CN116782872A - 制备多层球形颗粒的方法及包含由该方法制得的多层球形颗粒的化妆料组合物 - Google Patents
制备多层球形颗粒的方法及包含由该方法制得的多层球形颗粒的化妆料组合物 Download PDFInfo
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Abstract
本发明涉及一种制备多层球形颗粒的方法,更详细地,涉及一种包括以下步骤的制备多层球形颗粒的方法:i)制备包含有效成分的核成分和包含第一聚合物成分的壳溶液;ii)将所述步骤(i)的核成分和壳溶液通过电共挤出成型而形成核‑壳颗粒;iii)将所述步骤(ii)中获得的核‑壳颗粒进行干燥;和iv)用第二聚合物包封所述步骤(iii)的干燥的核‑壳颗粒。此外,本发明涉及一种包含由所述方法制得的多层球形颗粒的化妆料组合物。
Description
技术领域
本发明涉及一种制备多层球形颗粒的方法,更详细地,涉及一种包括以下步骤的制备多层球形颗粒的方法:i)制备包含有效成分的核成分和包含第一聚合物成分的壳溶液;ii)将所述步骤(i)的核成分和壳溶液通过电共挤出成型(electro-coextrusion)而形成核-壳颗粒;iii)将所述步骤(ii)中获得的核-壳颗粒进行干燥;和iv)用第二聚合物包封所述步骤(iii)的干燥的核-壳颗粒。
此外,本发明涉及一种包含由所述方法制得的多层球形颗粒的化妆料组合物。
背景技术
近年来,随着化妆品的多样化,消费者开始对化妆品的功效以及美学功能提出要求。因此,化妆品开发商正在努力创造具有多功能和易于使用的有效的产品以及美学上优越的产品。
另外,作为一种更稳定地递送有效成分(活性成分)的方法,有封装(encapsulation)技术。封装是将功能性物质捕获在由聚合物组成的小结构体中,以实现物理化学稳定性、挥发性和气味抑制、分散性的提高、通过固化来扩大应用范围以及控制释放带来的毒性的降低和功能性效果的提升等的技术。这种封装结构体通常具有由核-壳(core-shell)组成的胶囊形式或由核-基质(core-matrix)组成的颗粒形式。这种封装技术目前还没有在化妆品领域中得到积极应用。
发明内容
要解决的技术问题
因此,本发明的技术问题是提供一种可制备多层球形颗粒的方法,所述多层球形颗粒可以将化妆品成分以稳定的形式有效地递送至皮肤中,并且可以赋予在外观上的优异的美感。
此外,本发明的另一个技术问题是提供一种包含由所述方法制得的多层球形颗粒的化妆料组合物。
技术方案
为了解决上述技术问题,本发明提供了一种制备多层球形颗粒的方法,其包括以下步骤:
i)制备包含有效成分的核(core)成分和包含第一聚合物成分的壳(shell)溶液;
ii)将所述步骤(i)的核成分和壳溶液通过电共挤出成型而形成核-壳颗粒;
iii)将所述步骤(ii)中获得的核-壳颗粒进行干燥;和
iv)用第二聚合物包封所述步骤(iii)的干燥的核-壳颗粒。
此外,为了解决另一个技术问题,本发明提供了一种包含由所述方法制得的多层球形颗粒的化妆料(cosmetic)组合物。
以下,对本发明进行详细的说明。
根据本发明的一个方面,提供了一种制备多层球形颗粒的方法,其包括以下步骤:i)制备包含有效成分的核成分和包含第一聚合物成分的壳溶液;ii)将所述步骤(i)的核成分和壳溶液通过电共挤出成型而形成核-壳颗粒;iii)将所述步骤(ii)中获得的核-壳颗粒进行干燥;和iv)用第二聚合物包封所述步骤(iii)的干燥的核-壳颗粒。
在根据本发明的制备多层球形颗粒的方法的步骤(i)中,制备了包含有效成分的核成分和包含第一聚合物成分的壳溶液。
在根据本发明的一个具体实施方案中,所述有效成分可以选自例如油、蜡、烃、高级脂肪酸、高级醇、硅酮、酯及它们的混合物,但并不受限于此。
