CN105828637B - 杀微生物组合物 - Google Patents

杀微生物组合物 Download PDF

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CN105828637B
CN105828637B CN201480069620.9A CN201480069620A CN105828637B CN 105828637 B CN105828637 B CN 105828637B CN 201480069620 A CN201480069620 A CN 201480069620A CN 105828637 B CN105828637 B CN 105828637B
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E·西恩瓦蒂
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Abstract

本发明涉及含有N‑甲基‑1，2‑苯并异噻唑啉‑3‑酮和精油的协同性杀微生物组合物。

Description

杀微生物组合物
技术领域
本发明涉及一种所选择的杀微生物剂的协同组合，所述组合的活性比单一杀微生物剂所观察到的高。
背景技术
从早期开始，精油已被香水、制药、化妆品及食品行业用于调味或提升芳香，并且成为民间医药及芳香疗法中的愈合性以及治疗性活性成分。由从植物中所萃取出的芳香性和挥发性液体所构成的精油含有在植物的害虫抵御中起一定作用的化学物质(次级代谢物)并且通常具有抗微生物性。精油及其组分之抗菌性已得到充分证明。举例而言，迷迭香精油已显示出抗微生物力以及控制不同重量的阳性菌和阴性菌生长的有效性。亦对百里香油作为外用化妆品配方的防腐剂的用途进行了研究并且证实为及其有效。随着各个行业(家用产品、个人护理以及建筑材料)逐渐倾向于使用更多的天然产品，对精油作为天然防腐剂的关注也越来越高。然而，由使用精油作为防腐剂所产生的一个重要问题在于，作为单一的杀生物剂组分，这些精油大部分通常不够有效，并且经常需要呈极高的浓度以供有效保存。因此可能会造成负面的感官影响。因此需要一种提供增强的保存有效性的组合物，其使成本效益达到最大并且使感官影响降到最低。
此外，在一些情况下，即使单一的有机杀微生物剂呈高使用浓度，由于抵抗某些类型之微生物，例如对某些杀微生物剂具有抗性的那些微生物的活性较弱，或由于侵袭性的环境条件，其也无法提供对微生物的有效控制。有时会使用不同杀微生物剂的组合在特定的最终使用环境中提供对微生物的总体控制。举例而言，美国专利申请公开案第2007/0078118号揭示了N-甲基-1，2-苯并异噻唑啉-3-酮(MBIT)与其它杀生物剂的协同组合。然而，需要额外的杀微生物剂的组合来提供对微生物的有效控制，所述杀微生物剂具有增强的抵抗不同微生物株的活性。此外，出于环境和经济效益，需要包含较低水平的单一杀微生物剂的组合。当前市场，如家用和个人护理市场正在寻找基于天然成分之产品。尽管MBIT是家用和个人护理市场中的常用成分，但能够将所使用的MBIT量降到最低并且与天然成分进行组合，同时保持相同或更好的有效性将为有利的。
发明内容
本发明所要解决的问题在于提供所述额外的杀微生物剂的组合。
本发明涉及一种杀微生物组合物，其包含：(a)N-甲基-1，2-苯并异噻唑啉-3-酮；以及(b)至少一种精油。
