CN116059131B - 一种专用于氧化锌分散浆的成膜抑菌组合物及其制备方法和应用 - Google Patents
一种专用于氧化锌分散浆的成膜抑菌组合物及其制备方法和应用 Download PDFInfo
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- CN116059131B CN116059131B CN202211707311.2A CN202211707311A CN116059131B CN 116059131 B CN116059131 B CN 116059131B CN 202211707311 A CN202211707311 A CN 202211707311A CN 116059131 B CN116059131 B CN 116059131B
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- UNXRWKVEANCORM-UHFFFAOYSA-I triphosphate(5-) Chemical compound [O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O UNXRWKVEANCORM-UHFFFAOYSA-I 0.000 description 1
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- UFBIICBJIGGTEJ-UHFFFAOYSA-N zinc 2-hydroxybenzoic acid oxygen(2-) Chemical compound [O-2].[Zn+2].C(C=1C(O)=CC=CC1)(=O)O UFBIICBJIGGTEJ-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明提供了一种专用于氧化锌分散浆的成膜抑菌组合物及其制备方法和应用,属于精细化工中的化妆品技术领域。本发明通过在氧化锌分散浆中加入一定比例的壳聚糖及其衍生物等成膜剂和疏水组合物,制备得到的氧化锌分散浆的粉末相‑液体相分层效果较好,氧化锌粉体状态均匀,且形成的生物膜状态稳定,在不降低壳聚糖的抑菌性能同时还能具有较好的疏水性能,针对痤疮丙酸杆菌的抑菌效率达到99.9%。
Description
技术领域
本发明涉及精细化工中的化妆品技术领域,特别涉及一种专用于氧化锌分散浆的成膜抑菌组合物及其制备方法和应用。
背景技术
氧化锌是两性化合物,在诸多领域都有着广泛的应用,因其成本低廉、安全无毒,并且兼具屏蔽紫外线和除异味等功能,在化妆品、饲料助剂、纺织品等领域获得了广泛的商业化应用。尤其在化妆品领域备受欢迎,因氧化锌有着诸多功效,对皮肤具有良好的控油、收敛、消炎、抗紫外线以及抑菌等功能,可以代替部分酒精的添加,较少产生刺激性等安全问题。但氧化锌无附着力,作为功效成份单独涂敷到脸上容易脱落,导致作用时间较短而无法发挥功效。或氧化锌在以水或乙醇为溶剂的溶液中常容易出现析出,影响了氧化锌的应用。
