CN110934141B - 一种固态过氧乙酸长效灭菌粉及其制备方法 - Google Patents

一种固态过氧乙酸长效灭菌粉及其制备方法 Download PDF

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CN110934141B
CN110934141B CN201811108542.5A CN201811108542A CN110934141B CN 110934141 B CN110934141 B CN 110934141B CN 201811108542 A CN201811108542 A CN 201811108542A CN 110934141 B CN110934141 B CN 110934141B
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杨妍妍
张万国
邹贤信
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Likang Pharmaceutical Technology Jiangsu Co ltd
Shanghai Likang Disinfection High Tech Co ltd
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N37/00Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
    • A01N37/16Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing the group; Thio analogues thereof
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N37/00Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
    • A01N37/18Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing the group —CO—N<, e.g. carboxylic acid amides or imides; Thio analogues thereof

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Abstract

本发明公开了一种固态过氧乙酸长效灭菌粉,其组分及其重量百分含量如下:过氧根离子载体25.7‑43.4%;乙酰基载体15.8‑22.8%;酸度调节剂38.2‑55.0%;表面活性剂0.54‑0.77%;以上组分的重量百分含量总和为100%。本发明采用pH敏感性材料对酸度调节剂进行预先包衣,然后与过氧根离子载体、乙酰基载体和表面活性剂进行混合组成固态过氧乙酸长效灭菌粉。本发明提供的过氧乙酸灭菌粉性质稳定,保质期可达两年。与液体过氧乙酸相比,本发明过氧乙酸灭菌粉具有刺激性较弱,使用方便、安全,便于运输、储存等优点,枯草杆菌黑色变种芽孢ATCC9372具有很强的杀灭作用。本发明还涉及该过氧乙酸灭菌粉的制备方法。

