CN102186453A - 协同防腐混合物 - Google Patents

协同防腐混合物 Download PDF

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CN102186453A
CN102186453A CN2009801291529A CN200980129152A CN102186453A CN 102186453 A CN102186453 A CN 102186453A CN 2009801291529 A CN2009801291529 A CN 2009801291529A CN 200980129152 A CN200980129152 A CN 200980129152A CN 102186453 A CN102186453 A CN 102186453A
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罗西塔·努涅斯
约瑟夫·金伦
拉里·肯特·霍尔
克里斯特尔·内斯比特
克雷格·卡特
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Abstract

本发明公开了一种防腐配方，包含至少两种具有杀菌和/或杀真菌性能的化合物的组合，其中各组合选自：甲基异噻唑啉酮/吡罗克酮乙醇胺(piroctone olamine)；辛乙二醇(caprylyl glycol)/脱氢乙酸；十一烷醇/脱氢乙酸和月桂醇/山梨酸。

Description

协同防腐混合物
技术领域
本发明公开了包含杀菌和杀真菌化合物的协同防腐配方、减少制剂的细菌和真菌负荷的方法及本发明协同防腐配方用于减少制剂的细菌和真菌负荷的用途。
背景技术
大量个人、家用和工业产品、配方和制剂需要受到保护以免被细菌和真菌污染。这通常通过加入甲醛释放剂和/或对羟基苯甲酸酯类来实现，这是由于这些化合物的良好杀菌和杀真菌性能。
然而，现有技术的这些化合物有一些严重的缺点，即它们的保存能力太高使得其效果持续到甚至，例如洗液的情况下，其被涂覆到皮肤上、被吸收、分布于血液中并沉积在身体的主要器官上之后。由于甲醛和对羟基苯甲酸酯类损害酶功能，可能会干扰正常的人细胞和器官功能。
发明内容
因此，本发明所要解决的技术问题是提供避免现有技术的那些配方的缺点的防腐配方。这个问题通过至少两种化合物的惊人且不可预料的协同合作来减少所述配方的必要浓缩同时保持微生物控制而得以解决。
因此，本发明的一个目的是提供防腐配方，所述配方包含至少两种具有杀菌和/或杀真菌性能的化合物的组合，其中各组合选自：甲基异噻唑啉酮/吡罗克酮乙醇胺(piroctone olamine)；辛乙二醇(caprylyl glycol)/脱氢乙酸；十一烷醇/脱氢乙酸和月桂醇/山梨酸。
当所述杀菌化合物为甲基异噻唑啉酮时，优选所述杀菌化合物的浓度为1％-5％，而当其为辛乙二醇、十一烷醇和月桂醇时，其浓度为25％-75％。甚至更优选，当所述杀菌化合物为甲基异噻唑啉酮时，其浓度为1.5％％-3％，而当其为辛乙二醇、十一烷醇和月桂醇时，其浓度为30％-70％。
优选，所述杀真菌化合物的浓度为25％-99％。甚至更优选，本发明的杀真菌化合物的浓度为30％-95％。
除非另外明确说明，所有百分比以重量计。
甲基异噻唑啉酮的优选异构体为2-甲基异噻唑啉-3-酮。然而，其它异构体也落入本发明范围。
优选本发明的防腐配方与合适的溶剂组合。优选，所述溶剂选自二醇类。最优选，所述溶剂选自丙二醇、丁二醇和戊二醇。
本发明减少制剂的细菌和真菌负荷的方法优选包括将包含至少两种具有杀菌和/或杀真菌性能的化合物的防腐配方加入待保存的制剂中。优选的杀菌和杀真菌化合物、其优选浓度和组合如上所述。
通常，可将本发明制剂加入各种个人、家用和工业产品、配方和制剂中。
本发明的优选制剂选自如洗液、霜剂、软膏和油膏、洗净剂、清洁剂等化妆品制剂；妇女卫生制剂；擦拭剂；宠物护理制剂；如洗发剂、护发素、凝胶、固定剂和喷雾剂等护发制剂。
本发明的另一目的是本发明的协同防腐配方用于减少制剂的细菌和真菌负荷的用途。关于优选杀菌和杀真菌化合物、其优选浓度和组合及所述协同防腐配方可应用的优选制剂与以上给出的那些相同。
具体实施方式
现在通过以下非限定性实施例对本发明进行描述。
实施例1
