CN114209730A - 一种无乙醇复合微乳体系抗菌喷雾及其制备方法 - Google Patents
一种无乙醇复合微乳体系抗菌喷雾及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种无乙醇复合微乳体系抗菌喷雾及其制备方法。所述抗菌喷雾的原料包括天然活性物质、助表面活性剂、非离子型表面活性剂及蒸馏水。在天然活性物质中添加助表面活性剂,混合均匀,再添加非离子型表面活性剂,得到澄清透明的微乳体系;将微乳体系放入摇床中,水浴振荡至均匀后,间隔滴加蒸馏水,并继续振荡,待其恢复澄清透明状态,灌装在常压喷雾瓶内即可。本发明以薰衣草精油为主要成分,并通过其它两种活性成分分别与之复配,达到了协同增效的目的,大大增强了喷雾的抗菌效果;同时,所制备的复合微乳体系抗菌喷雾不含乙醇,表面活性剂含量少,其外观澄清透明,粒径小且稳定性好,并具有良好的铺展和润湿性能,且制备方法简便。
Description
技术领域
本发明涉及一种无乙醇复合微乳体系抗菌喷雾及其制备方法,属于抗菌日用品技术领域。
背景技术
过去常用的大多数抗菌药物:毒性大、威胁人体健康,并且其频繁使用,导致微生物对传统化学物质和药物的耐药性不断增强。精油作为一种天然抗菌剂,成为化学杀菌剂的替代品,在食品、化妆品以及药物等行业中引起了极大的关注,因此,近年来,随着消费者对使用天然成分的意识日益增强,精油越来越受欢迎。
薰衣草为唇形科薰衣草属植物,薰衣草精油是由薰衣草提炼而成,可以清热解毒,清洁皮肤,控制油分,祛斑美白,祛皱嫩肤、祛除眼袋黑眼圈,还可促进受损组织再生恢复等护肤功能。薰衣草精油还对心脏有镇静效果,可降低高血压、安抚心悸,对于失眠很有帮助。香芹酚是植物百里香和牛至精油的主要成分,是一种酚类化合物,呈淡黄色透明油状液体,它对细菌、霉菌和酵母具有很高的抗菌活性,具有广泛的应用价值,常用作消毒剂、杀菌剂、香料及化妆品的配方中。香茅醇是一种于香茅属植物香茅精油中发现的单萜烯类化合物,目前,香茅醇已被作为添加剂广泛应用于烟草、日化及食品领域,有研究发现,该化合物具有抗菌、抗炎、镇痛、抗氧化和抗肿瘤等药理作用。
植物精油具有显著的抗菌效果,在替代危害健康的合成防腐剂方面具有很大潜力。尽管它们有很好的效果,但仍然存在一些主要内在障碍,即低水溶性和生物利用度、挥发性和不稳定性,以及比较强烈的刺激性,因此导致它们还没有被广泛应用。纳米技术的最新进展有可能解决精油存在的这些缺陷。纳米乳液、微乳液等是目前用来包裹植物生物活性化合物的一些常用方法。
纳米乳液在热力学上是不稳定的,并且可以通过诸如奥斯特瓦尔德熟化,聚结和聚集等机制而不稳定,从而导致粒径分布的变化以及在储存过程中可能出现的可见的乳化/沉淀和相分离。此外,纳米乳液的形成通常需要高能量输入,例如高速或高压均质化。与纳米乳液不同,微乳液通常由组分在适当的组成下自发自组装而成,外部能量很少。微乳液具有贮存稳定性和降低生产成本的优点,在应用前可以用水稀释至任何油浓度仍可产生透明且稳定的微乳状液,可以降低运输和存储的成本。微乳液是热力学稳定、透明或半透明、低粘度和各向同性的分散体,可作为一些限制使用的物质的递送系统。
含醇类消毒剂的主要成分为乙醇(即酒精),易燃、易挥发,当空气中的酒精含量达到3.3%以上,遇到火源会发生闪爆,长期大量使用,会使病菌微生物产生抗药性,灭菌效果大大降低。为了给人们提供一种健康、安全绿色的抗菌消毒方式,本发明所制备的无乙醇复合微乳体系抗菌喷雾,不仅便于携带和使用,且在所选用的材料上有较小的接触角,具有良好的铺展和润湿性能,适用场景广泛,因此研究一种无乙醇复合微乳体系抗菌喷雾具有重要的意义。
发明内容
本发明所要解决的技术问题是:提供一种无乙醇复合微乳体系抗菌喷雾及其制备方法,以解决现有技术中植物精油水溶性、稳定性差和生物利用度低的问题。
为了解决上述技术问题,本发明采用以下技术方案:
