中，所述化妆品组合物是用于局部施用并留在皮肤上的乳液或霜剂。在没有另外明确说明的情况下，本文所述的所有范围均指包含在其中的所有范围。术语“包含”意指覆盖术语由…基本上组成和由…组成。为避免疑义，并且通过举例说明，包含油、水、乳化剂和有益剂的本发明的油连续纳米乳液是指包括基本上由上述组成的纳米乳液和由上述组成的纳米乳液。除了在操作对比示例中，或在另有明确说明的情况下，本说明书中表明材料或条件的量或比率和/或材料和/或用途的物理性质的所有数字均应理解为由词语“约”修饰。
发明详述
对于用于本发明的多重乳液中的油连续纳米乳液而言，基于所述纳米乳液总重量，其通常包含30至70重量％，在另一个实施方案中包含35至65重量％，在又一个实施方案中包含40至60重量％的水，并且包括其中包含的所有范围。
对于所述纳米乳液中的油而言，基于所述纳米乳液总重量，所述油通常占所述纳米乳液的25至70重量％，在另一个实施方案中占30至65重量％，在又一个实施方案中占35至60重量％，并且包括其中包含的所有范围。这类纳米乳液通常具有颗粒(水滴)尺寸为100至850纳米，在另一个实施方案中为150至800纳米，在又一个实施方案中为200至750纳米，包括其中包含的所有范围。
用于本发明的纳米乳液中的油仅限于在室温为液体(或加热至约35℃后为液体)，并且适用于施用于皮肤的局部组合物中的油。
适用的油的说明性示例包括硅油。
硅油可以分为挥发性和非挥发性种类。如本文所用，术语“挥发性”指在室温具有可测量蒸气压的那些材料。挥发性硅油优选地选自含有3-9个、优选地4-5个硅原子的环状或线性聚二甲基硅氧烷。
可用于本发明的非挥发性硅油包括聚烷基硅氧烷、聚烷基芳基硅氧烷和聚醚硅氧烷共聚物。这类可用于本发明的基本上非挥发性聚烷基硅氧烷包括，如在25℃，具有粘度为5-100,000厘沲的聚二甲基硅氧烷(如二甲基硅氧烷)
通常优选的硅氧烷来源为环戊硅氧烷和二甲硅油溶液。
本发明中用于制备乳液的合适的酯包括：
(1)具有10至20个碳原子的脂肪酸的烯基或烷基酯，如棕榈酸异丙酯、异硬脂酸异丙酯、异壬酸异壬酯、肉豆蔻酸油酯、肉豆蔻酸异丙酯、硬脂酸油酯和油酸油酯；
(2)醚酯，如乙氧基化脂肪醇的脂肪酸酯；
(3)多元醇酯，如乙二醇单-和二-脂肪酸酯、二甘醇单-和二-脂肪酸酯、聚乙二醇(200-6000)单-和二-脂肪酸酯、丙二醇单-和二-脂肪酸酯、聚丙二醇2000单油酸酯、聚丙二醇2000单硬脂酸酯、乙氧基化丙二醇单硬脂酸酯、甘油单-和二-脂肪酸酯、聚甘油聚脂肪酯、乙氧基化单硬脂酸甘油酯、1,3-单硬脂酸丁二醇酯、1,3-二硬脂酸丁二醇酯，聚氧乙烯多元醇脂肪酸酯、山梨聚糖脂肪酸酯和聚氧乙烯山梨聚糖脂肪酸酯。
(4)甾醇酯，其中大豆甾醇和胆固醇脂肪酸酯是其示例。
可用于本发明的其他油包括甘油三酯(动物和/或植物)，如大豆油、葵花籽油、椰子油、棕榈仁油、蓖麻油、菜籽油、棕榈油、葡萄籽油、辛酸/癸酸甘油三酯、红花油、鱼油或其混合物。
还有其他适用的油包括矿物油、霍霍巴油、异链烷烃、C12-C15烷基苯甲酸、聚α-烯烃、异十六烷、矿脂及其混合物(包括与上述油的混合物)等。在本发明的一个实施方案中，大豆油和葵花籽油为所使用的甘油三酯油。
在又一个实施方案中，辛酸癸酸甘油三酯是另一种适用于本发明的纳米乳液中的油。
可以使用适合于改变本发明的多重乳液中水相的pH的调节剂。该pH调节剂包括三乙胺、NaOH、KOH、H2SO4、HCl、C6H8O7(即柠檬酸)或其混合物。pH调节剂的加入量应使得本发明的多重乳液的所得pH为5至7.5。在一个实施方案中，pH为6至7.5，在又一个实施方案中，pH为6至7。
