CN114747570B - 一种超分子盐抑菌液及其制备方法 - Google Patents

一种超分子盐抑菌液及其制备方法 Download PDF

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CN114747570B
CN114747570B CN202210254602.4A CN202210254602A CN114747570B CN 114747570 B CN114747570 B CN 114747570B CN 202210254602 A CN202210254602 A CN 202210254602A CN 114747570 B CN114747570 B CN 114747570B
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任旭华
赵红川
项涛涛
沈珏锋
沈仿梁
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Zhejiang Lande Biotechnology Co ltd
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Abstract

本发明公开了一种超分子盐抑菌液，所述超分子盐抑菌液由以下质量百分含量的组分制成：0.2‑0.8%超分子盐抑菌剂，0.1‑0.3%蒲公英植物提取精油，4‑7%椰油酰胺两性基乙酸钠，5‑8%椰油基葡糖苷，4‑7%十二烷基硫酸酯铵，5‑7%三乙醇胺，1‑4%柠檬酸，0.3‑0.6%乙二胺四乙酸四钠，2‑4%烷基芳基磺酸盐，3‑5%异辛醇聚氧乙烯醚，余量为去离子水。本发明的超分子盐抑菌液配方合理科学，分散性与稳定性高，抑菌效果与使用安全性好的超分子盐抑菌液。本发明还公开了一种超分子盐抑菌液制备方法，工艺步骤简单，对设备要求低，可操作性强，适合工业化生产。