一种无乙醇复合微乳体系抗菌喷雾,其原料包括以质量百分比计的0.2~4%天然活性物质、2~6%助表面活性剂、8~16%非离子型表面活性剂及余量的蒸馏水。
优选地,所述的非离子型表面活性剂为吐温80。
优选地,所述的助表面活性剂为二丙二醇。
优选地,所述的天然活性物质为薰衣草精油、香芹酚和香茅醇。
更优选地,所述天然活性物质中的薰衣草精油与助表面活性剂的质量比为1: 0~1:3,优选为1:3。
更优选地,所述天然活性物质中的薰衣草精油与助表面活性剂的总质量与非离子型表面活性剂的质量比为5:5~2:8,优选为5:5~4:6。
更优选地,所述薰衣草精油与香芹酚的质量比为10:1;所述薰衣草精油与香茅醇的质量比为1:1。
本发明还提供了上述无乙醇复合微乳体系抗菌喷雾的制备方法,包括以下步骤:
步骤1):在天然活性物质中添加助表面活性剂,混合均匀,再添加非离子型表面活性剂,得到澄清透明的微乳体系;
步骤2):将步骤1)得到的微乳体系放入摇床中,水浴振荡至均匀后,间隔滴加蒸馏水,并继续振荡,待其恢复澄清透明状态,灌装在常压喷雾瓶内得到无乙醇复合微乳体系抗菌喷雾。
优选地,所述步骤2)中水浴振荡的温度为25℃,转速为150rpm,滴加蒸馏水的间隔时间为1~3h。
本发明以两种活性成分分别与薰衣草精油复配为油相,运用微乳化技术制备得到薰衣草精油复合微乳体系,其具有良好的离心稳定性、高低温稳定性,润湿性和抗菌活性。
本发明将无乙醇复合微乳体系以喷雾形式进行抑菌,便于携带和使用,且适用范围广泛。该微乳体系使薰衣草精油和其它两种精油成分进行复配,不仅提高其抗菌性能,且复配后同时具有镇静安眠、去除异味以及提供香味的功能。
与现有技术相比,本发明的优势在于:
(1)本发明采用微乳化技术,将薰衣草精油和香芹酚、香茅醇制成O/W型微乳体系,可溶于水溶性环境中,解决了传统植物精油在水中不溶解以及活性成分易挥发、不稳定的特点。本发明提供的无乙醇复合微乳体系澄清透明,粒径分布均匀,大小处于10~20nm之间,且具有良好的离心稳定性、高低温稳定性,润湿性和抗菌活性。
(2)精油水溶性较低,不易与细胞膜发生相互作用,而微乳化可使精油中的活性物质通过被微乳体系携带去破坏细胞膜,进而影响微生物的生物活性。但单个植物精油或精油成分的抑菌谱较窄,所制备的抗菌喷雾功能效果单一,本发明所制备的微乳体系抗菌喷雾通过复配,达到了协同增效的目的,大大增强了喷雾的抗菌效果。
(3)本发明提供的上述无乙醇复合微乳体系抗菌喷雾对人体皮肤无致敏危害,对呼吸道粘膜无刺激性,表面活性剂含量少,所使用的助表面活性剂为二丙二醇,是一种保湿剂,具有保湿护肤功能。且该体系对设备要求低,制备工艺简单,具有贮存稳定性和降低生产成本的优点,便于储藏和运输。
附图说明
图1、2为本发明的实施例1和实施例2中助表面活性剂分别对两种类型的无乙醇复合微乳体系(薰衣草精油和香芹酚复合微乳体系、薰衣草精油和香茅醇复合微乳体系)形成影响的伪三元相图;
图3-5为纯薰衣草精油(Bulk LEO)、薰衣草精油和香芹酚复合微乳体系LR3 以及其中的单个微乳体系L31、R3分别对大肠杆菌、金黄色葡萄球菌和白色念珠菌的生长抑制率图;
图6-8为纯薰衣草精油(Bulk LEO)、薰衣草精油和香茅醇复合微乳体系LT3 以及其中的单个微乳体系L32、T3分别对大肠杆菌、金黄色葡萄球菌和白色念珠菌的生长抑制率图。
具体实施方式
为使本发明更明显易懂,兹以优选实施例,并配合附图作详细说明如下。
本发明中的各实施例中所述的百分比若无特殊说明,均指质量百分比。
实施例1