壳聚糖具有广谱抗菌性、生物相容性、生物降解性,成膜性好。其作为功能性成分易于被人体吸收,在生物医学材料、食品和化妆品等领域具有较大的应用价值。但是壳聚糖的水溶性极差,也不溶于碱和大多数有机溶剂,壳聚糖自身形成的膜,抗水性能弱。CN105384974A公开了一种壳聚糖生物膜,以天然多糖壳聚糖为主要原料,添加天然抗菌物质或者辅助抗菌物质(氧化锌)增强壳聚糖的抗菌性能,将此膜应用于食品包装中,具有安全、高效、无污染、延长产品货架期等显著优点,但该专利着重在生物膜的抗菌抑菌性能探究,未对生物膜的抗水性能进行研究。
纯的水杨酸应用于化妆品时,溶解性差,水杨酸在水中属于微溶,对配方的运用会有一定的局限性。目前解决上面问题可以采用壳聚糖、水杨酸和聚苯乙烯磺酸钠在氧化锌的水醇溶液中配合使用的化妆品来解决,但是水杨酸、壳聚糖和聚苯乙烯磺酸钠三者在一般情况下是不能兼容的。
因此,本申请设计了一种专用于氧化锌分散浆的成膜抑菌组合物及其制备方法和应用。
发明内容
本发明提供了一种专用于氧化锌分散浆的成膜抑菌组合物及其制备方法和应用,其目的是为了解决:壳聚糖形成的膜,抗水性弱;水杨酸在水中的溶解性差;壳聚糖加入含有氧化锌的水醇溶液中,氧化锌的水醇溶液不再分层,氧化锌聚集导致产品外观状态改变;氧化锌等功效物停留时间短,作用时间短,涂敷到脸上容易脱落等问题。
为了达到上述目的,本发明的实施例提供了一种专用于氧化锌分散浆的成膜抑菌组合物及其制备方法和应用,通过在氧化锌分散浆中加入一定比例的壳聚糖及其衍生物等成膜剂和疏水组合物,制备得到的氧化锌分散浆的粉末相-液体相分层效果较好,氧化锌粉体状态均匀,且形成的生物膜状态稳定,在不降低壳聚糖的抑菌性能同时还能具有较好的疏水性能,针对痤疮丙酸杆菌的抑菌效率达到99.9%。
本发明一方面提供了一种专用于氧化锌分散浆的成膜抑菌组合物,所述专用于氧化锌分散浆的成膜抑菌组合物包括按重量百分数计的以下组分:氧化锌分散浆5~25%,成膜剂0.01~1%,疏水组合物0.01~10%;
所述氧化锌分散浆为氧化锌加入到乙醇水溶液中形成的粉末相-液体相双层产品;
所述疏水组合物为有机酸和亲水-亲油两性高分子聚合物的组合。
优选地,所述有机酸为水杨酸,添加量为0.05~2%。
优选地,所述亲水-亲油两性高分子聚合物为水溶性聚苯乙烯类,添加量为0.01~10%。
优选地,所述成膜剂为改性淀粉类、纤维素胶类、壳聚糖及其盐类、羧甲基壳聚糖、水溶性聚苯乙烯类、分子量小于120万的多糖类。更为优选地,壳聚糖为羧甲基脱乙酰壳多糖(水溶的)。
优选地,所述成膜抑菌组合物为5~25%氧化锌、1~50%乙醇、0.01~1%壳聚糖、0.01~10%聚苯乙烯磺酸钠、0.05~2%水杨酸,余下为水。
更为优选地,所述成膜抑菌组合物为18%氧化锌、30%乙醇、0.2%壳聚糖、0.5%聚苯乙烯磺酸钠、1%水杨酸,余下为水。
基于一个发明总的构思,本发明提供了上述专用于氧化锌分散浆的成膜抑菌组合物的制备方法,包括如下步骤:
步骤一:将水杨酸加入乙醇中溶解均匀得到溶液A;
步骤二:依次将水、氧化锌加入所述溶液A中,混合均匀,获得溶液B;
步骤三:向所述溶液B中加入成膜剂、亲水-亲油两性高分子聚合物,搅拌均匀,静置,获得专用于氧化锌分散浆的成膜抑菌组合物。
本发明还提供了上述制备方法制得的成膜抑菌组合物在氧化锌分散体系中的应用。
优选地,所述成膜抑菌组合物在氧化锌分散体系中的功能包括氧化锌分散体系成膜稳定,氧化锌粉体状态均匀,氧化锌生物膜具有疏水性,氧化锌生物膜兼具防水和抑菌性能。