Description

一种固态过氧乙酸长效灭菌粉及其制备方法
技术领域
本发明属于消毒杀菌剂技术领域,具体涉及一种固态过氧乙酸长效灭菌粉,此外本发明还涉及该过氧乙酸灭菌粉的制备方法。
背景技术
过氧乙酸由过氧化氢衍生出来的,其氧化能力在杀菌领域要远远大于过氧化氢,是一种广谱、高效、低廉的消毒剂和灭菌剂,对细菌繁殖体、真菌、病毒和芽孢等都有较强的杀灭作用。过氧乙酸被广泛应用于医疗器械及其他被病菌病毒污染的物品的消毒过程中,它是饮用水的消毒剂、杀菌灭菌剂和清洗剂,也是环境、物表、空气等疫源地消毒和预防性消毒的药品。过氧乙酸之所以被人们所看好,不仅仅是因为它的强氧化作用和高效、广谱杀菌作用,更重要的是它在使用后残留物为水、二氧化碳和氧,安全环保、完全无毒,是无污染洁净的氧化杀菌物质,在使用上完全符合环保标准。
从20世纪初人们首次利用过氧化氢和醋酸(或醋酸酐)合成过氧乙酸,到后来的利用乙醛氧化法生成过氧乙酸,随着科学技术的不断发展、工业技术的不断进步,制备过氧乙酸的方法也日新月异,例如过氧化氢与乙酰氯、乙酰酮以及乙酸和氧气在臭氧和紫外线照射的条件下反应等等,但是这些工艺制备的过氧乙酸都是以液体形态,不可避免存在以下缺点:1、由于溶液中同时含有大量醋酸的存在,使得样品不可避免具有醋酸的强烈刺激性气味。2、过氧乙酸由于其分子结构易释放原子态的氧从而稳定性很差,浓度大于20%时在高温条件下即有爆炸危险,而低浓度时易分解,不易贮存。3、使用时为酸性环境,过氧乙酸本身为强氧化剂,腐蚀性强,易造成器材的腐蚀损耗。
因此,为克服液体过氧乙酸不稳定、腐蚀性强、刺激性气味大等缺点,探索和开发固态过氧乙酸灭菌粉是非常有必要的。
发明内容
针对现有技术的上述不足,根据本发明的实施例,希望提供一种性质稳定,保质期限长久,刺激性弱,使用方便、安全,便于运输和储存,对枯草杆菌黑色变种芽孢ATCC9372具有很强杀灭作用的固态过氧乙酸长效灭菌粉并提供其制备方法。
根据实施例,本发明提供的一种固态过氧乙酸长效灭菌粉,其组分及其重量百分含量如下:
过氧根离子载体25.7-43.4%;
乙酰基载体15.8-22.8%;
酸度调节剂38.2-55.0%;
表面活性剂0.54-0.77%;
以上组分的重量百分含量总和为100%。
根据一个实施例,本发明前述固态过氧乙酸长效灭菌粉中,所述过氧根离子载体选自过氧化钠、过硼酸盐和过碳酸盐。
根据一个实施例,本发明前述固态过氧乙酸长效灭菌粉中,所述乙酰基载体选自乙酰乙胺、对二乙酰乙二胺和四乙酰乙二胺。
根据一个实施例,本发明前述固态过氧乙酸长效灭菌粉中,所述酸度调节剂是由pH敏感性材料与酸按照一定比例包衣而成,pH敏感性材料是欧巴代,酸为柠檬酸或羟基乙叉二膦酸。
根据实施例,本发明提供的一种固态过氧乙酸长效灭菌粉的制备方法,包括如下工艺步骤:以丙酮为溶剂,配制浓度为12~15%的欧巴代包衣液,将包衣液与酸按1:10混合均匀,并于流化床40℃干燥,冷至室温,得到酸度调节剂。将过氧根离子载体、乙酰基载体、表面活性剂置于40~50℃烘箱烘5小时,冷至室温。在20~30℃,10~20%RH的条件下,将过氧根离子载体、乙酰基载体、酸度调节剂、表面活性剂混合均匀,即可制得固态过氧乙酸长效灭菌粉。
本发明采用pH敏感性材料对酸度调节剂进行预先包衣,然后与过氧根离子载体、乙酰基载体和表面活性剂进行混合组成固态过氧乙酸长效灭菌粉。本发明固态过氧乙酸长效灭菌粉溶于水中,包衣的酸度调节剂缓慢释放酸性调节剂,为生成的过氧乙酸提供合适的pH环境,提升过氧乙酸的稳定性,显著延长过氧乙酸的使用周期。
本发明固态过氧乙酸长效灭菌粉,具有以下优点:1、固体形式存在,在使用前无味;溶解使用时也基本无味道。2、采用特殊分子结构牢固吸附活性氧,在固体形态时,不易分解,安全性高。3、使用为中性环境,有效避免了过氧乙酸对器材的腐蚀。4、溶解时间快,室温条件下30分钟到1小时即可溶解,释放高浓度的活性氧,高效消毒灭菌。5、使用时间长,溶解后可有效使用72小时。
相对于现有技术,本发明提供的过氧乙酸灭菌粉性质稳定,保质期可达两年。与液体过氧乙酸相比,本发明过氧乙酸灭菌粉具有刺激性较弱,使用方便、安全,便于运输、储存等优点。除此之外,本发明过氧乙酸灭菌粉对枯草杆菌黑色变种芽孢ATCC9372具有很强的杀灭作用。
具体实施方式
下面结合具体实施例,进一步阐述本发明。这些实施例应理解为仅用于说明本发明而不用于限制本发明的保护范围。在阅读了本发明记载的内容之后,本领域技术人员可以对本发明作各种改动或修改,这些等效变化和修改同样落入本发明权利要求所限定的范围。
以丙酮为溶剂,配制浓度为12~15%的欧巴代包衣液,将包衣液与酸按1:10混合均匀,并于流化床40℃干燥,冷至室温,得到酸度调节剂。将过氧根离子载体、乙酰基载体、表面活性剂置于40~50℃烘箱烘5小时,冷至室温。在20~30℃,10~20%RH的条件下,将过氧根离子载体、乙酰基载体、酸度调节剂、表面活性剂混合均匀,即可制得固态过氧乙酸长效灭菌粉。
实施例1
称取1.5g欧巴代,加入10mL丙酮,配制成15%的欧巴代包衣液,将1.4g包衣液与14g柠檬酸混合均匀,并于流化床40℃干燥,冷至室温,得到酸度调节剂。将8.5g过碳酸钠、5.8g四乙酰乙二胺、0.2g十二烷基苯磺酸钠置于40~50℃烘箱烘5小时,冷至室温。在20~30℃,10~20%RH的条件下,将8.5g过碳酸钠、5.8g四乙酰乙二胺、14g酸度调节剂、0.2g十二烷基苯磺酸钠混合均匀,即可制得固态过氧乙酸长效灭菌粉。
实施例2
称取1.5g欧巴代,加入10mL丙酮,配制成15%的欧巴代包衣液,将1.4g包衣液与14g柠檬酸混合均匀,并于流化床40℃干燥,冷至室温,得到酸度调节剂。将12.5g过硼酸钠、6g对二乙酰乙二胺、0.2g十二烷基硫酸钠置于40~50℃烘箱烘5小时,冷至室温。在20~30℃,10~20%RH的条件下,将12.5g过硼酸钠、6g对二乙酰乙二胺、14g酸度调节剂、0.2g十二烷基硫酸钠混合均匀,即可制得固态过氧乙酸长效灭菌粉。
实施例3
称取1.5g欧巴代,加入10mL丙酮,配制成15%的欧巴代包衣液,将1.68g包衣液与16.8g羟基乙叉二膦酸混合均匀,并于流化床40℃干燥,冷至室温,得到酸度调节剂。将12g过硼酸钠、5.5g四乙酰乙二胺、0.25g二甲基苯磺酸钠置于40~50℃烘箱烘5小时,冷至室温。在20~30℃,10~20%RH的条件下,将12g过硼酸钠、5.5g四乙酰乙二胺、16.8g酸度调节剂、0.25g二甲基苯磺酸钠混合均匀,即可制得固态过氧乙酸长效灭菌粉。
试验例1
依据《消毒技术规范》(卫生部2002年版)进行稳定性测定,取上述各实施例固态过氧乙酸长效灭菌粉置37℃恒温箱内3个月,平均过氧乙酸含量下降率为8.50%,有效期为2年。实验结果如表1所示。
表1.固态过氧乙酸长效灭菌粉加速稳定性实验结果
Figure BDA0001808479230000051
试验例2
依据《消毒技术规范》(卫生部2002年版)进行杀菌试验,取上述各实施例固态过氧乙酸长效灭菌粉的水溶液(含过氧乙酸2.0g/L;过氧化氢1.25g/L),进行5次试验,均浸泡10min,对不锈钢载体上的枯草杆菌黑色变种芽孢ATCC9372完全杀灭,定性灭菌试验合格(各试验组均无菌生长)。实验结果如表2所示。
表2.固态过氧乙酸长效灭菌粉水溶液对枯草杆菌黑色变种芽孢的定性灭菌实验结果
Figure BDA0001808479230000052
注:1.“-”表示无菌生长。
2.各次试验阴性对照均无菌生长。
3.各次试验阳性对照均有菌生长。
综上所述,本发明固态过氧乙酸长效灭菌粉性质稳定,保质期可达两年。与液体过氧乙酸相比,本发明过氧乙酸灭菌粉具有刺激性较弱,使用方便、安全,便于运输、储存等优点。除此之外,本发明过氧乙酸灭菌粉对枯草杆菌黑色变种芽孢ATCC9372具有很强的杀灭作用。

