CN113796393A - 具有持久缓释能力的环保型精油乳液及其制备方法与应用 - Google Patents
具有持久缓释能力的环保型精油乳液及其制备方法与应用 Download PDFInfo
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- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
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- A01N65/28—Myrtaceae [Myrtle family], e.g. teatree or clove
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- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
- A01N65/40—Liliopsida [monocotyledons]
- A01N65/44—Poaceae or Gramineae [Grass family], e.g. bamboo, lemon grass or citronella grass
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- A23K10/00—Animal feeding-stuffs
- A23K10/30—Animal feeding-stuffs from material of plant origin, e.g. roots, seeds or hay; from material of fungal origin, e.g. mushrooms
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Abstract
本发明提供了一种具有持久缓释能力的环保型精油乳液及其制备方法与应用。该环保型精油乳液包括植物精油成分、多功能复合助溶剂、天然表面活性剂和水;多功能复合助溶剂包括第一助溶剂组分和第二助溶剂组分;第一助溶剂组分包括甲基纤维素和乙基纤维素的一种或两种,第二助溶剂组分包括香芹酚、丁香酚和桂皮醛中的一种或两种以上的组合。多功能复合助溶剂不仅可以增强精油在油相中的溶解性和混溶性,提高油相粘度,而且可以减缓乳液涂覆后精油的挥发。本发明提供的乳液采用环境友好的配方,在分散状态下具有良好稳定性。该乳液的显著特点是涂覆后在干燥过程中,油相会形成连续凝胶网络减缓精油的挥发,进而提供缓释能力和持久抑菌能力。
Description
技术领域
本发明涉及一种基于精油制备的具有持久缓释能力的环保型精油乳液及其制备方法与应用,属于抗菌乳液制备技术领域。
背景技术
随着抗生素的滥用,微生物抗药性问题持续威胁着全球公共卫生体系。根据世界卫生组织报告,至今每年至少有70万人死于抗药性疾病,同时越来越多的常见病,比如呼吸道和泌尿系统感染,变得难以治愈。如果不采取行动,因为抗药性问题死亡的人数将于2050年可增至1000万人。
近几年,因为抗生素新药研发成本和难度的增加,有效抗生素新药处于停滞状态。根据美国感染病学会(Infectious Diseases Society of American,IDSA)的看法,现在使用中的所有抗生素都是1984年前发现的一种药物的衍生物。世界各国都注意到了这一危机,并试图寻找解决方法。除了通过优化人类和动物卫生工作中抗生素的使用方法,寻找新一代的抗菌药物,已经引起了学术界及工业界广泛的关注。
具有抗菌效果的植物精油或其提取物已广泛应用在不同的抗菌产品中,但这些油溶性物质在水相中分散性较差,其在水相中的稳定分散和涂覆后的缓慢释放是限制其应用的关键问题。现阶段对精油的负载方式可以通过微胶囊包覆或者增溶乳化等技术实现精油的稳定性和适用性。其中,增溶乳化技术具有成本较低,物理化学稳定和释放性优良等特点,使其能够广泛适用于工业生产和实际应用中。然而,现有的精油乳液也有两个明显短板。首先,为了增加精油的稳定性,常常在乳液中添加合成表面活性剂和有机溶剂,破坏了乳液本身的环保性并会影响精油的生物活性;其次,这些精油乳液涂覆在不同表面后,往往会发生快速的破乳,释放出包裹的精油,而释放出的精油会在较短时间内挥发,无法实现涂覆后的长效抑菌的需求。