在本发明的一个实施方案中，应特别注意的是，当有益剂为氨基酸(如胱氨酸)时，将具有10至14的pH且其中溶解有氨基酸的油连续粗乳液与具有2至5的pH的粗乳液组合。将所述粗乳液混合并剪切以产生适合用作本发明的水连续多重乳液的内相的纳米乳液。
通过使用常规仪器，如从Thermo
市售的pH计，评估本发明期望的纳米和多重乳液的水相pH值。
适用于本发明用于制备纳米乳液的乳化剂通常具有2.5至小于8.0，优选地3至7.0，最优选地3至6.5的HLB，包括其中包含的所有范围。
适用于制备本发明的油连续纳米乳液的乳化剂类型的说明性示例为丙二醇异硬脂酸酯、乙二醇硬脂酸酯山梨聚糖倍半油酸酯、卵磷脂、油醇聚醚-2、硬脂醇聚醚-2、ceteth-2甘油硬脂酸酯、PEG-30二聚羟基硬酯酸酯。
其他适用的乳化剂包括二硬脂酸乙二醇酯、油酸甘油酯、山梨聚糖单油酸酯、山梨聚糖三硬脂酸酯、山梨聚糖三油酸酯、山梨聚糖单棕榈酸酯、月桂基PEG-10、(三甲基硅氧基)硅烷基乙基聚二甲基硅氧烷(Dow
ES-5300)或其混合物。
适用于制备包含本发明纳米乳液的水连续乳液的乳化剂类型的说明性示例为聚山梨醇酯85、月桂醇聚醚-4、月桂酸钠、鲸蜡硬脂基葡糖苷、PEG-8油酸酯、吐温20、吐温40、油醇聚醚-10或其混合物。
在本发明的油连续纳米乳液和水连续多重乳液中，乳化剂通常并独立地占每种乳液(即纳米和水连续两者)的1.0至10重量％，优选地1.2至8重量％，最优选地1.5至7.5重量％，包括其中包含的所有范围。
所述水连续乳液的外相通常占所述水乳液中的油包水的25至70重量％。在一个实施方案中，所述外相占所述水乳液中的油包水的35至65重量％。在又一个实施方案中，外相占所述水乳液中的油包水的40至60重量％。
对于适用于本发明的任选的皮肤有益剂而言，其仅受限于其能够被局部施用且适合于溶解于本发明多重乳液的油相或水相的范围。应当理解，有益剂在水相中的溶解性可以通过用本文所述的调节剂改变或调节水相的pH而受到影响。
适合包含在多重乳液的水相中的有益剂的说明性示例是酸，如氨基酸，如精氨酸、缬氨酸或组氨酸。其他适用的水溶性有益剂包括维生素B2、烟酰胺(维生素B3)、维生素B6、维生素C及其混合物等。也可以使用这些维生素的水溶性衍生物。如，维生素C衍生物如抗坏血酸四异棕榈酸酯、抗坏血酸磷酸镁和抗坏血酸糖苷可以单独使用或彼此联合使用。适用于本发明的多重乳液的水相中的其他水溶性有益剂包括4-乙基间苯二酚，提取物例如鼠尾草、芦荟、绿茶、葡萄籽、百里香、洋甘菊、蓍草、黄瓜、甘草或迷迭香提取物或其混合物。也可以使用水溶性防晒剂，如恩索利唑。当存在于本发明的乳液(即纳米和多重)的水相中时，基于所述纳米乳液和所述多重乳液的水相的总重量(视情况而定)，水溶性有益剂(包括混合物)的总量可以为0.0至15重量％，优选地0.001至10重量％，最佳地0.01至6重量％，并包括其中包含的所有范围。
在所述多重乳液的纳米乳液的水相中包括水不溶性有益剂也在本发明的范围内，所述水不溶性有益剂如不溶性氨基酸，如苯丙氨酸、酪氨酸、色氨酸、胱氨酸或其混合物，其通过水的pH值改变来提高其溶解性。在一个实施方案中，不溶性有益剂占所述多重乳液总重量的0.02至5重量％，在另一个实施方案中占0.1至3重量％，在又一个实施方案中占0.3至2重量％，包括其中包含的所有范围。
当制备具有不溶性有益剂(如，胱氨酸)的纳米乳液时，通常制备具有10至14的pH的第一油包水粗乳液，以溶解不溶性有益剂。将其与具有2.5至4的pH且无有益剂的第二油包水粗乳液组合。将所述粗乳液混合(高pH对于低pH的重量比为75:30至50:50或70:30至60至40，包括其中包含的所有比率)。在本文所述的条件下均质化或剪切所得的粗乳液的混合物，以产生适用作本发明的多重乳液的内相的油连续纳米乳液。