进行防腐挑战试验以评价所述共混物在成品化妆品制剂中的性能。测试在本文中所述的洗发剂和洗液基体中进行。按照如下制备标准的混合细菌培养物。将金黄色葡萄球菌(ATCC 6538)、大肠杆菌(ATCC 8739)和绿脓杆菌(ATCC 9027)的三个单独胰酶大豆琼脂(Tryptic Soy Agar)斜面培养物在约35℃孵育～24小时。接着用5mL无菌磷酸盐缓冲液(Phosphate Buffered Dilution Water，PBDW)洗涤各斜面培养物。将该5mL转移到另外5mLBPDW以获得总共10mL的单独细菌悬浮液。在用PBDW空白样品校准仪器后通过分光光度法测定各单独的悬浮液在530nm的吸光率。将各单独的悬浮液标准化至～109CFU/mL。从各单独的悬浮液中将5ml无菌转移到一个无菌样品杯中以获得“混合细菌”。接着将0.2mL标准细菌溶液与40g的各种洗发剂和洗液样品进行孵育，每个样品被混合均匀。
将白色念珠菌(ATCC 10231)的两个单独的沙保罗氏琼脂(Sabouraud Agar)斜面培养物和黑曲霉(ATCC 16404)的三块沙保罗氏琼脂板在约30℃分别孵育～24小时和5天。接着用5mL无菌磷酸盐缓冲液(PBDW)洗涤念球菌斜面培养物。将该5mL转移到另外5mL BPDW中以获得总共10mL的单独念球菌悬浮液。就曲霉菌而言，将无菌棉签浸入10mL无菌PBDW管，接着浸入无菌Tween80管。然后将该棉签在各曲霉菌板之间来回，在每次孢子除去过程中将孢子转移到该10mL PBDW管中。从各悬浮液中将1mL转移到另外的9mL PBDW管中。在血球计数器上对这些1∶9悬浮液各自进行测定并将原始悬浮液标准化至～107细菌/mL。从各单独的悬浮液中将7mL无菌转移到一个无菌样品杯中以获得“混合真菌”。接着将0.4mL标准真菌溶液与40g的各种洗发剂和洗液样品进行孵育，每个样品被混合均匀。
在第0、7、14和28天。按照如下取样。将1克各样品无菌转移到另外的9mL D/E中性肉汤中以形成10-1稀释。在BPDW中制备系列稀释物至10-6稀释。通过带有胰酶大豆琼脂的倾倒板将细菌培养物的系列稀释物涂板并在～35℃孵育48小时。通过带有沙保罗氏琼脂的倾倒板将真菌样品的系列稀释物涂板并在～30℃孵育72小时。培养期后对各板计数。结果显示于表1和2中。28天后，所述共混物有效地减少细菌和真菌数。
表1
防腐挑战数据
混合细菌数(CFU/克)
Figure BPA00001307179900051
接种物：
混合细菌-接近等量的绿脓杆菌、金黄色葡萄球菌和大肠杆菌9×105-5.5×106
表2
防腐挑战数据
混合真菌数(CFU/克)
Figure BPA00001307179900052
接种物：
混合真菌-接近等量的白色念珠菌和黑曲霉6.9×104-1.2×105
实施例2
按照如下确定各组分和二元配方的最低抑菌浓度(MIC)。按照实施例1中所述制备金黄色葡萄球菌(革兰氏阳性)、大肠杆菌和绿脓杆菌(都是革兰氏阴性)的各细菌悬浮液和白色念珠菌和黑曲霉的各真菌悬浮液。用PBDW将各悬浮液标准化，分别获得～108CFU/mL或～107细菌/mL的各细菌和真菌。
将各组分和二元配方稀释于DI水或丙二醇(适合溶解的)以获得总共10,000ppm的原始活性溶液。采用该10,000ppm溶液，在无菌营养肉汤(Nutrient Broth)中进行1∶9稀释，获得1,000ppm活性溶液。将5mL所得1,000ppm稀释液转移到5mL无菌营养肉汤(NB)中以获得500ppm活性溶液。重复这种稀释方案直到下降至3.90ppm活性。在无菌沙氏葡萄糖肉汤(Sabouraud Dextrose Broth，SDB)中进行同样的稀释以进行真菌MIC测试。制备待测试的5种微生物每种的这种系列的9种活性溶液(3.9ppm-1000ppm)。
从大肠杆菌悬浮液中取0.1mL加入所得9种在NB中的5mL活性溶液的每一个中。将各试管充分混合。对每种细菌悬浮液重复这样的步骤。同样，将0.1mL白色念球菌悬浮液加入所得9种在SDB中的5mL活性溶液的每一个中。用黑曲霉在各组稀释液中重复这样的步骤。将各试管充分混合。通过适当地接种5mL NB或SDB制备各生物的对照物。将全部三组细菌试管在35℃孵育48小时，将两种真菌试管在30℃孵育72和120小时。培养期结束时，将各试管混合并相对对照物视觉观察浊度。将没有浊度的最低浓度记录为最低抑菌浓度(MIC)。将结果显示于表3和4中。
协同值(synergism value)为(QA/Qa+QB/Qb)。QA是混合物中组分A的浓度，Qa是单独使用的组分A的浓度，QB是混合物中组分B的浓度，Qb是单独使用的组分B的浓度。当协同值低于1时，混合物是有协同作用的(synergistic)。等于1和大于1的(QA/Qa+QB/Qb)分别表示相加效应和对抗效应。
表3
各防腐配方对细菌的MIC值(ppm)
Figure BPA00001307179900071
表4
各防腐配方对细菌、酵母和真菌的MIC值(ppm)
配方含有吡罗克酮乙醇胺
Figure BPA00001307179900081