因此,研究制备新型具有持久缓释能力的环保型、高效抗菌乳液是满足未来的市场需求和发掘新型消费潜力的关键。
发明内容
为解决上述技术问题,本发明的目的在于提供一种基于精油制备的、具有持久缓释能力的环保型精油乳液及其制备方法与应用。该乳液通过添加多功能复合助剂,能够增强增加精油组分在油相中的溶解性和混溶性,并形成连续凝胶网络帮助减缓涂覆后精油的挥发,提高持久缓释能力。
为达到上述目的,本发明提供了一种基于精油制备的环保型精油乳液,其中,该环保型精油乳液包括植物精油成分、多功能复合助溶剂、天然表面活性剂或食品级表面活性剂、水;
其中,所述多功能复合助溶剂包括第一助溶剂组分和第二助溶剂组分;所述第一助溶剂组分包括甲基纤维素(Methyl cellulose,优选食品级甲基纤维素)和乙基纤维素(Ethyl cellulose,优选食品级乙基纤维素)的一种或两种,所述第二助溶剂组分包括香芹酚、丁香酚和桂皮醛中的一种或两种以上的组合。
根据本发明的具体实施方案,所述多功能复合助溶剂还可以包括第三助溶剂组分;优选地,所述第三助溶剂组分包括生物乙醇(Ethanol)、天然甘油(glycerol)和天然植物源乙二醇(ethylene glycol)等中的一种或两种以上的组合。
根据本发明的具体实施方案,优选地,以环保型精油乳液的总质量计,所述多功能复合助溶剂的含量为0.01-20%,更优选为0.01-15%。
根据本发明的具体实施方案,优选地,以多功能复合助溶剂的总质量计,所述第一助溶剂组分的含量为10-60%,所述第二助溶剂组分的含量为40-90%。
根据本发明的具体实施方案,所述第三助溶剂组分的含量可以根据需要确定,适量即可,例如占环保型精油乳液总质量的10%以下。
根据本发明的具体实施方案,优选地,以该环保型精油乳液的总质量计,所述天然表面活性剂的含量为1-65%。
根据本发明的具体实施方案,优选地,所述天然表面活性剂包括皂角素(TeaSaponin)、生物明胶(Gelatin)、阿拉伯胶(Gum Arabic)、鼠李糖脂(Rhamnolipids)、淀粉基表面活性剂(Amylopectin)和烷基糖苷(APGs)等中的一种或两种以上的组合。
根据本发明的具体实施方案,优选地,以环保型精油乳液的总质量计,所述植物精油成分的含量为0.01%-20%。
根据本发明的具体实施方案,优选地,所述植物精油成分包括丁香精油、柠檬草精油、依兰精油、尤加利精油、樟脑精油、罗马洋甘菊精油、罗文沙叶精油、茶树精油、松针精油、绿化白千层精油、鼠尾草精油、牛至精油、巴西土荆芥精油、大叶胺精油、广藿香精油、香芋精油、肉桂醛、松油醇、薰衣草精油、雪松精油、丝柏精油等中的一种或两种以上的组合。
根据本发明的具体实施方案,优选地,所述植物精油成分还包括香芹酚、百里酚、异戊二烯、芳樟醇、孜然芹烯、α-姜黄烯、月桂烯、草酚酮、蒎烯、茴香醇、金合欢烯、α-桉叶醇、油杉醇、桂皮醛、茴香醚、茴香烯、扁柏酸、保幼酮、柏木脑、A-毕橙茄醇、T-Muurolol、T-Cadinol、Epicubenol、8-Acetoxyelemol、甲基正壬酮、异戊醛、异戊酸、薄荷醇、薄荷酮等中的一种或两种以上的组合。
根据本发明的具体实施方案,在上述环保型精油乳液中,所添加的水可以是饮用级过滤水、去离子水、蒸馏水或二次蒸馏水等。
根据本发明的具体实施方案,以质量百分比计,上述环保型精油乳液的组成可以包括:植物精油成分0.01%-20%、多功能复合助溶剂0.01-20%、天然表面活性剂1-65%、余量水;各组分的百分比之和为100%。
本发明采用了多功能复合助溶剂,该多功能复合助溶剂能够增强单一组分精油或多组分精油在油相中的溶解性和混溶性,并形成连续凝胶网络帮助减缓涂覆后精油的挥发。此外,在植物精油成分中添加多功能复合助溶剂,以及天然或食品级表面活性剂,能够调节油相的粘度,制备得到复合油相;将复合油相与水相混合、乳化后能够制备得到水包油乳液。该乳液采用环境友好的配方,在分散状态下具有良好稳定性。涂覆后在干燥过程中,乳液中的油相会形成连续凝胶网络减缓精油的挥发,进而提供缓释能力和持久抑菌能力。