Claims (3)

1.一种固态过氧乙酸长效灭菌粉,其特征是,其组分及其重量百分含量如下:
过氧根离子载体25.7-43.4%;
乙酰基载体15.8-22.8%;所述乙酰基载体选自乙酰乙胺、对二乙酰乙二胺和四乙酰乙二胺;
酸度调节剂38.2-55.0%;该酸度调节剂由pH敏感性材料与酸包衣而成;所述pH敏感性材料是欧巴代,所述酸为柠檬酸或羟基乙叉二膦酸;
表面活性剂0.54-0.77%;
以上组分的重量百分含量总和为100%。
2.根据权利要求1所述的固态过氧乙酸长效灭菌粉,其特征在于,所述过氧根离子载体选自过氧化钠、过硼酸盐和过碳酸盐。
3.一种根据权利要求1-2所述的任一固态过氧乙酸长效灭菌粉的制备方法,其特征是,包括如下工艺步骤:
以丙酮为溶剂,配制浓度为12~15%的欧巴代包衣液,将该包衣液与酸按照1:10进行包衣,并于流化床40℃干燥,冷至室温,得到酸度调节剂;所述酸为柠檬酸或羟基乙叉二膦酸;
将过氧根离子载体、乙酰基载体、表面活性剂置于40~50℃烘箱烘5小时,冷却至室温;
在20~30℃,10~20%RH的条件下,将过氧根离子载体、乙酰基载体、酸度调节剂、表面活性剂混合均匀,即制得固态过氧乙酸长效灭菌粉。
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