本发明亦涉及一种抑制或控制微生物生长的方法，所述方法包含以下步骤：将杀微生物组合物添加到工业工艺用水；超过滤；工业或消费型胶粘剂；家用产品；化妆品；洗漱用品；洗发剂；肥皂；去垢剂；工业清洁剂；地板抛光剂；衣物漂洗水；医疗装置；诊断试剂保存；食品；饮料和工业工艺巴氏灭菌器；抽水马桶；娱乐用水；水池以及温泉中。
另外，本发明提供一种涂料组合物，其包含：(a)N-甲基-1，2-苯并异噻唑啉-3-酮；以及(b)至少一种精油，其中N-甲基-1，2-苯并异噻唑啉-3-酮与精油的重量比为1∶52到1∶160,000。
此外，本发明涉及一种包含N-甲基-1，2-苯并异噻唑啉-3-酮和至少一种精油的产品，其中N-甲基-1，2-苯并异噻唑啉-3-酮与精油的重量比为1∶52到1∶160,000。
最后，本发明涉及一种干膜，其由包含以下步骤的方法制成：在基板上涂覆一层前述涂料组合物，并且干燥涂料组合物或使涂料组合物变干。
具体实施方式
如本文所用，除非上下文另外明确指出，否则以下术语具有指定定义。“MBIT”为N-甲基-1，2-苯并异噻唑啉-3-酮。术语“精油”是指含有从植物中所衍生的挥发性芳香化合物的疏水性液体。精油的实例包括油，诸如矿物油、冬青油、蓖麻油、松油、杏仁油、香茅油、百里香油以及迷迭香油。本发明精油包括百里香油CAS号8007-46-3和迷迭香油CAS号8000-25-7。术语“杀微生物剂”与“抗微生物剂”同义，是指能够杀灭、抑制或控制微生物在某一场所生长的化合物；杀微生物剂包括杀细菌剂、杀真菌剂以及除藻剂。
术语“微生物”包括例如真菌(诸如酵母菌和霉菌)、细菌以及藻类，较佳包括真菌和细菌。术语“场所(locus)”是指受到微生物污染的工业系统或产品。整篇说明书中使用以下缩写：ppm＝每百万份的重量份(重量/重量)、mL＝毫升、ATCC＝美国典型培养物保藏中心、MBC＝最低杀生物浓度、并且MIC＝最低抑制浓度。除非另外规定，否则温度以摄氏度(℃)为单位，并且所提及的百分比(％)是按重量计。以活性成分计以ppm(w/w)为单位提供有机杀微生物剂的量。
已意外发现，本发明组合物在合并的活性成分含量低于单一杀微生物剂的活性成分含量下提供增强的杀微生物功效。超出权利要求书中所列的那些杀微生物剂以外的其它杀微生物剂可存在于组合物中。
抗微生物组合物包含N-甲基-1，2-苯并异噻唑啉-3-酮和精油。
在本发明的某些组合物中，抗微生物组合物包含N-甲基-1，2-苯并异噻唑啉-3-酮和百里香油。优选地，N-甲基-1，2-苯并异噻唑啉-3-酮与百里香油的重量比为1∶52到1∶160,000。
在本发明的某些组合物中，抗微生物组合物包含N-甲基-1，2-苯并异噻唑啉-3-酮和迷迭香油。优选地，N-甲基-1，2-苯并异噻唑啉-3-酮与迷迭香油的重量比为1∶250到1∶16,000。
本发明组合物中的杀微生物剂可以“按原样”使用或可以先用溶剂或固体载剂对其进行调配。适合溶剂包括，例如水；二醇，诸如乙二醇、丙二醇、二乙二醇、二丙二醇、聚乙二醇以及聚丙二醇；丙三醇；二醇醚；诸如丙二醇醚、二乙二醇单丁基醚、二丙二醇甲基醚、乙二醇乙醚、乙二醇单丁基醚；醇，诸如甲醇、乙醇、丙醇、异丙醇、苯乙醇、苯氧乙醇以及苯氧丙醇；酮，诸如丙酮和甲基乙基酮；酯，诸如乙酸乙酯、乙酸丁酯、柠檬酸三乙酰酯以及三乙酸甘油酯；碳酸酯，诸如碳酸丙烯酯和碳酸二甲酯及其混合物。溶剂优选地选自水、二醇、二醇醚、酯以及其混合物。适合固体载剂包括，例如环糊精、二氧化硅、粘土、动物脂肪、硅藻土、蜡、纤维素材料、碱金属和碱土金属(例如钠、镁、钾)金属盐(例如氯化物、硝酸盐、溴化物、硫酸盐)以及木炭。