在根据本发明的另一个具体实施方案中,所述油可以使用例如澳洲坚果油、橄榄油、荷荷巴油、葵花籽油、摩洛哥坚果油、山茶油、鳄梨油、大豆油(soybean oil)、葡萄籽油、蓖麻油、米糠油(rice bran oil)等,但并不受限于此。
在根据本发明的另一个具体实施方案中,所述蜡可以使用例如巴西棕榈蜡(carnauba wax)、小烛树蜡(candelilla wax)、荷荷巴油、蜂蜡、羊毛脂(lanolin)等,但并不受限于此。
在根据本发明的另一个具体实施方案中,所述烃可以使用例如液体石蜡、石蜡、凡士林(VaselineTM,petroleum jelly)、地蜡(ceresin)、微晶蜡(microcrystalline wax)、角鲨烷(squalane)等,但并不受限于此。
在根据本发明的另一个具体实施方案中,所述高级脂肪酸可以使用例如月桂酸(lauric acid)、肉豆蔻酸(myristic acid)、棕榈酸(palmitic acid)、硬脂酸(stearicacid)、异硬脂酸(isostearic acid)等,但并不受限于此。
在根据本发明的另一个具体实施方案中,所述高级醇可以使用例如鲸蜡醇、硬脂醇、异硬脂醇、2-辛基十二醇、苹果酸二异硬脂醇(diisostearyl malate)等,但并不受限于此。
在根据本发明的另一个具体实施方案中,所述硅酮可以使用例如聚二甲基硅氧烷(polydimethylsiloxane)、环甲基硅油、硅酮聚合物、硅油等,但并不受限于此。
在根据本发明的另一个具体实施方案中,所述酯可以使用例如十六烷基乙基己酸酯(cetyl ethylhexanoate)、PEG-20甘油三异硬脂酸酯(peg-20glyceryltriisostearate)、癸酸/辛酸甘油三酯(capric/caprylic triglyceride)、2-乙基己酸三甘油酯(glyceryl tri(2-ethylhexanoate))、异壬酸异壬酯(isononyl isononanoate)、异壬酸乙基己酯(ethylhexyl isononanoate)、棕榈酸乙基己酯(ethylhexyl palmitate)、异硬脂酸异硬酯(isostearyl isostearate)、新戊二醇二癸酸酯(neopentyl glycoldicaprate)、新戊二醇二乙基己酸酯(neopentyl glycol diethylhexanoate)、辛基十二烷基肉豆蔻酸酯(octyldodecyl myristate)、季戊四醇四乙基己酸酯(pentaerythrityltetraethylhexanoate)、季戊四醇四异硬脂酸酯(pentaerythrityl tetraisostearate)、异壬酸异十三烷基酯(isotridecyl isononanoate)、三羟甲基丙烷三异硬脂酸酯(trimethylolpropane triisostearate)、角鲨烷(squalene)等,但并不受限于此。
在根据本发明的另一个具体实施方案中,所述有效成分是油溶性(oil-soluble)化妆品成分,例如,可以使用视黄醇、视黄醛、油溶性甘草酸(glycyrrhizicacid)、cica粉(cica powder)、辅酶Q10、虾青素(astaxanthin)、艾地苯醌(idebenone)、共轭亚油酸(CLA)、维生素E(生育酚)、维生素D、亚麻酸(linolenic acid)、生物素(biotin)等。
在根据本发明的另一个具体实施方案中,所述有效成分可以与共价有机骨架(covalent organic framework,COF)形成复合物。共价有机骨架是具有扩展结构的二维或三维有机固体,其中构造块(building blocks)由强共价键连接。在根据本发明的另一个具体实施方案中,所述有效成分可以例如与基于环糊精(cyclodextrin)的共价有机骨架形成复合物。