在所述纳米乳液的油相中任选地包括油溶性有益剂也在本发明的范围内。关于这类油溶性有益剂的唯一限制为，当局部施用时，其适合于为皮肤提供益处。
可任选地用于本发明的油溶性有益剂的类型的说明性示例包括维生素，如维生素A、D、E和K(及其油溶性衍生物)、防晒剂如乙基己基甲氧基肉桂酸酯、双-乙基己氧苯酚甲氧苯基三嗪、2-乙基己基-2-氰基-3,3-二苯基-2-丙酸、甲酚曲唑三硅氧烷、3,3,5-三甲基环己基2-羟基苯甲酸酯、2-乙基己基-2-羟基苯甲酸酯或其混合物。
其他适用的任选的油溶性有益剂包括间苯二酚，如4-己基间苯二酚、4-苯乙基间苯二酚、4-环戊基间苯二酚、4-环己基间苯二酚、4-异丙基间苯二酚或其混合物。此外，可以使用5-取代的间苯二酚，如4-环己基-5-甲基苯-1,3-二醇、4-异丙基-5-甲基苯-1,3-二醇及其混合物等。5-取代的间苯二酚及其合成在共同转让的美国公开专利申请号2016/000669A1中有所描述。
甚至其他适用的油溶性活性物质包括omega-3脂肪酸、omega-6脂肪酸、氯咪巴唑、法呢醇、熊果酸、肉豆蔻酸、香叶基香叶醇、油基甜菜碱、椰油酰基羟乙基咪唑啉、己酰基鞘氨醇、12-羟基硬脂酸、岩芹酸、共轭亚油酸、萜品醇、百里酚及其混合物等。
在本发明的一个实施方案中，所使用的任选的油溶性有益剂为视黄酸前体。
在本发明的一个实施方案中，视黄酸前体为视黄醇、视黄醛、视黄醇丙酸酯、视黄醇棕榈酸酯、视黄醇乙酸酯或其混合物。通常优选的是视黄醇丙酸酯、视黄醇棕榈酸酯及其混合物。
在又一个实施方案中，适用的视黄酸前体是由Molecular Design International提供的、以
名称市售的对甲氧基苯基氧代乙醇视黄酸酯。其可与本文所述的油溶性活性物质混合使用。
当将任选的(即0.0至15重量％)油溶性活性物质用于本发明的纳米乳液的油相中时，其通常占本发明的多重乳液中纳米乳液总重量的0.001至15重量％，在另一个实施方案中占0.05至7.0重量％，在又一个实施方案中占0.1至5重量％，并且包括其中包含的所有范围。
理想地可以将防腐剂并入本发明的纳米乳液的水相和多重乳液的外相中，以防止潜在有害微生物的生长，尽管不含防腐剂的这类乳液也在本发明的范围内。用于本发明的合适的传统防腐剂为对羟基苯甲酸的烷基酯。其他防腐剂包括乙内酰脲衍生物、丙酸盐和各种季铵化合物。化妆品化学师熟悉适当的防腐剂，并常规地选择它们以满足防腐剂挑战试验并提供产品稳定性。特别优选的防腐剂是碘代丙炔基氨甲酸丁酯、苯氧乙醇、1,2-辛二醇、羟基苯乙酮、乙基己基甘油、己二醇、对羟基苯甲酸甲酯、对羟基苯甲酸丙酯、咪唑烷基脲、脱氢乙酸钠和苯甲醇。防腐剂的选择应该考虑所述组合物的用途以及所述防腐剂与乳液中其他成分之间可能的不相容性。防腐剂的使用量优选地为所述多重乳液总重量的0.01重量％至2重量％，包括其中包含的所有范围。1,2-辛二醇和苯氧乙醇或碘代丙炔基氨甲酸丁酯和苯氧乙醇的组合是优选的，其中苯氧乙醇和1,2-辛二醇共同且优选地占本发明的所述乳液或最终用途组合物的总重量的小于1.8重量％。还优选的是单独使用羟基苯乙酮或与其他防腐剂混合使用的防腐剂系统。