本发明还提供了上述环保型精油乳液的制备方法,其流程如图1所示。该方法包括以下步骤:
将植物精油成分和多功能复合助溶剂混合,通过加热搅拌制备得到均一溶液,然后与天然表面活性剂混合得到油相;当采用第三助溶剂组分时,该第三助溶剂组分在加入天然表面活性剂之前添加;
将油相和水相混合乳化制成乳液,得到所述环保型精油乳液。
根据本发明的具体实施方案,上述制备方法可以包括以下具体步骤:
制备多功能复合助溶剂:将第一助溶剂组分(甲基纤维素和/或乙基纤维素)与第二助溶剂组分(香芹酚、丁香酚和桂皮醛中的一种或两种以上的组合)混合,通过一定条件加热(90-190℃)和搅拌(转速500-1000r/min)处理得到均一的溶剂相,冷却后即得到多功能复合助溶剂;
制备油相:将植物精油成分与多功能复合助溶剂混合,通过一定条件加热(90-190℃)和搅拌(转速500-1000r/min)处理得到均一的油相,然后在搅拌状态下加入天然表面活性剂,加入完成之后搅拌至溶液澄清,得到油相;
在搅拌状态下,将油相滴加到水相之中,然后经过高速均质、搅拌,得到透明乳液,即所述环保型精油乳液。
本发明还提供了上述环保型精油乳液在表面抗菌、杀菌喷雾和/或饲料添加中的应用;优选地,当制备抗菌涂层时,该所述环保型精油乳液是通过浸涂、喷涂、旋涂、滴铸、淋涂、漆涂、真空涂中的一种或者两种以上的方法进行制备。
涂覆后在干燥过程中,本发明的环保型精油乳液的油相会形成连续凝胶网络减缓精油的挥发,进而提供缓释能力和持久抑菌能力。
本发明提供的环保型精油乳液是通过在天然的或商业化的精油(或精油成分)中添加多功能复合助溶剂和天然表面活性剂,经过对油相的预处理,以及水油混合液的高速搅拌、乳化均质等方法,最终制备得到在分散状态下具有良好稳定性,涂覆后能提供缓释能力和持久抑菌能力的精油乳液。
本发明提供的环保型精油乳液在医学防疫及公共卫生学具有良好应用价值,例如公共设施、医学护具、个人卫生防护用品、家庭用品、医药包装、食品包装等方面的抗菌喷涂应用,以及在饲料添加、蔬菜水果防腐以及种子保护等方面的应用。
附图说明
图1为本发明提供的环保型精油乳液的制备方法的流程图。
图2为实施例1制备的多功能复合助溶剂的凝胶转变结果。
图3为多功能复合助溶剂在液体和凝胶状态下的挥发测试结果。
图4为未添加多功能复合助溶剂所制备得到的精油乳液的稳定性测试结果。
图5为添加多功能复合助溶剂所制备得到的环保型精油乳液的稳定性测试结果。
图6为环保型精油乳液的表面涂覆后释放能力的测试结果。
图7为添加不同精油制备得到的精油乳液的抗菌性能测试结果。
图8为不同组分的抗菌精油乳液在不同表面上涂覆后持久抗菌能力的测试结果。
具体实施方式
为了对本发明的技术特征、目的和有益效果有更加清楚的理解,现对本发明的技术方案进行以下详细说明,但不能理解为对本发明的可实施范围的限定。
实施例1
本实施例提供了一种具有良好的稳定性和持久缓释能力的环保型精油乳液,其是通过以下步骤制备的:
(1)制备多功能复合助溶剂:将0.5g粉末状乙基纤维素加入0.8g香芹酚和0.2g桂皮醛中,加热到160℃,600r/min磁力搅拌至完全溶解,得到多功能复合助溶剂,冷却到室温备用。
(2)制备复合精油油相:将0.5g多功能复合助溶剂与1g薄荷精油(或丁香精油)加入烧杯中,在转速500r/min磁力搅拌下滴加0.5ml浓度为10wt%的甘油乙二醇溶液(第三助溶剂组分);在室温下搅拌30min至溶液澄清后,加入3.5g烷基糖苷APGs,600r/min磁力搅拌条件下,室温搅拌至溶液澄清,得到薄荷精油油相(或丁香精油油相)。
(3)制备复合精油乳液:搅拌下,取3.5g含薄荷精油(或丁香精油)的油相滴加到7g蒸馏水中,高速均质20min,850r/min搅拌4h,得到透明乳浊液,即得到环保型精油乳液。
稳定性测试:
首先将实施例1制备得到的多功能复合助溶剂涂覆在玻璃片上进行观察并测量其在空气中的质量损失。图2为多功能复合助溶剂的凝胶转变情况。由图2可以看出:在自然蒸发过程中,多功能复合助溶剂会由自由流动的液态,转换为凝胶态;进一步的观察表明,凝胶内部存在大量的连续网络结构。