当在溶剂中调配杀微生物剂组分时，配方可任选地含有表面活性剂。当此类配方含有表面活性剂时，它们一般呈可乳化浓缩液、乳液、微乳化浓缩液或微乳液形式。可乳化浓缩液在添加足够量的水之后会形成乳液。微乳化浓缩液在添加足够量的水之后会形成微乳液。此类乳化和微乳化浓缩液一般为本领域中所熟知的；此类配方优选地不含表面活性剂。对于关于制备不同微乳液和微乳化浓缩液的进一步的一般细节和具体细节可参考美国专利第5,444,078号。
杀微生物剂组分亦可被调配呈分散液形式。分散液的溶剂组分可为有机溶剂或水，优选地为水。此类分散液可含有佐剂，例如共溶剂、钳合剂或螯合剂、胺类、增稠剂、抗冷冻剂、分散剂、填充剂、颜料、表面活性剂、生物分散剂、磺基丁二酸酯、萜类、呋喃酮、聚阳离子、稳定剂、阻垢剂以及抗腐蚀添加剂。
所属领域的技术人员应了解，可依次、同时将本发明杀微生物剂组分添加到所在场所，或可在添加到所在场所之前进行合并。优选地，同时或依次将第一杀微生物剂和第二杀微生物剂组分添加到所在场所中。当同时或依次添加杀微生物剂时，每一单个组分可含有佐剂，诸如溶剂、增稠剂、抗冷冻剂、著色剂、螯合剂(诸如乙二胺四乙酸、乙二胺二丁二酸、亚胺二丁二酸及其盐)、分散剂、表面活性剂、生物分散剂、磺基丁二酸酯、萜类、呋喃酮、聚阳离子、稳定剂、阻垢剂以及抗腐蚀添加剂。
可通过将杀微生物有效量的组合物引入受到微生物侵袭的所在场所处来使用本发明杀微生物组合物。适合场所包括例如：工业工艺用水；电涂沉积系统；冷却塔；空气洗涤器；气体洗涤器；矿浆；废水处理；观赏性喷泉；逆渗透过滤；超过滤；压舱水；蒸发冷凝器；热交换器；纸浆和造纸加工流体以及添加剂；淀粉；塑料；乳液；分散液；油漆；胶乳；涂料，诸如清漆；建筑产品，诸如胶泥、嵌缝胶以及密封剂；建筑胶粘剂，诸如陶瓷胶粘剂、地毯背衬胶粘剂以及层压胶粘剂；工业或消费型胶粘剂；摄影化学品；印刷流体；家用产品，诸如盥洗室和厨房清洁剂以及卫生擦拭物；化妆品；洗漱用品、洗发剂；肥皂；去垢剂；工业清洁剂；地板抛光剂；衣物漂洗水；金属加工流体；输送机润滑剂；液压流体；皮革和皮革产品；纺织物；纺织品；木材和木材品，诸如胶合板、木屑板、墙板、刨花板(flakeboard)、叠层梁(laminatedbeam)、定向绞合板、硬质纤维板以及碎木板(particleboard)；石油加工液；燃料；油田流体，诸如喷水、压裂液以及钻井泥浆；农业佐剂保存；表面活性剂保存；医疗装置；诊断性试剂保存；食品保存，诸如食品塑料或纸质包装；食品；饮料以及工业工艺巴氏灭菌器；抽水马桶；娱乐用水；水池以及温泉。
优选地，本发明杀微生物组合物用于抑制微生物在选自以下各者中的一个或多个场所的生长：工业工艺用水；超过滤；工业或消费型胶粘剂；家用产品；化妆品；洗漱用品；洗发剂；肥皂；去垢剂；工业清洁剂；地板抛光剂；衣物漂洗水；医疗装置；诊断性试剂保存；食品；饮料以及工业工艺巴氏灭菌器；抽水马桶；娱乐用水；水池以及温泉。
抑制或控制微生物和较高水生生命形态在所在场所中生长所需的本发明组合物的特定量取决于受保护的具体场所。通常，如果在所在场所中组合物提供0.1到1,000ppm的异噻唑啉成分，那么控制微生物在所在场所中生长的本发明组合物量为足够的。优选地，组合物的异噻唑酮成分以至少0.5ppm，更优选至少4ppm并且最优选至少10ppm的量存在于所在场所中。优选地，组合物的异噻唑酮成分以不超过1000ppm，更优选不超过500ppm，并且最优选不超过200ppm的量存在于所在场所中。