增稠剂适用于本发明的乳液。特别有用的是多糖。示例包括纤维、淀粉、天然/合成树胶和纤维素制品。淀粉的代表为化学改性的淀粉，如羟丙基淀粉磷酸钠和辛烯基琥珀酸铝淀粉。木薯淀粉通常是优选的，麦芽糊精也是。合适的树胶包括黄原胶、菌核胶、果胶、刺梧桐胶、阿拉伯胶、琼脂、瓜尔胶(包括Acacia senegal guar)、角叉菜胶、藻酸盐及其组合。合适的纤维素制品包括羟丙基纤维素、羟丙基甲基纤维素、乙基纤维素、羧甲基纤维素钠(纤维素胶/羧甲基纤维素)和纤维素(如纤维素微纤丝、纤维素纳米晶体或微晶纤维素)。纤维素微纤丝的来源包括次级细胞壁材料(如木浆、棉花)、细菌纤维素和初级细胞壁材料。优选地，初级细胞壁材料的来源选自果实、根、球茎、块茎、种子、叶及其组合的薄壁组织；更优选地选自柑橘类果实、番茄类果实、桃类果实、南瓜类果实、奇异果类果实、苹果类果实、芒果类果实、甜菜、甜菜根、芜菁、欧洲防风草、玉米、燕麦、小麦、豌豆及其组合；甚至更优选地选自柑橘类果实、番茄类果实及其组合。初级细胞壁材料的最优选来源是来自柑橘类果实的薄壁组织。柑橘类纤维，如
作为AQ Plus提供的那些，也可以用作纤维素微纤丝的来源。纤维素源可以通过任何已知的方法进行表面改性，包括在Colloidal PolymerScience中，Kalia等人，“Nanofibrillated cellulose:surface modification andpotential applications”(2014),Vol 292,Pages5-31中描述的方法。
合成聚合物是另一类有效的增稠剂。该类别包括交联的聚丙烯酸酯(如Carbomers)、聚丙烯酰胺(如
305)和牛磺酸共聚物(如
EG和
AVC)，所述共聚物分别被INCI命名为Sodium Acrylate/SodiumAcryloyldimethyl Taurate和Acryloyl Dimethyltaurate/Vinyl PyrrolidoneCopolymer。另一种适用于增稠的优选的合成聚合物是由Seppic市售的，并且以名称Simulgel INS100销售的丙烯酸酯基聚合物。也可以使用碳酸钙、气相二氧化硅和镁-铝-硅酸盐。
当使用时，基于所述多重乳液总重量，增稠剂的量可以为所述多重乳液的0.001至20重量％，优选地0.1至15重量％，最优选地0.2至10重量％，并且包括其中包含的所有范围。麦芽糊精、黄原胶和羧甲基纤维素通常是优选的。
香味剂、固定剂、螯合剂(如乙二胺四乙酸)、盐(如NaCl)和脱落剂可任选地包含在本发明的多重乳液中。这些物质中的每一种均可以为基于多重乳液总重量的约0.03至约5重量％，优选地0.1至3重量％，包括其中包含的所有范围。
常规保湿剂可以在本发明的多重乳液中用作添加剂(添加到所述多重乳液的纳米乳液和/或外水相中)，以在局部施用这类乳液时帮助保湿皮肤。这些通常为多元醇类材料。典型的多元醇包括甘油(即甘油(glycerine)或丙三醇(glycerin))、丙二醇、二丙二醇、聚丙二醇、聚乙二醇、山梨醇、羟丙基山梨醇、己二醇、1,3-丁二醇、异戊二醇、1,2,6-己三醇、乙氧基甘油、丙氧基化甘油及其混合物。最优选的是甘油、丙二醇或其混合物。所使用的保湿剂的量可以为所述多重乳液和/或所述纳米乳液的外水相的总重量的0.0至35重量％。通常，保湿剂占所述多重乳液的外水相的总重量和/或所述纳米乳液的总重量的0.0至20重量％，优选地0.001至15重量％，最优选地2至12重量％。当保湿剂在外水相和所述纳米乳液中均以15重量％或以上存在时，在一个实施方案中，基于所述多重乳液的总重量，多重乳液中防腐剂的总重量不超过1.3重量％(更优选地0.15至0.65重量％)。