先将薰衣草精油与香芹酚以质量比10:1混合、与香茅醇以质量比1:1混合,然后按照薰衣草精油与助表面活性剂二丙二醇的质量比1:0、1:1、1:2 和1:3添加二丙二醇,最后按照表面活性剂与(薰衣草精油/二丙二醇)的质量比为0:10、1:9、2:8、3:7、4:6、5:5、6:4、7:3、8:2、9:1和10: 0配置混合体系,25℃150rpm水浴振荡至均匀后,间隔1~3h滴加蒸馏水,振荡,记录体系由澄清变浑浊的临界点,并计算临界点时体系中各成分所占比例,以薰衣草精油/二丙二醇、表面活性剂和水分别为三个顶点,绘制拟三元相图。其中网格区域为非微乳相区,空白灰色区域为微乳相区,其分界线即为澄清和浑浊的临界点。通过三元相图能够较为直观地了解助表面活性剂对(微乳区)面积的影响,从而确定微乳单相区,计算出微乳单相区占三元相图总面积的比例 (Am)。
实施例1所得薰衣草精油和香芹酚复合微乳体系以及薰衣草精油和香茅醇复合微乳体系各组成成分对微乳体系的影响分别如图1和图2所示(图1和图2 中的a、b、c和d分别表示薰衣草精油与二丙二醇的质量比为1:0、1:1、1: 2和1:3),在不含助表面活性剂二丙二醇的情况下,形成的微乳体系区域面积都很小,随着助表面活性剂二丙二醇含量的增加,微乳面积有一个增大的趋势,且按比例配置所形成的无限稀释线条数也在逐条增加。
实施例2
在薰衣草精油和二丙二醇质量比为1:3的拟三元相图中,选择最小可稀释比的无限稀释线,即在可无线稀释线中表面活性剂含量相对较小的一条无线稀释线,即图1中单相区的点LR3。具体过程如下:将薰衣草精油与香芹酚以质量比 10:1混合,摇晃均匀,然后按照薰衣草精油与助表面活性剂二丙二醇的质量比 1:3添加二丙二醇,继续摇晃均匀作为油相,最后按照油相与吐温80的质量比为5:5配置混合体系,25℃150rpm水浴振荡至均匀后,缓慢滴加蒸馏水至薰衣草精油浓度为2%,香芹酚浓度为0.2%。灌装到常压喷雾瓶内,灌装前,喷雾瓶需经环氧乙烷灭菌处理。
实施例3
在薰衣草精油和二丙二醇质量比为1:3的拟三元相图中,选择最小可稀释比的无限稀释线,即在可无线稀释线中表面活性剂含量相对较小的一条无线稀释线,即图2中单相区的点LT3。具体过程如下:将薰衣草精油与香茅醇以质量比 1:1混合,摇晃均匀,然后按照薰衣草精油与助表面活性剂二丙二醇的质量比1: 3添加二丙二醇,继续摇晃均匀作为油相,最后按照油相与吐温80的质量比为4: 6配置混合体系,25℃150rpm水浴振荡至均匀后,缓慢滴加蒸馏水至薰衣草精油浓度为2%,香茅醇浓度为2%。灌装到常压喷雾瓶内,灌装前,喷雾瓶需经环氧乙烷灭菌处理。
为了更清晰客观的展现所述无乙醇复合微乳体系抗菌喷雾制剂的稳定性、润湿性和抗菌效果,可做如下测试:
1.粒径大小
使用Omni多角度粒度及高灵敏Zeta电位分析仪,采用动态光散射技术测量了实施例2以及实施例3的粒径。
2.稳定性测试
离心稳定性:取适量制备好的薰实施例2和实施例3于离心管中,分别在 4000rpm和10000rpm下各离心30min,以蒸馏水为空白对照,在550nm波长下测定其离心后的透光率。
高低温稳定性:微乳体系于-4℃的冰箱中放置24h,取出恢复至室温时观察,无沉淀和无变色现象,透明产品不混浊;40℃的保温箱中放置24h,取出恢复至室温时观察,无异味、无分层和无变色现象,透明产品不混浊。
3.接触角的测定
采用座滴法测量微乳体系的静态接触角,选用的固体材料分别为玻璃、陶瓷和猪皮。通过测定微乳体系在固体材料上的接触角,与蒸馏水进行比较,对无乙醇复合微乳体系抗菌喷雾的润湿性进行评价。
4.抑菌效果测试
通过微量肉汤稀释法测OD值来计算纯薰衣草精油(Bulk LEO)、实施例2-LR3及其所包含的单个微乳体系(L31:薰衣草精油微乳体系、R3:香芹酚微乳体系)和实施例3-LT3及其所包含的单个微乳体系(L32:薰衣草精油微乳体系、T3:香茅醇微乳体系)对大肠杆菌、金黄色葡萄球菌和白色念珠菌的抑菌率,试样抑菌率按照如下公式进行计算:
式中,C为生长对照OD值,C0为无菌对照OD值,A为试样OD值。
测试结果如下所示:
无乙醇复合微乳体系抗菌喷雾制剂粒径、多分散性指数及稳定性测试结果见表1。
表1