图3为多功能复合助溶剂在液体和凝胶状态下的挥发测试。图3所示的结果表明,未添加乙基纤维素的0.8g香芹酚和0.2g桂皮醛的混合液体(未添加水)可以在空气中较快的挥发,实施例1的步骤(1)添加乙基纤维素得到的多功能复合助溶剂由于凝胶网络的形成,可以大幅减缓内部有机液体的挥发。
图4为在未加入多功能复合助溶剂的情况下,由天然精油和水直接乳化得到的乳液在静止一周后的稳定性情况。由图4可以看出,乳液稳定性存在差异,其中,丁香油酚、桂皮醛作为精油组分的乳液比较稳定,其它则发生破乳现象。
图5为实施例1制备的环保型精油乳液加入多功能复合助溶剂后的稳定性测试结果。其中,图片分别为薄荷精油(左)和丁香精油(右)加入复合助溶剂后制备的乳液及其光学照片。由图5可以看出:在静止一周后,加入复合助溶剂后所制备的精油乳液都没有发生破乳现象。光学照片显示乳液均为乳浊液,表示所制备的乳液具有良好的稳定性。
释放能力测试:
图6为实施例1制备的环保型精油乳液的表面涂覆测试结果。其中,光学照片(左下图)为薄荷精油乳液玻璃片上涂覆2小时和24小时后,用刀片划出划痕后的结果。由图6可以看出,在涂覆后随着乳液中水分和精油的减少,流动性降低,涂层逐渐变成凝胶态。质量测试结果表明,涂层的质量损失是一个逐渐减慢的过程。
实施例2
本实施例提供了一种环保型复合精油乳液,其是通过以下步骤制备的:
(1)制备多功能复合助溶剂:将0.5g粉末状甲基纤维素加入0.6g香芹酚和0.4g桂皮醛中,加热到160℃、600r/min磁力搅拌至完全溶解,得到多功能复合助溶剂,冷却到室温备用。
(2)制备环保型乳液油相:将0.5g多功能复合助溶剂分别与1g不同混合比例混合的香芹酚/丁香精油(丁香精油:香芹酚=6:4、4:6、2:8)混合,分别加入烧杯中,在500r/min磁力搅拌下滴加0.5ml浓度为10wt%的甘油乙二醇溶液;在室温下搅拌30min至溶液澄清后,加入3.5g烷基糖苷APGs,600r/min磁力搅拌,室温搅拌至溶液澄清,得到油相。
(3)制备环保型复合精油乳液:搅拌下,将1.5g油相滴加到8.5g水中,高速均质20min后,850r/min搅拌4h,得到透明乳浊液,即基于香芹酚/丁香精油复合组分的环保型精油乳液。
抗菌性测试:
本测试使用革兰氏阳性菌S.aureus对乳液进行抗菌测试,具体测试方法为:将2ml分别含S.aureus的Luria-Bertani肉汤置于培养皿中,5min后对培养皿进行精油基乳液喷涂,24h后通过测定细菌菌落数,空白对照为不经精油基乳液喷涂的培养皿。
图7为不同比例的丁香/香芹酚精油复合乳液对革兰氏阳性菌S.aureus的抗菌性能测试结果图。其中,a图为空白对照组,b图为丁香精油与香芹酚配比(E:C)6:4的乳液;c图为丁香精油与香芹酚配比4:6的乳液;d图为丁香精油与香芹酚配比2:8的乳液;e图为不同丁香精油与香芹酚配比的乳液对革兰氏阳性菌S.aureus的抗菌效果;f图为不同丁香精油与香芹酚配比的乳液在一周后的稳定性测试。
由图7可以看出,当丁香与香芹酚的配比为2:8时,所得到的乳液具有良好的杀菌性,杀菌率高达99.99%。乳液为透明乳浊液,具有良好稳定性。
实施例3
本实施例展示了含有不同精油组分的环保型精油乳液在表面涂覆后的持久抗菌效果测试结果,其中,环保型精油乳液为实施例1和实施例2所制备的,实施例1的薄荷精油乳液命名为乳液1,实施例2中的丁香与香芹酚配比为2:8的复合精油乳液命名为乳液2。
表面涂覆抗菌测试:
本测试使用革兰氏阳性菌S.aureus对涂覆抗菌乳液的不同表面进行抗菌测试。具体测试方法为:
首先将乳液1和乳液2通过喷涂或浸渍法,分别涂膜在不同形状的表面上,包括记号笔、印章和面罩等,干燥2小时后进行抗菌测试测试;
然后将配制好的含S.aureus的Luria-Bertani肉汤,喷涂在已经涂抹了精油乳液的表面,放置不同时间后,通过棉签在样品表面取样,结合细菌菌落培养CFU,测定细菌菌落数。
图8为涂覆乳液1的不同表面的照片以及它们对革兰氏阳性菌S.aureus的抗菌性能测试结果。由图8中的a图可以看出,抗菌乳液可以均匀的涂覆在记号笔、印章和面罩上。由图8中的b图可以看出,在上述三个表面上,涂覆乳液1或乳液1后2-72小时的时间内,均能实现有效的抑菌。