当制备本发明的纳米乳液时，可以混合期望的成分以产生水相和油相。在室温至85℃的大气条件下，其可以在中等剪切力下与乳化剂混合。利用磁性搅拌棒进行，或在配有如叶轮(如，涡轮或锚)或由供应商(如Esco-Labs、AG、
或Charles Ross&Son)市售的转子/定子高剪切混合器的市售混合器中完成混合以制备所得的预纳米乳液(即，1-20微米的粗乳液)。混合的剪切速率可以变化，并且优选地设定为使得所得的预纳米乳液不会充气至显示可见气泡的程度。通常，用搅拌器或刮刀在35至500rpm，优选地40至250rpm，最优选地45至150rpm下进行混合以制备预纳米乳液。用转子/定子进行剪切以制备期望的油连续纳米乳液，这通常通过将转速设定为1000至8000rpm，优选地2000至7000rpm，最优选地2500至6250rpm来完成，包括其中包含的所有范围。
所得预纳米乳液的粘度通常为1,000至65,000cps，优选地为2,000至45,000cps，最优选地为5,000至35,000cps，包括其中包含的所有范围，其中使用Brookfield(DV-1+)粘度计在25℃温度并且设定为20RPM，RV6持续30秒来测量粗乳液的粘度。
此外，所述油连续纳米乳液可以通过将所得的预纳米乳液(或当有益剂为氨基酸时的预纳米乳液的混合物)在预混合后或同时加入高剪切混合器(如转子/定子)混合器或均质化器以产生本发明期望的油包水纳米乳液。这类纳米乳液同样具有100至850nm的颗粒液滴尺寸，包括其中包含的所有范围。在压力设定为50至2000，优选地250至1000，最优选地300至800psi(包括其中包含的所有范围)的情况下，一次通过均质化器(当选择均质化器时)后，令人惊讶地实现油连续纳米乳液制备。用于制备本发明的纳米乳液的优选装置是
转子/定子混合器或均质化器(如Sonic Sonolator)。在特别优选的实施方案中，并且当使用均质化器时，压力设定为50至1000psi。所得纳米乳液的粘度将落在750至55,000cps，优选地1,200至40,000cps，最优选地1,500至30,000cps的范围内，包括其中包含的所有范围。
将含或不含保湿剂的水与所得油连续纳米乳液(和具有8或更高HLB的乳化剂)组合，并在中等剪切力下混合，以产生本发明的多重乳液。所述多重乳液具有在用油制备的常规水包油乳液而不是油包水乳液范围内的粘度。通常，多重乳液的内相的油滴尺寸为1至35，优选地2至30，最优选地8至20微米，包括其中包含的所有范围。所述多重乳液的粘度通常为1,000至60,000cps，并且在另一个实施方案中为3,000至55,000cps，包括其中包含的所有范围。在另一个实施方案中，本发明的外水相中的水与保湿剂的重量比为70:30至55:45，包括其中包含的所有比率。
消费者可以将本发明的多重乳液用于局部施用于身体，尤其是头发或皮肤，最优选地用于保湿皮肤。
本发明的多重乳液的包装通常为瓶、管或罐。其他合适的包装包括泡罩包装或小袋。多个本发明也可以从自动分配器或用推进剂加压的包装中分配。
所提供的示例旨在促进对本发明的理解。它们不旨在限制权利要求的范围。
实施例1纳米乳液，1％胱氨酸(氨基酸作为有益剂)，油连续并且pH 7。
分别制备高pH(pH 12)预纳米乳液和低pH(pH 2.5)预纳米乳液。当制备所述高pH预纳米乳液时(表1a)，在水相中的所有成分在混合容器中组合并用磁力搅拌棒混合(在室温和中度剪切力下)，得到透明的混合物。在配有顶置搅拌器的单独混合容器中通过组合和混合成分(也在中度剪切力下和室温)制备油相。当所得混合物澄清时终止混合。随后将水溶液逐渐加入到具有所述油相的混合容器中，同时提供搅动/搅拌以混合两相。当获得均匀的混合物并且油连续粗乳液具有约10微米的颗粒尺寸之后，停止搅拌。