在根据本发明的另一个具体实施方案中,所述第一聚合物可以选自纳米纤维素、纤维素、羟乙基纤维素、微晶纤维素、淀粉(starch)、聚甲基丙烯酸甲酯(PMMA)、黄原胶、卡波姆(CarbomerTM,poly(acrylic acid))、丙烯酸酯/C10-30烷基丙烯酸酯交联聚合物、阿拉伯树胶、瓜尔胶(guar gum)、聚乙烯醇(PVA)、聚乙烯吡咯烷酮(PVP)、明胶、透明质酸、胶原蛋白、普鲁兰多糖、聚乙交酯(PGA)、琼脂(agar)、阿拉伯树胶、角叉菜胶、吉兰糖胶(gellangum)、刺梧桐树胶(karaya gum)、甲基纤维素、槐豆胶(locust bean gum)、藻朊酸盐、海藻酸钠、葡甘露聚糖、琥珀酰壳聚糖、普鲁兰多糖丙交酯、壳聚糖、聚乙二醇(PEG)-聚己内酯(PCL)-聚乙二醇(PEG)的三嵌段共聚物、泊洛沙姆407(PluronicTMF-127)、乙酰羟丙基纤维素及它们的混合物,但并不受限于此。
在根据本发明的另一个具体实施方案中,所述第一聚合物可以使用两种以上的聚合物的混合物。
在根据本发明的另一个具体实施方案中,所述第一聚合物可以使用三种以上的聚合物的混合物。
在根据本发明的另一个具体实施方案中,所述壳溶液中第一聚合物的浓度可以为1-50重量%、2-45重量%或5-40重量%。
在根据本发明的制备多层球形颗粒的方法的步骤(ii)中,将包含有效成分的核成分和包含第一聚合物成分的壳溶液通过电共挤出成型而形成核-壳颗粒。
在电共挤出成型中,彼此不同的物质在电场下从两个同轴毛细管中流出并形成由核-壳组成的胶囊(图1)。由于要被包封的中心物质(核)的特性的影响小,可以容易地应用于各种功能性物质或它们的混合物的封装,并且封装效率非常优异。
在根据本发明的另一个具体实施方案中,所述核成分的电共挤出成型可以以0.1-10mL/分钟、0.2-8mL/分钟或0.5-5mL/分钟的流速(flow rate)进行。
在根据本发明的另一个具体实施方案中,所述壳溶液的电共挤出成型可以以0.5-20mL/分钟、1-15mL/分钟或3-12mL/分钟的流速进行。
在根据本发明的另一个具体实施方案中,所述电共挤出成型可以在1000-5000伏特(V)、1500-4000伏特(V)或2000-3000伏特(V)下进行。
在根据本发明的另一个具体实施方案中,所述电共挤出成型中可以使用氯化钙(calcium chloride)溶液作为固化剂。
在根据本发明的制备多层球形颗粒的方法的步骤(iii)中,将步骤(ii)中获得的核-壳颗粒进行干燥。
在根据本发明的另一个具体实施方案中,所述核-壳颗粒的干燥可以在60-90℃下进行。
在根据本发明的制备多层球形颗粒的方法的步骤(iv)中,用第二聚合物包封(encapsulation)步骤(iii)中获得的干燥的核-壳颗粒以制备多层球形颗粒。
用所述第二聚合物包封可以通过本领域中已知的方法进行,并且不作特别限制。
在根据本发明的另一个具体实施方案中,所述第二聚合物是可以可以充当化妆品成分的聚合物,例如可以选自胶原蛋白、透明质酸、普鲁兰多糖、蛋白多糖、β-葡聚糖、葡聚糖、聚谷氨酸、壳聚糖及它们的混合物,但并不受限于此。
在根据本发明的另一个具体实施方案中,由所述方法制备的多层球形颗粒的直径可以为200-1500μm。
根据本发明的另一个方面,提供了一种包含由所述方法制得的多层球形颗粒的化妆料组合物。
在本发明中,化妆料组合物可以配制成各种产品,如化妆水、乳液、身体乳液、面霜、精华、安瓿和BB(遮瑕霜)霜等,但并不受限于此。本发明中化妆料组合物可以根据剂型的需要包含不同含量的多层球形颗粒,例如可以包含含量为0.1-50重量%的多层球形颗粒。