优选地,所述成膜抑菌组合物应用到氧化锌分散体系中对痤疮丙酸杆菌的抑菌率达到99.9%。
壳聚糖(结构如下)无毒无味,是一种大分子直链高聚物,可从蚕蛹、蛋壳以及海洋生物的贝壳中提取,由于其自身独特的理化特性使壳聚糖拥有广泛的应用范围,主要源于质子化氨基以及其他官能团能参与不同的键合。氨基被质子化后,不仅能与含有强电负性原子(氧、氮)的化学活性物质或呈负电性的离子或基团以氢键或静电作用形式结合生成聚合物,还可与许多阴离子如钼酸根离子、钒酸根离子、或含阴离子基团的物质如苯甲酸三聚磷酸钠结合形成新物质,称为离子交联反应,这种交联可增加壳聚糖抵御化学降解的能力。
壳聚糖又称脱乙酰甲壳素,是由甲壳素经脱乙酰化反应得到的一种多糖类有机聚合物。壳聚糖的成膜性能好,具有广谱抗菌性,生物相容性以及生物降解性,广泛应用于食品领域,作为一种功能性成分被人体吸收。
氧化锌是两性化合物,在诸多领域都有广泛的应用,氧化锌在化妆品领域也有着诸多功效,对皮肤具有良好的控油、收敛、消炎、抗紫外线以及抑菌等功能,可以代替部分酒精的添加,较少产品的刺激性等安全问题。作为一种可吸收降解的环境友好型生物高分子,壳聚糖被认为是最有效的抗菌生物聚合物之一。特殊的功能和结构使壳聚糖在生物医学材料和食品等领域具有潜在的应用价值。但是壳聚糖的水溶性极差,也不溶于碱溶液和大多数有机溶剂,因此其应用受到限制。为改善壳聚糖的溶解性,可对其进行改性。壳聚糖改性方法包括物理改性、化学改性和复合改性,化学改性主要有烷基化、酰基化、醚化、席夫碱化及接枝共聚等方法。本专利优选羧基化改性以及壳聚糖季铵盐化改性。壳聚糖的改性可以极大地改善壳聚糖的水溶性、生物相容性、抗菌性等,使壳聚糖的利用价值和应用范围得到提高和扩大。
水溶性的聚苯乙烯磺酸钠(PSS)(结构如下)是一种具有良好表面活性作用的高分子聚合物,近年来在工业废水处理中作为助凝剂、聚合物接枝改性、晶体形貌生长调节剂、化妆品等领域。作为有机磺酸盐,由于其具有亲正离子基团-SO3-和疏水烃链,可以作为吸附剂,很好的吸附在含有正电荷的物体表面。
水杨酸(结构如下)是一种化妆品中经常使用,β-羟基的脂溶性有机酸,广泛存在于自然界中,如柳树树皮、白珠树树叶以及甜桦树等,同时是重要的精细化工原料。在化妆品行业中,水杨酸具有剥脱角质,加速表皮更新,光滑皮肤,淡化色斑、清除粉刺痤疮、溶解角栓、改善毛孔堵塞等功效。此外,在祛痘产品中,水杨酸可以抑制和杀灭导致皮肤感染的痤疮丙酸杆菌等菌,能够有效改善和治疗痤疮。然而,水杨酸存在水分散性差、遇光易氧化变色、高温不稳定和生物利用度低等缺点,在护肤品中难以达到有效浓度,导致产品效果不佳。其次,如果产品中添加了高浓度的水杨酸,对皮肤有很强的刺激性,使用后会产生红斑、瘙痒、刺痛等现象。因此,为了克服水杨酸在化妆品配制和使用中的缺点、同时提高其生物利用度,亟待研究开发稳定且低刺激的水杨酸的使用方法,使其有效发挥护肤功效。
本发明的反应机理为:氧化锌表面带有正电荷,在溶液干燥成膜的过程中,吸引水杨酸上的羧基和聚苯乙烯磺酸钠上的阴离子基团聚苯乙烯磺酸根,而暴露出苯酚和聚苯乙烯的结构,大大提高氧化锌自身的抗水性能,同时氧化锌本身的抗菌抑菌能力,可以协同壳聚糖、水杨酸的成膜性,大大增加抑菌效果,还可以隔绝污染源,减少微生物的二次污染。
本发明的上述方案有如下的有益效果:
本发明在护肤品中的应用,氧化锌粉末在水-乙醇体系中形成生物膜,在不改变产品外观状态的情况下,既具有疏水性能、又具有抑菌性能,提升功效物的驻留时间,提升产品功效。具体表现为涂抹该组合物,酒精挥发后,会在皮肤上形成一层膜,而壳聚糖、氧化锌、水杨酸、聚苯乙烯磺酸钠形成的膜具有较强抗水性能,通过接触角表征,三者的接触角远优于单一原料。
壳聚糖、水杨酸、聚苯乙烯磺酸钠三者,一般情况下是不能兼容的,因为壳聚糖跟水杨酸在溶液中呈阴离子,只有加入氧化锌后,阴阳离子反应,体系获得均衡。而聚苯乙烯磺酸钠加入氧化锌的乙醇水溶液中,是不分层的,只有加入水杨酸才会分层,使得体系具有稳定分层的外观,且上层溶液澄清。也就是说壳聚糖、聚苯乙烯磺酸钠和水杨酸三者组合可以使得氧化锌的乙醇水溶液达到稳定且分层的外观。
具体实施方式
为使本发明要解决的技术问题、技术方案和优点更加清楚,下面将结合具体实施例进行详细描述。
除非另有定义,下文中所使用的所有专业术语与本领域技术人员通常理解含义相同。本文中所使用的专业术语只是为了描述具体实施例的目的,并不是旨在限制本发明的保护范围。
除非另有特别说明,本发明中用到的各种原材料、试剂、仪器和设备等均可通过市场购买得到或者可通过现有方法制备得到。
各组分原料信息见如下:
本发明针对现有的问题,提供了一种专用于氧化锌分散浆的成膜抑菌组合物及其制备方法和应用。
实施例1
探究不同成膜剂对体系粉体状态的影响,包括如下步骤:
1)按照100g计算,称取18g ZnO,加入到30g的乙醇(95%)和47g的去离子水中,搅拌均匀,得到氧化锌的分散浆A;
2)取所述氧化锌的分散浆A,按照下表1的配比添加成膜剂,并将去离子水补足至100g,搅拌均匀,搅拌速度为300rpm,搅拌时间为2min,观察体系加入成膜剂后的体系分层状态、粉体状态以及成膜剂溶解情况。
表1
从表1可知,在氧化锌的水-乙醇分散体系中,加入分子量中等偏小的壳聚糖、羧甲基壳聚糖、壳糖胺盐酸盐、水溶性聚苯乙烯类、纤维素胶类、改性淀粉类、脂肪醇丙烯酸酯共聚物类等成膜剂,粉体状态是均匀的。
实施例2
探究氧化锌的分散浆中加入不同改性的壳聚糖,与不同成膜剂搭配对体系分层状态、粉体状态以及抗水性能的影响,包括如下步骤:
1)按照100g计算,称取18g的ZnO、0.2g的MHA加入到30g的乙醇(95%)和47g的去离子水中,搅拌均匀,得到氧化锌的分散浆B;取所述氧化锌的分散浆B,按照下表2的配比加入不同成膜剂(FlexanⅡ、普鲁兰多糖、ST 720)并将去离子水补足至100,搅拌均匀,搅拌速度300rpm,搅拌时间为2min;
2)按照100g计算,称取18g的ZnO、0.2g的MHA、加入到47g的去离子水中,再加入36g的乙醇(95%)和1.9g的水杨酸的混合液,搅拌均匀后得到氧化锌的分散浆C;取所述氧化锌的分散浆C,按照下表2的配比加入不同成膜剂(FlexanⅡ、Sensory、S-97、Cekol 150、ST720)并将去离子水补足至100,搅拌均匀,搅拌速度300rpm,搅拌时间为2min;
3)按照100g计算,称取18g的ZnO、0.5g的FlexanⅡ加入到47g的去离子水中,再加入36g的乙醇(95%)和1.9g的水杨酸的混合液,搅拌均匀后得到氧化锌的分散浆D;取所述氧化锌的分散浆D,按照下表2的配比加入不同成膜剂(MHA、普鲁兰多糖、陕西帕尼尔水溶性壳聚糖、海壳素R)并将去离子水补足至100,搅拌均匀,搅拌速度300rpm,搅拌时间为2min。