表1a.高pH预纳米乳液
| 重量％* | |
| 水相 | |
| 去离子水 | 平衡 |
| NaOH | 0.7 |
| NaCl | 0.4 |
| EDTA | 0.4 |
| 胱氨酸 | 1.4 |
| 油相 | |
| CCT** | 36.6 |
| DC ES-5300*** | 5.8 |
*基于高pH粗乳液的总重量
**辛酸癸酸甘油三酯
***有机硅乳化剂,Dow Corning
以类似于此实施例中所述高pH预纳米乳液所描述的方法制备低pH预纳米乳液，约10微米，(表1b)。
表1b.低pH粗乳液
*基于低pH粗乳液的总重量
**辛酸癸酸甘油三酯
***有机硅乳化剂,Dow Corning
将所得高pH和低pH粗乳液以2.6/1的比率在配有刮刀和转子/定子高剪切装置(ESCO-LABOR AG，瑞士)的1升ESCO混合器中分别混合2分钟，仅以约50至100RPM的速率使用刮刀。制备具有高pH和低pH粗乳液两者的混合物。
随后在相同的ESCO混合器中制备所述高和低pH预纳米乳液混合物，并且激活所述转子/定子以3000～6000rpm的速率剪切混合物长达5分钟，直至具有液滴尺寸为650nm的含有1重量％胱氨酸的纳米乳液形成。
表1c.含有1％胱氨酸的纳米乳液
*基于纳米乳液(颗粒尺寸为100nm)的总重量
**辛酸癸酸甘油三酯
***有机硅乳化剂,Dow Corning
实施例2
将实施例2的纳米乳液和如下成分组合和混合以制备多重乳液。
*来自实施例2
在室温25℃和大气压下，将所得混合物用设定为150rpm的金属叶轮进行剪切。回收具有15微米的水颗粒尺寸的多重乳液。多重乳液为约45重量％的外水相，约24重量％的油相和约31重量％的内水相。
实施例3
实施例2的多重乳液在45℃储存3个月。令人惊讶的是，在所述多重乳液的扫描电子显微镜后，没有观察到任何形式的脱水收缩、聚结或团聚。另外，评估了根据实施例2制备的多重乳液的粘度对比剪切速率曲线。意外地发现，尽管本发明的纳米乳液可以包含活性物质和/或保湿剂，但本发明的多重乳液的感官曲线与含有少于3重量％的甘油或者不含甘油的水包油乳液一致。
Claims (11)
1.一种包含多重乳液的化妆品组合物，该多重乳液包含：
(a)内相，其包括包含乳化剂的油包水纳米乳液，所述纳米乳液具有100至850nm的颗粒尺寸，并且进一步包含基于所述纳米乳液总重量的0.0至15重量％的油溶性有益剂、0.0至15重量％的水溶性有益剂和0.0至20重量％的保湿剂；和
(b)外水相，其包含水、基于所述外水相总重量的0.0至20重量％的保湿剂和0.0至15重量％的水溶性有益剂，
所述化妆品组合物包含基于所述化妆品组合物总重量的20至65重量％的纳米乳液，条件是所述纳米乳液和外水相不同时具有0.0重量％的保湿剂，并且其中所述多重乳液的纳米乳液的水相包含选自不溶性氨基酸的水不溶性有益剂，所述不溶性氨基酸选自苯丙氨酸、酪氨酸、色氨酸、胱氨酸或其混合物；并且其中所述水不溶性有益剂占所述多重乳液总重量的0.02至5重量％。
2.根据权利要求1所述的化妆品组合物，其中所述纳米乳液的油相包含0.01至15重量％的油溶性有益剂。
3.根据权利要求1或2所述的组合物，其中所述油溶性有益剂为维生素A、D、E、K、乙基己基甲氧基肉桂酸酯、双-乙基己氧苯酚甲氧苯基三嗪、2-乙基己基-2-氰基-3,3-二苯基-2-丙酸、甲酚曲唑三硅氧烷、3,3,5-三甲基环己基2-羟基苯甲酸酯、2-乙基己基-2-羟基苯甲酸酯或其混合物。