有益效果
本发明可以以优异的包封效率和各种有效成分的高生产效率制备多层球形颗粒,根据本发明制得的多层球形颗粒可以将有效成分以稳定的形式有效地递送至皮肤中,而且可以赋予在外观上的优异的美感。
附图说明
图1是电共挤出成型设备的示意图。
图2是放大拍摄实施例1中制得的多层球形颗粒的照片。
图3是测量实施例1中制得的多层球形颗粒的粒度的结果。
具体实施方式
以下,通过实施例,对本发明进行更具体的说明。但是,以下实施例仅仅是为了帮助理解本发明而例示的,本发明的范围并不受限于此。
实施例1:利用明胶/阿拉伯树胶/卡波姆的多层球形颗粒的制备
根据以下表1的组成,由成分A制备壳溶液,并且通过将成分B的核成分和作为固化剂的1%氯化钙溶解在纯化水中来制备溶液。然后,使用封装器(Encapsulator)B-390(Buchi公司,瑞士),在以下条件下使用上述溶液进行电共挤出成型,从而获得核-壳颗粒。
–喷嘴(Nozzle):150μm(核),400μm(壳)
–流速(Flow rate):1.5mL/分钟(核),10mL/分钟(壳)
–频率(Frequency):600Hz
–压力(Pressure):0.5巴
–振幅(Amplitude):3
–充电(Charge):2300V
在80℃下,将获得的核-壳颗粒干燥12小时,然后将干燥的核-壳颗粒放入容器中,然后向其中缓慢加入成分C,用带翼分散器将它们混合10分钟来进行包封,从而制备多层球形颗粒。
[表1]
实施例2:利用藻朊酸盐/纳米纤维素/卡波姆的多层球形颗粒的制备
根据以下表2的组成,通过与实施例1中所述相同的方法制备多层球形颗粒。
[表2]
实施例3:利用藻朊酸盐/阿拉伯树胶/角叉菜胶的多层球形颗粒的制备
根据以下表3的组成,通过与实施例1中所述相同的方法制备多层球形颗粒。
[表3]
实施例4:利用黄原胶/PVA/卡波姆的多层球形颗粒的制备
根据以下表4的组成,通过与实施例1中所述相同的方法制备多层球形颗粒。
[表4]
实施例5:利用PVP/瓜尔胶/丙烯酸酯/C10-30烷基丙烯酸酯交联聚合物的多层球
形颗粒的制备
根据以下表5的组成,通过与实施例1中所述相同的方法制备多层球形颗粒。
[表5]
实施例6:利用阿拉伯树胶/吉兰糖胶/槐豆胶的多层球形颗粒的制备
根据以下表6的组成,通过与实施例1中所述相同的方法制备多层球形颗粒。
[表6]
实施例7:利用葡甘露聚糖/吉兰糖胶/卡波姆的多层球形颗粒的制备
根据以下表7的组成,通过与实施例1中所述相同的方法制备多层球形颗粒。
[表7]
实施例8:利用琥珀酰壳聚糖/普鲁兰多糖丙交酯/卡波姆的多层球形颗粒的制备
根据以下表8的组成,通过与实施例1中所述相同的方法制备多层球形颗粒。
[表8]
实施例9:利用琥珀酰壳聚糖/PEG-PCL-PEG/卡波姆的多层球形颗粒的制备
根据以下表9的组成,通过与实施例1中所述相同的方法制备多层球形颗粒。
[表9]
实施例10:利用琥珀酰壳聚糖/纳米纤维素/卡波姆的多层球形颗粒的制备
根据以下表10的组成,通过与实施例1中所述相同的方法制备多层球形颗粒。
[表10]
实施例11:利用琥珀酰壳聚糖/乙酰羟丙基纤维素/卡波姆的多层球形颗粒的制备
根据以下表11的组成,通过与实施例1中所述相同的方法制备多层球形颗粒。
[表11]
实施例12:利用琥珀酰壳聚糖/泊洛沙姆407/卡波姆的多层球形颗粒的制备
根据以下表12的组成,通过与实施例1中所述相同的方法制备多层球形颗粒。
[表12]
实施例13和比较例:含有和不含有多层球形颗粒的润肤乳的制备
根据以下表13的组成,将各成分引入容器中,在80℃的温度下进行溶解,然后利用均质混合器混合5分钟后进行冷却、脱气,从而获得润肤乳。