表2
注:接触角粗测方法是将样品涂抹到基底上,待样品在基底上干燥后,在距离基底2厘米左右的位置滴一滴水,观测水滴在膜表面的接触角随着时间的变化。
从表2可知,在氧化锌的水-乙醇分散浆中,加入MHA跟其他的成膜剂,接触角粗略估计都不大;先添加水杨酸,再加入MHA跟其他的成膜剂,如FlexanⅡ跟Cekol 150,接触角最大,但是Cekol 150的粉体状态不够均匀;在水杨酸、FlexanⅡ固定的情况下,加入不同壳聚糖和多糖,其中MHA跟海壳素的表现最好。
实施例3
壳聚糖与聚苯乙烯磺酸钠确定下,探究搭配不同原料对体系外观的改善情况,包括如下步骤:
1)按100g计算,称取18g的ZnO、0.2gMHA、0.5g的FlexanⅡ加入到47g的水中,然后加入36g的乙醇(95%)和水杨酸的溶液,将去离子水补足至100后,搅拌均匀,搅拌速度300rpm,搅拌时间为2min。
2)按照100g计算,称取18g的ZnO、0.2g的MHA、0.5gFlexanⅡ加入到36g的乙醇(95%)和47g的去离子水中,搅拌均匀,得到氧化锌的分散浆E;取所述氧化锌的分散浆E,按照下表3的配比加入不同原料(柠檬酸、乙醇酸、扁桃酸、ST 720、普鲁兰多糖、精氨酸、壬二酸)并将去离子水补足至100,搅拌均匀,搅拌速度300rpm,搅拌时间为2min。
表3
从表3可以看出,在氧化锌的分散浆中,添加水杨酸、壳聚糖、聚苯乙烯磺酸钠制得的产品,外观状态最好,粉体也较均匀。尤其是,在氧化锌的分散浆中加入有机酸制备的膜,抗水性能最好。其中,有机酸优选水杨酸。
实施例4
探究壳聚糖、聚苯乙烯磺酸钠、水杨酸三者最优配比,包括如下步骤:
1)按100g计算,称取18g的ZnO、0.2gMHA、0.5g的FlexanⅡ加入到50.3g的水中,然后加入30g的乙醇(95%)和1g的水杨酸的混合液,搅拌均匀,搅拌速度300rpm,搅拌时间为2min;
2)按照下表4中的原料配比重复步骤1)的操作。
表4
从表4可知,通过观察不同配比下,体系的分层状态,粉体聚集情况,以及接触角测试数据,得出MHA的添加量0.2%,FlexanⅡ添加量0.5%,水杨酸添加量1%为最优配比。
实施例5
接触角测试:
仪器:Contact Angle Systerm OCA 25
基底:盖玻片
测试方法,包括如下步骤:
1、将盖玻片浸泡在样品中5s,取出45℃干燥后继续浸泡5s,再次干燥,取出;
2、设置仪器参数,自动滴3ul去离子水在制备好的盖玻片上;
3、捕捉不同时间接触角图片;
4、对比不同时间接触角变化。
表5
注:表格中所有样品均采用乙醇水溶液作为溶剂。
由上表5可知:样品5、样品7、样品8、样品9的接触角最大,但区别不大,对样品5、样品7、样品8、样品9进行更长时间的接触角观测,结果见下表6。
表6
注:表格中所有样品均采用乙醇水溶液作为溶剂
由此可知,加了MHA、FlexanⅡ、水杨酸三者的接触角的最大,抗水性能最好。
实施例6
氧化锌与生物膜抗水性能测试(仪器、基底同实施例5):
测试方法,包括如下步骤:
1、将盖玻片浸泡在样品中1s,取出45℃干燥;