Description

一种超分子盐抑菌液及其制备方法
技术领域
本发明涉及一种抑菌液，尤其是涉及一种超分子盐抑菌液及其制备方法。
背景技术
公共环境往往夹杂很多微生物，包括常见的大肠杆菌、金黄色葡萄球菌、白色念珠菌。调查发现多数环境中存在的革兰氏阳性菌、大肠埃希氏菌存活时间长达2个月，主要通过与人接触而附着在人的皮肤上，因此，做好日常抑菌消毒是预防抑菌传染的最重要环节。
市面上销售的抑菌液种类繁多，大部分使用的是三氯生、对氯间二甲苯酚等有机化合物作为抑菌剂，这些有机抑菌剂一般具有毒性，长期使用会对肝脏系统、呼吸道产生刺激，使用安全性较差，且稳定性也较差。
发明内容
本发明是为了解决现有以有机化合物作为抑菌剂的抑菌液使用安全性与化学稳定性较差的问题，提供了一种配方合理科学，分散性与稳定性高，抑菌效果与使用安全性好的超分子盐抑菌液。
本发明还提供了一种超分子盐抑菌液制备方法，工艺步骤简单，对设备要求低，可操作性强，适合工业化生产。
为了实现上述目的，本发明采用以下技术方案：一种超分子盐抑菌液，所述超分子盐抑菌液由以下质量百分含量的组分制成：0.2-0.8％超分子盐抑菌剂，0.1-0.3％蒲公英植物提取精油，4-7％椰油酰胺两性基乙酸钠，5-8％椰油基葡糖苷，4-7％十二烷基硫酸酯铵，5-7％三乙醇胺，1-4％柠檬酸，0.3-0.6％乙二胺四乙酸四钠，2-4％烷基芳基磺酸盐，3-5％异辛醇聚氧乙烯醚，余量为去离子水。本发明以超分子盐抑菌剂作为主要抑菌成分，同时辅以蒲公英植物提取精油，具有安全、环保、抑菌效果好等优点；而本发明为解决超分子盐抑菌剂在水中溶解度低，不易均匀溶解的问题，本发明中以椰油酰胺两性基乙酸钠、椰油基葡糖苷、十二烷基硫酸酯铵、乙二胺四乙酸四钠、烷基芳基磺酸盐及异辛醇聚氧乙烯醚作为复合增溶体系，以增加超分子盐抑菌剂在水中的溶解度并形成溶液，本发明中对于增溶体系的原料及含量选择非常重要，增溶体系的原料及含量选择不当，均会造成产品浑浊不透明，因此，基于HLB 值、兼容性等多种因素的考虑，本发明选择椰油酰胺两性基乙酸钠、椰油基葡糖苷、十二烷基硫酸酯铵、乙二胺四乙酸四钠、烷基芳基磺酸盐及异辛醇聚氧乙烯醚进行复配形成增溶体系，并严格限定各组分的含量，同时添加三乙醇胺及柠檬酸作为pH缓冲剂，维持整个溶液体系pH的稳定，最终使本发明的超分子盐抑菌液最终能够获得均一、稳定的状态，稳定性高。
作为优选，所述超分子盐抑菌剂为甜菜碱水杨酸超分子离子盐、烟酰胺壬二酸超分子离子盐或左旋肉碱酚酸超分子离子盐。
作为优选，所述甜菜碱水杨酸超分子离子盐通过以下方法制得：将水杨酸和食品级甜菜碱加入无水乙醇中，水杨酸和食品级甜菜碱的摩尔比为(1-1.2)：(0.8-1)，搅拌均匀后升温至40-50℃反应4-8h，反应后冷却至-10℃，减压过滤，过滤物用无水乙醇洗涤后，减压干燥，即得甜菜碱水杨酸超分子离子盐。
作为优选，所述烟酰胺壬二酸超分子离子盐通过以下方法制得：将烟酰胺和壬二酸加入醇水混合物中，烟酰胺和壬二酸的摩尔比为(0.95-1)：(1-1.05)，搅拌均匀后升温至50-60℃反应3-5h，减压过滤，过滤物减压干燥，即得烟酰胺壬二酸超分子离子盐。本发明设计了烟酰胺壬二酸超分子离子盐的制备方法，工艺步骤简单，操作方便，收率与纯度高，实验证明，烟酰胺壬二酸超分子盐具有较好的抑菌效果。
作为优选，所述醇水混合物为异丙醇与去离子水按质量比1:1.5混合而成。
作为优选，所述左旋肉碱酚酸超分子离子盐通过以下方法制得：将左旋肉碱、没食子酸及水杨酸加入无水乙醇中，左旋肉碱、没食子酸及水杨酸的摩尔比为(1.9-2)：(1-1.05)： (1-1.05)，搅拌均匀后升温至40-50℃反应4-6h，反应后冷却至-10℃，减压过滤，过滤物用无水乙醇洗涤后，减压干燥，即得左旋肉碱酚酸超分子离子盐。本发明设计了左旋肉碱酚酸超分子离子盐的制备方法，工艺步骤简单，操作方便，收率与纯度高；实验证明，左旋肉碱酚酸超分子离子盐具有较好的抑菌效果。
一种超分子盐抑菌液制备方法，所述制备方法包括以下步骤：按质量百分含量配比称取各组分后，先将椰油酰胺两性基乙酸钠、椰油基葡糖苷、十二烷基硫酸酯铵、三乙醇胺、柠檬酸、乙二胺四乙酸四钠、烷基芳基磺酸盐、异辛醇聚氧乙烯醚和去离子水混合后，在搅拌状态下加热，再加入蒲公英植物提取精油、超分子盐抑菌剂，最后搅拌至全部溶解，冷却，静置至泡沫消失，即得超分子盐抑菌液。本发明中最后加入蒲公英植物提取精油、超分子盐抑菌剂，以便于蒲公英植物提取精油、超分子盐抑菌剂能均匀、充分溶解、分散；在加热状态下加入，有助于提高溶解速度与溶解效果。
作为优选，所述加热温度为50-55℃。
因此，本发明具有如下有益效果：
(1)设计得到了一种超分子盐抑菌液，以超分子盐抑菌剂作为主要抑菌成分，同时配以增溶体系，配方合理科学，稳定性高，抑菌效果与使用安全性好；