[表13]
实施例14:含有多层球形颗粒的身体乳液的制备
根据以下表14的组成,将各成分引入容器中,在80℃的温度下进行溶解,然后利用均质混合器混合5分钟后进行冷却、脱气,从而获得身体乳液。
[表14]
实施例15:含有多层球形颗粒的面霜的制备
根据以下表15的组成,将各成分引入容器中,在80℃的温度下进行溶解,然后利用均质混合器混合5分钟后进行冷却、脱气,从而获得面霜。
[表15]
实施例16:含有多层球形颗粒的精华的制备
根据以下表16的组成,将各成分引入容器中,在80℃的温度下进行溶解,然后利用均质混合器混合5分钟后进行冷却、脱气,从而获得精华。
[表16]
实施例17:含有多层球形颗粒的透明精华的制备
根据以下表17的组成,将各成分引入容器中,在80℃的温度下进行溶解,然后利用均质混合器混合5分钟后进行冷却、脱气,从而获得透明精华。
[表17]
实施例18:含有多层球形颗粒的BB面霜的制备
用三辊碾磨设备通过处理3次来制备成分A,将成分B加入制备部中加热至75-80℃,然后加入用三辊碾磨设备处理过的成分A并使其分散。在单独的容器中溶解成分C,然后用均质混合器搅拌的同时加热至80-85℃。将成分C加入到上述制得的成分中,并将混合物乳化10分钟。在乳化完成后,利用搅拌器进行搅拌的同时将所得产物冷却至45℃,然后再次冷却至25℃,然后放入容器中进行熟化。
[表18]
/>
实验例1:多层球形颗粒的粒度的测量
利用粒度仪(Mastersizer 2000,马尔文(MLAVERN)公司,英国)测量实施例1中制得的多层球形颗粒的尺寸,并将其结果示于图3中。根据测量结果,可知粒度为438-1092μm。
实验例2:视黄醇含量变化的测量
在保持25℃下的遮光条件和40℃下的曝光(Lightexposure)条件的同时以7天的间隔定量分析实施例13和比较例的润肤乳中的视黄醇的含量的变化,持续一个月。此时使用的仪器是HPLC(沃特世(Waters)公司,美国),分析条件如下。将分析的结果示于表19中,在40℃下的曝光条件记载于括号中。
–检测(Detection):紫外分光光度计(UV-Spectrophotometer)(325nm)
–色谱柱(Column):C18(3.9×150mm)
–流速:1.0mL/分钟
–流动相(Mobile phase):甲醇(Methanol):H2O(90:10)
[表19]
天数 | 0 | 7 | 13 | 22 | 29 | 35 |
实施例13 | 100(100) | 98(99) | 97(95) | 94(92) | 92(88) | 90(86) |
比较例 | 100(100) | 90(90) | 85(84) | 65(60) | 60(32) | 45(20) |
(视黄醇残留含量%)
实验例3:经皮吸收促进效果实验
将作为人造皮肤的的Neoderm(Tego Science公司,韩国)安装在弗兰兹型扩散池(Franz-type diffusion cell)(Lab fine instruments公司,韩国)中并进行实验。在弗兰兹型扩散池的接收(receptor)池(5mL)中加入50mM的磷酸盐缓冲液(pH为7.4,0.1M的NaCl),然后在32℃下将扩散池(diffusion cell)以600rpm进行混合并分散,并将50μl的实施例13的润肤乳和比较例的润肤乳加入供给(donor)池中。按照预定的时间进行吸收和扩散,发生吸收和扩散的皮肤面积设为0.64cm2。有效成分的吸收和扩散结束后,利用干燥的KimwipesTM或10ml的乙醇清除掉未被吸收并残留在皮肤上的残留物,并使用尖端型均质机(homogenizer),将吸收并扩散有有效成分的皮肤进行磨碎,然后使用4ml的二氯甲烷提取吸收到皮肤内部的视黄醇。之后,利用0.45μm的尼龙膜(nylon membrane)过滤器对提取液进行过滤,并通过高效液相色谱(HPLC)法在以下条件下测量视黄醇的含量后将其结果示于表20中。