实施例4
本实施例提供了一种放大制备环保型精油乳液的方法,其包括以下步骤:
(1)制备多功能复合助溶剂:将3g乙基纤维素粉末和1g甲基纤维素粉末,与4g香芹酚、1g丁香酚和15g桂皮醛混合均匀,加热到160℃,600r/min磁力搅拌至完全溶解,得到多功能复合助溶剂,冷却到室温备用。
(2)制备环保型乳液油相:将20g多功能复合助溶剂和200ml生物乙醇置于烧杯中,随后搅拌下滴加入12g丁香精油、48g牛至精油、10g柠檬草精油和10g罗马洋甘菊精油;在500r/min机械搅拌下加入10ml甘油;室温下机械搅拌30min至溶液澄清后,加入350g烷基糖苷APGs,1000r/min条件下,室温搅拌至溶液澄清,得到油相。
(3)乳液制备:在搅拌条件下,取150g油相添加到850g的水中,高速均质1h后,1200r/min搅拌4h,得到乳液,即环保型精油乳液,也可以称为环保型缓释抗菌乳液。
实施例1-2、4制备的环保型精油乳液的VOC均低于120g/L,满足GB18582-2008标准规定的限量值要求。
Claims (10)
1.一种具有持久缓释能力的环保型精油乳液,其中,该环保型精油乳液包括植物精油成分、多功能复合助溶剂、天然表面活性剂或食品级表面活性剂、水;
其中,所述多功能复合助溶剂包括第一助溶剂组分和第二助溶剂组分;所述第一助溶剂组分包括甲基纤维素和乙基纤维素的一种或两种,所述第二助溶剂组分包括香芹酚、丁香酚和桂皮醛中的一种或两种以上的组合。
2.根据权利要求1所述的环保型精油乳液,其中,所述多功能复合助溶剂还包括第三助溶剂组分;优选地,所述第三助溶剂组分包括生物乙醇、天然甘油和天然植物源乙二醇中的一种或两种以上的组合。
3.根据权利要求1或2所述的环保型精油乳液,其中,以该环保型精油乳液的总质量计,所述多功能复合助溶剂的含量为0.01-20%;优选为0.01-15%。
4.根据权利要求1-3任一项所述的环保型精油乳液,其中,以所述多功能复合助溶剂的总质量计,所述第一助溶剂组分的含量为10-60%,所述第二助溶剂组分的含量为40-90%。
5.根据权利要求1-4任一项所述的环保型精油乳液,其中,以该环保型精油乳液的总质量计,所述天然表面活性剂的含量为1-65%。
6.根据权利要求1-5任一项所述的环保型精油乳液,其中,所述天然表面活性剂包括皂角素、生物明胶、阿拉伯胶、鼠李糖脂、淀粉基表面活性剂和烷基糖苷中的一种或两种以上的组合。
7.根据权利要求1-6任一项所述的环保型精油乳液,其中,以该环保型精油乳液的总质量计,所述植物精油成分的含量为0.01%-20%。
8.根据权利要求1-7任一项所述的环保型精油乳液,其中,所述植物精油成分包括丁香精油、柠檬草精油、依兰精油、尤加利精油、樟脑精油、罗马洋甘菊精油、罗文沙叶精油、茶树精油、松针精油、绿化白千层精油、鼠尾草精油、牛至精油、巴西土荆芥精油、大叶胺精油、广藿香精油、香芋精油、肉桂醛、松油醇、薰衣草精油、雪松精油、丝柏精油中的一种或两种以上的组合;
优选地,所述植物精油成分还包括香芹酚、百里酚、异戊二烯、芳樟醇、孜然芹烯、α-姜黄烯、月桂烯、草酚酮、蒎烯、茴香醇、金合欢烯、α-桉叶醇、油杉醇、桂皮醛、茴香醚、茴香烯、扁柏酸、保幼酮、柏木脑、A-毕橙茄醇、T-Muurolol、T-Cadinol、Epicubenol、8-Acetoxyelemol、甲基正壬酮、异戊醛、异戊酸、薄荷醇、薄荷酮中的一种或两种以上的组合。
9.根据权利要求1-8任一项所述的环保型精油乳液的制备方法,其包括以下步骤:
将植物精油成分和多功能复合助溶剂混合,通过加热搅拌制备得到均一溶液,然后与天然表面活性剂混合得到油相;
将油相和水相混合乳化制成乳液,得到所述环保型精油乳液。
10.根据权利要求1-9任一项所述的环保型精油乳液在表面抗菌、杀菌喷雾和/或饲料添加中的应用;
优选地,所述环保型精油乳液是通过浸涂、喷涂、旋涂、滴铸、淋涂、漆涂、真空涂中的一种或者两种以上的方法制备抗菌涂层。
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