从表1的结果可知,无乙醇复合微乳体系抗菌喷雾的粒径都非常小,样品颗粒的多分散性指数较低,说明所制备的复合微乳体系均匀性较好。将两种类型不同比例的无乙醇复合微乳体系分别以4000rpm和10000rpm离心30分钟,高低温处理,微乳体系均未发生相分离现象,仍然保持澄清透明。进一步证明所制备的无乙醇复合微乳体系各相均一、热力学稳定性好。
无乙醇复合微乳体系抗菌喷雾的接触角见表2。
表2
实施例3的微乳体系液滴容易吸附在进样器外壁,可能是因为在含有一定量的表面活性剂和助表面活性剂的情况下,又含有香茅醇,导致表面张力过小,润湿性太好,固无法测出其接触角。由表2可知,与蒸馏水相比,本研究制备的无乙醇复合微乳体系抗菌喷雾在所选用的固体材料上的接触角显著降低,提高溶液在固体表面上的润湿和铺展性能。
抑菌效果测试结果:
如图3所示,薰衣草精油和香芹酚浓度分别为1%和0.1%时,实施例2-LR3 对大肠杆菌的抑制率达到了73.54%。如图4所示,对于薰衣草精油和香芹酚浓度分别为0.02%和0.002%时,LR3对金黄色葡萄球菌的抑制率为98.67%,此时, Bulk LEO对金黄色葡萄球菌没有抑制作用,L31和R3对金黄色葡萄球菌的抑制率分别为35.72%和25.46%。在图5中,薰衣草精油和香芹酚浓度分别仅为0.09%和0.009%时,LR3对白色念珠菌的抑制率就已经达到100%,而Bulk LEO、L31 和R3对白色念珠菌均没有出现抑制作用。
如图6所示,薰衣草精油浓度为1%时,Bulk LEO才对大肠杆菌出现抑制作用,抑制率为29.43%,同等精油浓度的L32对大肠杆菌的抑制率为69.55%,含 1%香茅醇的T3对大肠杆菌的抑制率为56.05%,而相对应的复合微乳体系LT3 对大肠杆菌的抑制率提高到了82.70%。如图7所示,薰衣草精油和香茅醇浓度都为0.09%时,Bulk LEO对金黄色葡萄球菌没有抑制作用,L32和T3对金黄色葡萄球菌的抑制率分别为18.97%和46.73%,而LT3对金黄色葡萄球菌的抑制率达到99.32%。在图8中,薰衣草精油和香茅醇浓度都仅为0.06%时,T3和LT3 对白色念珠菌的抑制率都达到了100%,说明形成复合微乳体系LT3后,很好的保留了T3对白色念珠菌的抑菌性能。
Claims (9)
1.一种无乙醇复合微乳体系抗菌喷雾,其特征在于,原料包括以质量百分比计的0.2~4%天然活性物质、2~6%助表面活性剂、8~16%非离子型表面活性剂及余量的蒸馏水。
2.如权利要求1所述的无乙醇复合微乳体系抗菌喷雾,其特征在于,所述的非离子型表面活性剂为吐温80。
3.如权利要求1所述的无乙醇复合微乳体系抗菌喷雾,其特征在于,所述的助表面活性剂为二丙二醇。
4.如权利要求1所述的无乙醇复合微乳体系抗菌喷雾,其特征在于,所述的天然活性物质为薰衣草精油、香芹酚和香茅醇。
5.如权利要求4所述的无乙醇复合微乳体系抗菌喷雾,其特征在于,所述天然活性物质中的薰衣草精油与助表面活性剂的质量比为1:0~1:3。
6.如权利要求4所述的无乙醇复合微乳体系抗菌喷雾,其特征在于,所述天然活性物质中的薰衣草精油与助表面活性剂的总质量与非离子型表面活性剂的质量比为5:5~2:8。
7.如权利要求4所述的无乙醇复合微乳体系抗菌喷雾,其特征在于,所述薰衣草精油与香芹酚的质量比为10:1;所述薰衣草精油与香茅醇的质量比为1:1。
8.权利要求1-7任意一项所述的无乙醇复合微乳体系抗菌喷雾的制备方法,其特征在于,包括以下步骤:
步骤1):在天然活性物质中添加助表面活性剂,混合均匀,再添加非离子型表面活性剂,得到澄清透明的微乳体系;
步骤2):将步骤1)得到的微乳体系放入摇床中,水浴振荡至均匀后,间隔滴加蒸馏水,并继续振荡,待其恢复澄清透明状态,灌装在常压喷雾瓶内得到无乙醇复合微乳体系抗菌喷雾。
9.如权利要求8所述的制备方法,其特征在于,所述步骤2)中水浴振荡的温度为25℃,转速为150rpm,滴加蒸馏水的间隔时间为1~3h。
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