Claims (9)

1.一种防腐配方，包含至少两种具有杀菌和/或杀真菌性能的化合物的组合，其中各组合选自：甲基异噻唑啉酮/吡罗克酮乙醇胺；辛乙二醇/脱氢乙酸；十一烷醇/脱氢乙酸和月桂醇/山梨酸。
2.根据权利要求1所述的化合物，其中当所述杀菌化合物为甲基异噻唑啉酮时，其浓度为1％-5％，而当其为辛乙二醇、十一烷醇和月桂醇时，其浓度为25％-75％。
3.根据权利要求2所述的化合物，其中当所述杀菌化合物为甲基异噻唑啉酮时，其浓度为1.5％-3％，而当其为辛乙二醇、十一烷醇和月桂醇时，其浓度为30％-70％。
4.根据权利要求1-3中的任一项所述的化合物，其中所述杀真菌化合物的浓度为25％-99％。
5.根据权利要求4所述的化合物，其中所述杀真菌化合物的浓度为30％-95％。
6.一种减少制剂的细菌和真菌负荷的方法，所述方法包括将权利要求1-5中任一项所述的防腐配方加入所述制剂中。
7.根据权利要求6所述的方法，其中所述制剂选自个人、家用和工业产品、配方和制剂。
8.根据权利要求7所述的方法，其中所述制剂选自如洗液、霜剂、软膏和油膏、洗净剂、清洁剂等化妆品制剂；妇女卫生制剂；擦拭剂；宠物护理制剂；如洗发剂、护发素、凝胶、固定剂和喷雾剂等护发制剂。
9.根据权利要求1-5中任一项所述的防腐配方用于减少制剂的细菌和真菌负荷的用途。
CN2009801291529A 2008-06-03 2009-05-20 协同防腐混合物 Expired - Fee Related CN102186453B (zh)

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CN109258648A (zh) * 2018-10-25 2019-01-25 黑龙江工业学院 一种食品机械用杀菌剂组合物

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AU2009254255B2 (en) 2014-02-27
CN102186453B (zh) 2013-11-13
WO2009146800A3 (en) 2010-07-22
ATE541554T1 (de) 2012-02-15
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EP2296614A2 (en) 2011-03-23
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WO2009146800A2 (en) 2009-12-10
BRPI0913389A2 (pt) 2015-11-24
EA021050B1 (ru) 2015-03-31
ZA201009047B (en) 2011-09-28
US20110301206A1 (en) 2011-12-08
US9060952B2 (en) 2015-06-23
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EP2153813A1 (en) 2010-02-17
BRPI0913389B1 (pt) 2017-07-04

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