[表20]
从表20可知,与常规的润肤乳相比,根据本发明的润肤乳的经皮吸收更优异。
实验例4:皮肤保湿力的测量
涂覆实施例13和比较例的润肤乳后,使用Corneometer CM850(Courage+Khazakaelectronic GmbH,德国)测量保湿力,并将其结果示于表21中。从表21可知,与不添加多层球形颗粒的润肤乳相比,含有多层球形颗粒的润肤乳具有更优异的保湿力。
[表21]
(Corneometer/任意单位)。
Claims (14)
1.一种制备多层球形颗粒的方法,其包括以下步骤:
i)制备包含有效成分的核成分和包含第一聚合物成分的壳溶液;
ii)将所述步骤(i)的核成分和壳溶液通过电共挤出成型而形成核-壳颗粒;
iii)将所述步骤(ii)中获得的核-壳颗粒进行干燥;和
iv)用第二聚合物包封所述步骤(iii)的干燥的核-壳颗粒。
2.根据权利要求1所述的制备多层球形颗粒的方法,其特征在于,所述步骤(i)的有效成分选自油、蜡、烃、高级脂肪酸、高级醇、硅酮、酯及它们的混合物。
3.根据权利要求2所述的制备多层球形颗粒的方法,其特征在于,所述步骤(i)的有效成分与共价有机骨架(COF)形成复合物。
4.根据权利要求1所述的制备多层球形颗粒的方法,其特征在于,所述步骤(i)的第一聚合物选自纳米纤维素、纤维素、羟乙基纤维素、微晶纤维素、淀粉、聚甲基丙烯酸甲酯(PMMA)、黄原胶、卡波姆、丙烯酸酯/C10-30烷基丙烯酸酯交联聚合物、阿拉伯树胶、瓜尔胶、聚乙烯醇(PVA)、聚乙烯吡咯烷酮(PVP)、明胶、透明质酸、胶原蛋白、普鲁兰多糖、聚乙交酯(PGA)、琼脂、阿拉伯树胶、角叉菜胶、吉兰糖胶、刺梧桐树胶、甲基纤维素、槐豆胶、藻朊酸盐、海藻酸钠、葡甘露聚糖、琥珀酰壳聚糖、普鲁兰多糖丙交酯、壳聚糖、聚乙二醇(PEG)-聚己内酯(PCL)-聚乙二醇(PEG)的三嵌段共聚物、泊洛沙姆407、乙酰羟丙基纤维素及它们的混合物。
5.根据权利要求1所述的制备多层球形颗粒的方法,其特征在于,所述步骤(i)的壳溶液中第一聚合物的浓度为1-50重量%。
6.根据权利要求1所述的制备多层球形颗粒的方法,其特征在于,所述步骤(ii)中核成分的电共挤出成型以0.1-10mL/分钟的流速进行。
7.根据权利要求1所述的制备多层球形颗粒的方法,其特征在于,所述步骤(ii)中壳溶液的电共挤出成型以0.5-20mL/分钟的流速进行。
8.根据权利要求1所述的制备多层球形颗粒的方法,其特征在于,所述步骤(ii)的电共挤出成型在1000-5000伏特(V)下进行。
9.根据权利要求1所述的制备多层球形颗粒的方法,其特征在于,所述步骤(ii)的电共挤出成型中使用氯化钙溶液作为固化剂。
10.根据权利要求1所述的制备多层球形颗粒的方法,其特征在于,所述步骤(iii)的干燥在60-90℃下进行。
11.根据权利要求1所述的制备多层球形颗粒的方法,其特征在于,所述步骤(iv)的第二聚合物选自胶原蛋白、透明质酸、普鲁兰多糖、蛋白多糖、β-葡聚糖、葡聚糖、聚谷氨酸、壳聚糖及它们的混合物。
12.根据权利要求1所述的制备多层球形颗粒的方法,其特征在于,所述制得的多层球形颗粒的直径为200-1500μm。
13.一种化妆料组合物,其包含根据权利要求1至12中任一项所述的方法制得的多层球形颗粒。
14.根据权利要求13所述的化妆料组合物,其中,所述多层球形颗粒的含量为0.1-50重量%。
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