(2)设计得到了一种超分子盐抑菌液制备方法，通过分步混配即可，工艺步骤简单，对设备要求低，可操作性强，适合工业化生产。
附图说明
图1是本实施例4中得到的超分子盐抑菌液实物图。
图2是对比例1中得到的超分子盐抑菌液实物图。
图3是对比例2中得到的超分子盐抑菌液实物图。
图4是对比例3中得到的超分子盐抑菌液实物图。
具体实施方式
下面结合具体实施方式对本发明做进一步的描述。
实施例1
(1)制备甜菜碱水杨酸超分子离子盐
将水杨酸138.12g(1mol)和食品级甜菜碱93.72g(0.8mol)加入600g无水乙醇中，搅拌均匀后升温至40℃反应6h，反应后冷却至-10℃，减压过滤，过滤物用无水乙醇洗涤后，减压干燥，得白色固体粉末(甜菜碱水杨酸超分子离子盐)190g，收率为93％。
元素分析C12H17NO5
项目 C％ H％ N％ O％
计算值 56.47 6.67 5.49 31.37
测定值 56.3 6.69 5.45 31.40
实施例2
制备烟酰胺壬二酸超分子离子盐
将烟酰胺112.13g(1mol)和壬二酸197.63g(1.05mol)加入醇水混合物(异丙醇300g+水450g) 中，拌均匀后升温至50℃反应3h，减压过滤，过滤物减压干燥，得白色粉末(烟酰胺壬二酸超分子离子盐)260g，收率为84％.
元素分析C15H22N2O5
项目 C％ H％ N％ O％
计算值 58.06 7.10 9.03 25.81
测定值 58.01 7.12 8.99 25.85
实施例3
制备左旋肉碱酚酸超分子离子盐
将左旋肉碱322.4g(2mol)、没食子酸178.63g(1.05mol)及水杨酸145.02g(1.05mol)加入 600g无水乙醇中，搅拌均匀后升温至40℃反应6h，反应后冷却至-10℃，减压过滤，过滤物用无水乙醇洗涤后，减压干燥，得白色固体粉末(左旋肉碱酚酸超分子离子盐)520g，收率为83％。
元素分析C14H21NO7
项目 C％ H％ N％ O％
计算值 53.33 6.67 4.44 35.56
测定值 53.30 6.70 4.41 35.58
对实施例1得到的甜菜碱水杨酸超分子离子盐、实施例2得到的烟酰胺壬二酸超分子离子盐及实施例3得到的左旋肉碱酚酸超分子离子盐进行抗菌和抑菌效果测试，测试方法采用 WS/T650-2019抗菌和抑菌效果评价方法，测试结果如表1所示。
表1实施例1-3中得到的超分子离子盐抗菌和抑菌效果
Figure SMS_1
从表1可以看出，实施例1-3中得到的超分子离子盐对大肠杆菌及金黄色葡萄球菌具有优异的抑菌效果。
实施例4
按表2所示的配方称取各组分，先将椰油酰胺两性基乙酸钠、椰油基葡糖苷、十二烷基硫酸酯铵、三乙醇胺、柠檬酸、乙二胺四乙酸四钠、烷基芳基磺酸盐、异辛醇聚氧乙烯醚和去离子水混合后，在搅拌状态下加热至50-55℃，再加入蒲公英植物提取精油、超分子盐抑菌剂，最后搅拌至全部溶解，冷却，静置至泡沫消失，即得超分子盐抑菌液。
得到的超分子盐抑菌液实物如图1所示。从图1可见，得到的产品均匀、透明，无沉淀。
对比例1
对比例1与实施例4相比，区别在于：未添加三乙醇胺及柠檬酸，用去离子水替代，其余与实施例4完全相同。得到的超分子盐抑菌液实物如图2所示。
从图2可见，得到的产品朦胧，不透明的。
对比例2
对比例2与实施例4相比，区别在于：未添加异辛醇聚氧乙烯醚，用去离子水替代，其余与实施例4完全相同。
得到的超分子盐抑菌液实物如图3所示。
从图3可见，得到的产品也是朦胧，不透明的。
对比例3
对比例3与实施例4相比，区别在于：未添加椰油基葡糖苷，用去离子水替代，其余与实施例4完全相同。
得到的超分子盐抑菌液实物如图4所示。
从图4可见，得到的产品是朦胧，不透明的，且带有少量沉淀。
实施例5
实施例5与实施例4不同之处在于，配方如表2所示；在搅拌状态下加热至52℃，其余与实施例4完全相同。
实施例6
实施例6与实施例4不同之处在于，配方如表2所示；在搅拌状态下加热至5℃，其余与实施例6完全相同。
表2实施例4-6中超分子抑菌液配方
Figure SMS_2
对实施例4-6得到的超分子抑菌液进行抗菌和抑菌效果测试及稳定性测试，其中抗菌和抑菌效果测试按照“WS/T650-2019抗菌和抑菌效果评价方法”；稳定性测试具体方法为“GB/T38499-2020消毒剂稳定性评价方法”。得到的结果如表3所示。
表3实施例4-6得到的抑菌液的抗菌和抑菌效果及稳定性测试结果
Figure SMS_3
从表3可知，实施例4-6得到的抑菌液对大肠杆菌、金黄色葡萄球菌的抑菌率均超过97％，有非常好的抑菌效果，且稳定性高。
以上所述的实施例只是本发明的一种较佳的方案，并非对本发明作任何形式上的限制，在不超出权利要求所记载的技术方案的前提下还有其它的变体及改型。