本发明杀微生物组合物可包括在涂料组合物中。可单独地或呈混合物形式或其任何组合将N-甲基-1，2-苯并异噻唑啉-3-酮和至少一种精油添加到涂料组合物中。优选的涂料组合物是液体。涂料组合物可以是水性或非水性的。按涂料组合物的重量计，水性涂料组合物一般含有混合物重量的30％或更多的水。
在其中N-甲基-1，2-苯并异噻唑啉-3-酮和至少一种精油包括在油漆或其它涂料组合物中的实施例中，优选的涂料组合物为液体组合物，尤其含有聚合物在水性介质中的分散液的组合物。
涂料组合物被设计成使得可以将一层涂料组合物容易地涂覆到衬底上，并且随后进行干燥或使其变干以形成干膜。涂料组合物含有粘合剂。粘合剂含有以下中的一种或多种：一种或多种聚合物、一种或多种低聚物和/或一种或多种单体。粘合剂中的低聚物和单体被设计成用于在形成干膜期间或之后聚合和/或交联。粘合剂中的聚合物可以或可以不被设计成在形成干膜期间或之后交联。
涂料组合物任选地含有一或多种颜料。颜料是呈小固体粒子形式的矿物或有机物质。颜料为干膜提供完全或部分的不透明度。
抗微生物化合物组合适用于保存涂覆油漆或其它液体涂料组合物之后所得的干膜涂层。优选地，抗微生物组合物是包含本文所揭示的抗微生物化合物组合中一或多种的水性乳胶漆，或干膜涂层由将油漆涂覆到表面而产生。水性乳胶漆是水性液体涂料组合物，其中粘合剂是呈乳胶形式(即，呈聚合物粒子分散在整个水中的形式)的聚合物。更优选的是其中粘合剂含有一或多种丙烯酸聚合物的水性乳胶漆。
本发明还涵盖一种用于在建筑材料中，尤其在干膜涂层中防止微生物生长的方法，其通过将所主张的抗微生物化合物组合中的任一种并入到材料中来进行。
通常，抗微生物组合物用于抑制细菌和/或真菌的生长。预期一些实施例可含有一或多种额外的抗微生物化合物。
实例
材料和方法
通过测试大范围的化合物浓度和比率来证明本发明组合的协同作用。
协同作用的一个测量方式为由库尔F.C.；艾斯曼P.C.；斯威托维兹H.D.和迈尔R.L.在应用微生物学(Applied Microbiology)9：538-541(1961)中所描述的工业上的公认方法，使用比率通过下式测定：
Qa/QA+Qb/QB＝协同指数(“SI”)
其中：
QA＝单独起作用的化合物A(第一组分)的浓度(ppm)，其产生端点(化合物A的MIC)。
Qa＝混合物中化合物A的浓度(ppm)，其产生端点。
QB＝单独起作用的化合物B(第二组分)的浓度(ppm)，其产生端点(化合物B的MIC)。
Qb＝混合物中化合物B的浓度(ppm)，其产生端点。
当Qa/QA与Qb/QB之和大于1时，表示拮抗作用。当和等于1时，表明加成作用，并且当小于1时，证明协同作用。SI越低，由特定混合物所显示出的协同作用越强。杀微生物剂的最低抑制浓度(MIC)为在防止增加的微生物生长的一组特定条件下进行测试的最低浓度。被测试的微生物为大肠杆菌(大肠杆菌，ATCC#8739)、酵母菌、白色念珠菌(白色念珠菌，ATCC#10231)以及霉菌、黑曲霉(黑曲霉，ATCC#16404)。