4.根据权利要求1-3所述的组合物，其中所述油溶性有益剂为4-苯乙基间苯二酚、4-环戊基间苯二酚、4-环己基间苯二酚、4-异丙基间苯二酚、4-环己基-5-甲基苯-1,3-二醇、4-异丙基-5-甲基苯-1,3-二醇或其混合物。
5.根据权利要求1-4所述的组合物，其中所述纳米乳液的水相和/或所述多重乳液的外水相包含0.001至10重量％的水溶性有益剂。
6.根据权利要求5所述的组合物，其中所述水溶性有益剂为精氨酸、缬氨酸、组氨酸、维生素B2、烟酰胺(维生素B3)、维生素B6、维生素C、抗坏血酸四异棕榈酸酯、抗坏血酸磷酸镁、抗坏血酸糖苷、4-乙基间苯二酚、鼠尾草提取物、芦荟提取物、绿茶提取物、葡萄籽提取物、百里香提取物、洋甘菊提取物、蓍草提取物、黄瓜提取物、甘草提取物、迷迭香提取物、恩索利唑或其混合物。
7.根据权利要求1-6所述的组合物，其中所述油溶性有益剂为omega-3脂肪酸、omega-6脂肪酸、氯咪巴唑、法呢醇、熊果酸、肉豆蔻酸、香叶基香叶醇、油基甜菜碱、椰油酰基羟乙基咪唑啉、己酰基鞘氨醇、12-羟基硬脂酸、岩芹酸、共轭亚油酸、萜品醇、百里酚视黄醇、视黄醛、视黄醇丙酸酯、视黄醇棕榈酸酯、视黄醇乙酸酯或其混合物。
8.根据权利要求1-7所述的组合物，其中所述纳米乳液中的水和/或所述外水相包含0.001-15重量％的保湿剂。
9.根据权利要求1-8所述的组合物，其中所述保湿剂为甘油。
10.权利要求1的所述组合物使皮肤保湿的用途。
11.根据权利要求1-9所述的组合物，其中通过包括以下步骤的方法制备所述多重乳液的内相的油包水纳米乳液：
制备具有10至14的pH的第一油包水粗乳液，以溶解所述水不溶性有益剂；将所述第一油包水粗乳液与具有2.5至4的pH且无有益剂的第二油包水粗乳液组合；将所述第一和第二粗乳液乳液以75:30至50:50的重量比混合；均质化或剪切所得的粗乳液的混合物，以产生油连续的纳米乳液。
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| EA201991003A1 (ru) * | 2016-12-21 | 2019-12-30 | Юнилевер Н.В. | Композиции для личной гигиены, содержащие малорастворимые соединения |
| WO2019224048A1 (en) * | 2018-05-23 | 2019-11-28 | Unilever Plc | Nanoemulsions and a method for making the same |
| CN109199878A (zh) * | 2018-09-26 | 2019-01-15 | 华南理工大学 | 一种美白防晒w/o/w多重乳液及其制备方法 |
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| CN1138982A (zh) * | 1994-12-06 | 1997-01-01 | 赫里尼·柯蒂斯公司 | 洗去型水包油包水组合物 |
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| CN109276515A (zh) * | 2018-10-30 | 2019-01-29 | 广州瑾洋化妆品有限公司 | 一种含有生物活性胶原肽的组合物及其制备方法与应用 |
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