Claims (7)

1.一种超分子盐抑菌液，其特征在于，所述超分子盐抑菌液由以下质量百分含量的组分制成：0.2-0.8%超分子盐抑菌剂，0.1-0.3%蒲公英植物提取精油，4-7%椰油酰胺两性基乙酸钠，5-8%椰油基葡糖苷，4-7%十二烷基硫酸酯铵，5-7%三乙醇胺，1-4%柠檬酸，0.3-0.6%乙二胺四乙酸四钠，2-4%烷基芳基磺酸盐，3-5%异辛醇聚氧乙烯醚，余量为去离子水；所述超分子盐抑菌剂为甜菜碱水杨酸超分子离子盐、烟酰胺壬二酸超分子离子盐或左旋肉碱酚酸超分子离子盐。
2.根据权利要求1所述的一种超分子盐抑菌液，其特征在于，所述甜菜碱水杨酸超分子离子盐通过以下方法制得：将水杨酸和食品级甜菜碱加入无水乙醇中，水杨酸和食品级甜菜碱的摩尔比为（1-1.2）：（0.8-1），搅拌均匀后升温至40-50℃反应4-8h，反应后冷却至-10℃，减压过滤，过滤物用无水乙醇洗涤后，减压干燥，即得甜菜碱水杨酸超分子离子盐。
3.根据权利要求1所述的一种超分子盐抑菌液，其特征在于，所述烟酰胺壬二酸超分子离子盐通过以下方法制得：将烟酰胺和壬二酸加入醇水混合物中，烟酰胺和壬二酸的摩尔比为（0.95-1）：（1-1.05），搅拌均匀后升温至50-60℃反应3-5h，减压过滤，过滤物减压干燥，即得烟酰胺壬二酸超分子离子盐。
4.根据权利要求3所述的一种超分子盐抑菌液，其特征在于，所述醇水混合物为异丙醇与去离子水按质量比1:1.5混合而成。
5.根据权利要求1所述的一种超分子盐抑菌液，其特征在于，所述左旋肉碱酚酸超分子离子盐通过以下方法制得：将左旋肉碱、没食子酸及水杨酸加入无水乙醇中，左旋肉碱、没食子酸及水杨酸的摩尔比为（1.9-2）：（1-1.05）：（1-1.05），搅拌均匀后升温至40-50℃反应4-6h，反应后冷却至-10℃，减压过滤，过滤物用无水乙醇洗涤后，减压干燥，即得左旋肉碱酚酸超分子离子盐。
6.一种如权利要求1所述的超分子盐抑菌液制备方法，其特征在于，所述制备方法包括以下步骤：按质量百分含量配比称取各组分后，先将椰油酰胺两性基乙酸钠、椰油基葡糖苷、十二烷基硫酸酯铵、三乙醇胺、柠檬酸、乙二胺四乙酸四钠、烷基芳基磺酸盐、异辛醇聚氧乙烯醚和去离子水混合后，在搅拌状态下加热，再加入蒲公英植物提取精油、超分子盐抑菌剂，最后搅拌至全部溶解，冷却，静置至泡沫消失，即得超分子盐抑菌液。
7.根据权利要求6所述的超分子盐抑菌液制备方法，其特征在于，所述加热温度为50-55℃。
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