通过评估抑制微生物生长所需的最低杀生物剂或杀生物剂掺合物浓度来确定MBIT与第二杀生物剂的协同作用。使用96孔微量滴定板形式进行全部研究。针对全部研究，将含有不同浓度的单独MBIT、单独第二杀生物剂或两种杀生物化学物质的组合的200μl微生物生长培养基添加到微量滴定板的个别孔中。确切地说，胰酶大豆培养液(TSB)用于细菌(大肠杆菌，ATCC#8739)，酵母菌麦芽萃取物培养液(YMB)用于酵母菌(白色念珠菌，ATCC#10231)并且马铃薯右旋糖培养液(PDB)用于霉菌(黑曲霉，ATCC#16404)。将最终浓度呈104CFU/mL或104个孢子/毫升的测试生物体施加到平行实验中的每一孔中以开始MIC评估。利用不含杀生物剂之生长培养基作为每一实验设定中的对照组以确认每一生物体的生长存活率。
除了这些杀生物剂浓度的64个可能性组合以外，在微生物生长抑制研究中评估每一个别杀生物剂的8个浓度(2倍稀释)。需要评估个别杀生物剂浓度来获得抑制浓度端点以供进行协同指数计算。添加生物体之后，将96孔微量滴定板在25℃下培育48小时或直至在不含杀生物剂的对照孔中观察到生长为止。基于视觉生物体生长浊度将个别孔评分为生长或无生长。除产生微生物生长抑制的合并的杀生物剂浓度以外，记录下使得生物体无生长的最低单一活性杀生物剂浓度、MBIT和第二杀生物剂的浓度以供计算协同指数。
这些微生物代表了许多消费型和工业应用中的天然污染物。在25℃(酵母菌和霉菌)或30℃(细菌)下培育不同时间之后，在视觉上评估各板的微生物生长(浊度)以便确定MIC。
证明本发明MBIT组合的协同作用的测试结果展示在下表1和表2中。
展现协同作用的两种杀生物剂的比率展示在下表1和表2中。
表1
Figure BDA0001022211370000061
Figure BDA0001022211370000071
在比率1∶52到1∶160,000下证明了MBIT与百里香的协同作用。
表2
Figure BDA0001022211370000072
Figure BDA0001022211370000081
在比率1∶250到1∶16,000下证明了MBIT与迷迭香的协同作用。

Claims (7)

1.一种杀微生物组合物，所述杀微生物组合物包含：
(a)N-甲基-1,2-苯并异噻唑啉-3-酮；以及
(b)至少一种精油；
其中，所述精油选自百里香油和迷迭香油，
限制条件是，当所述精油为百里香油时，N-甲基-1,2-苯并异噻唑啉-3-酮与精油的重量比为1:52到1:160,000，而当所述精油为迷迭香油时，N-甲基-1,2-苯并异噻唑啉-3-酮与迷迭香油的重量比为1:250到1:16,000。
2.一种抑制或控制微生物生长的方法，所述方法包含以下步骤：将根据权利要求1所述的杀微生物组合物添加到选自下组的一个或多个场所中：工业工艺用水中；超过滤；工业或消费型胶粘剂；家用产品；工业清洁剂；衣物漂洗水；医疗装置；诊断试剂保存；食品；饮料和工业工艺巴氏灭菌器；娱乐用水；水池以及温泉。
3.一种抑制或控制微生物生长的方法，所述方法包含以下步骤：将根据权利要求1所述的杀微生物组合物添加到选自下组的一个或多个场所中：化妆品；洗漱用品；去垢剂；抽水马桶；和地板抛光剂。
4.一种抑制或控制微生物生长的方法，所述方法包含以下步骤：将根据权利要求1所述的杀微生物组合物添加到选自下组的一个或多个场所中：洗发剂，和肥皂。
5.一种涂料组合物，其包含根据权利要求1所述的杀微生物组合物。
6.一种产品，其包含根据权利要求1所述的杀微生物组合物。
7.一种干膜，其由包含以下步骤的方法制成：在基板上涂覆一层根据权利要求5所述的涂料组合物，并且干燥所述涂料组合物或使所述涂料组合物变干。
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