2、设置仪器参数,自动滴3ul去离子水在制备好的盖玻片上;
3、捕捉15分钟的接触角图片;
4、将样品板浸泡到水中,分别停留5分钟、10分钟、15分钟;
5、取出45℃干燥后,再次测试接触角图片。
表7
从表7可知,样品5的接触角下降31.2%,样品7在水中暴露15min后接触角下降了15.35%。这是因为在短时间浸泡后,水滴会逐渐将样品在载玻片上形成的薄膜溶解掉,所以样品7比样品5表现更好,抗水性更好。
实施例7
成膜抑菌组合物的抑菌率测试结果如下表8。
表8
注:样品ZMF即样品7。
该样品对痤疮丙酸杆菌的抑菌率高达99.9%,表明该产品具有显著的抑菌能力,具有祛痘作用。
本发明的上述方案具有如下的有益效果:
1.本发明通过在氧化锌的分散浆中添加聚苯乙烯磺酸钠和水杨酸,使得产品原有的外观状态得以保持,解决了壳聚糖等成膜剂加入到水醇溶液后,氧化锌的乙醇水溶液不再分层的问题;
2.本发明通过添加疏水组合物(有机酸和亲水-亲油两性高分子聚合物)使生物膜的抗水性能增强,从而避免壳聚糖或者聚苯乙烯磺酸钠本身形成的膜遇水即溶、抗水性不好的缺陷;且该生物膜具有较强的疏水性能,不仅减少氧化锌等功效物脱落,还可以给到创伤区的进一步保护,隔绝外界微生物、粉尘等的二次污染,增加功效物的作用时间和作用量;长效缓释氧化锌跟水杨酸,增强了产品的抑菌性能,起到长效抑菌的作用;
3.本发明成膜抑菌组合物应用范围广,不仅满足人体、动物等成膜抑菌需求,而且还可以用于食品、农业领域,且制备工艺简单、经济,适用于工业化生产。
以上所述是本发明的优选实施方式,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明所述原理的前提下,还可以作出若干改进和润饰,这些改进和润饰也应视为本发明的保护范围。
Claims (5)
1.一种专用于氧化锌分散浆的成膜抑菌组合物,其特征在于,所述专用于氧化锌分散浆的成膜抑菌组合物包括按重量百分数计的以下组分:18%氧化锌、30%的乙醇、0.2%壳聚糖、0.5%聚苯乙烯磺酸钠、1%水杨酸,余下为水;
其中,所述成膜抑菌组合物的制备方法,包括如下步骤:
称取18g的氧化锌、0.2g壳聚糖、0.5g的聚苯乙烯磺酸钠加入到50.3g的水中,然后加入30g的乙醇和1g的水杨酸的混合液,搅拌均匀,搅拌速度300rpm,搅拌时间为2min,即得。
2.一种如权利要求1所述的专用于氧化锌分散浆的成膜抑菌组合物的制备方法,其特征在于,包括如下步骤:称取18g的氧化锌、0.2g壳聚糖、0.5g的聚苯乙烯磺酸钠加入到50.3g的水中,然后加入30g的乙醇和1g的水杨酸的混合液,搅拌均匀,搅拌速度300rpm,搅拌时间为2min,即得。
3.如权利要求1所述的专用于氧化锌分散浆的成膜抑菌组合物或权利要求2所述的制备方法制得的成膜抑菌组合物在氧化锌分散体系中的应用。
4.根据权利要求3所述的应用,其特征在于,所述成膜抑菌组合物在氧化锌分散体系中的功能包括氧化锌分散体系成膜稳定,氧化锌粉体状态均匀,氧化锌生物膜具有疏水性,氧化锌生物膜兼具防水和抑菌性能。
5.根据权利要求3所述的应用,其特征在于,所述成膜抑菌组合物应用到氧化锌分散体系中对痤疮丙酸杆菌的抑菌率达到99.9%。
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