CN118105324B - 一种美白抑菌牙膏及其制备方法 - Google Patents
一种美白抑菌牙膏及其制备方法 Download PDFInfo
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- CN118105324B CN118105324B CN202410244986.0A CN202410244986A CN118105324B CN 118105324 B CN118105324 B CN 118105324B CN 202410244986 A CN202410244986 A CN 202410244986A CN 118105324 B CN118105324 B CN 118105324B
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Abstract
本发明公开了一种美白抑菌牙膏及其制备方法。所述的美白抑菌牙膏由以下质量百分比计的原料制备而成：竹盐9～12％、o‑伞花烃‑5‑醇0.05～0.1％、酵素0.1～0.5％、甘草酸1～2％、磨擦型二氧化硅15～25％、增稠型二氧化硅5～10％、增稠剂0.5～1％、保湿剂15～30％、发泡剂2～3％、清凉剂0.05～0.1％、香精0.5～1％，余量为水。本发明的牙膏具有显著抑菌效果，且兼具明显牙齿美白作用，是一种天然绿色、安全性高的功能型牙膏。
Description
技术领域
本发明属于口腔清洁用品技术领域，具体涉及一种美白抑菌牙膏及其制备方法。
背景技术
由于日常生活中的烟、茶、咖啡、有色食物等易沉积于牙齿表面，逐渐使牙齿变黄或变黑，形成牙齿外源性污渍，影响牙齿的美观，还容易导致龋齿、牙龈炎等口腔问题的产生，所以广大消费者对具有美白牙齿作用的牙膏格外青睐，市场需求强烈。
竹盐是原盐经特殊加工得到的食用保健盐，以碱性著称，具有抗氧化、抗炎、杀菌、治疗胃肠道疾病、抗癌、抗肿瘤等功效。在牙膏制备领域中，竹盐也是常见的原料之一。
o-伞花烃-5-醇(O-Cymen-5-OL，IPMP)是一种广谱、低毒的杀菌剂，对细菌、真菌、酵母菌和霉菌均具有杀菌作用。研究表明，在混合非离子表面活性剂或CMC等高分子化合物的时候，有时会因包含或吸附在表面活性剂的胶粒中等原因导致其杀菌力下降。此外，强碱也有可能导致因造盐化合物引起的钝化以及功效下降。受限于o-伞花烃-5-醇上述使用条件的限制，目前未见竹盐联合o-伞花烃-5-醇在牙膏制备的相关报道。
发明内容
有鉴于此，本发明的目的在于提供一种美白抑菌牙膏，该牙膏配方克服o-伞花烃-5-醇和竹盐的配伍问题，成功制备出具有显著抑菌作用，且牙齿美白效果明显的产品。
本发明提供的美白抑菌牙膏，由以下质量百分比计的原料制备而成：竹盐9～12％、o-伞花烃-5-醇0.05～0.1％、酵素0.1～0.5％、甘草酸1～2％、磨擦型二氧化硅15～25％、增稠型二氧化硅5～10％、增稠剂0.5～1％、保湿剂15～30％、发泡剂2～3％、清凉剂0.05～0.1％、香精0.5～1％，余量为水。
优选的，所述的酵素为木瓜蛋白酶、葡糖氧化酶或乳过氧化物酶。
更优选的，所述的酵素为木瓜蛋白酶。木瓜蛋白酶是一种在酸性、中性、碱性环境下均能分解蛋白质的蛋白酶，能有效水解唾液或菌斑中的蛋白质，改善色素附着，有利于改善牙齿表面色渍。
优选的，所述的增稠剂为羧甲基纤维素钠、黄原胶、卡波姆、羟乙基纤维素中的一种或其组合。
优选的，所述的保湿剂为甘油、山梨醇、丙二醇、聚乙二醇中的一种或其组合。
优选的，所述的发泡剂为十二烷基硫酸钠、十二酰基肌氨酸钠、泊洛沙姆、椰油酰胺丙基甜菜碱中的一种或其组合。
优选的，所述的清凉剂为薄荷醇、赤藓醇、木糖醇中的一种或其组合。
优选的，所述的香精为食用香精。所述的香精有留兰香、肉桂、冬青油、茴香脑等。
优选的，所述的磨擦型二氧化硅为Zeodent105或AC77。
优选的，所述的增稠型二氧化硅为Sipernat 22S。
本发明还提供一种美白抑菌牙膏的制备方法，包括以下步骤：将甘草酸、保湿剂和水，混合，搅拌溶解，然后加入磨擦型二氧化硅、增稠型二氧化硅、增稠剂、发泡剂，真空搅拌溶解，最后加入竹盐、o-伞花烃-5-醇、酵素、清凉剂、香精，继续搅拌溶解，在真空度≥0.094MPa保持抽泡3～5min，出料，灌装。
牙膏中添加9～12％竹盐会导致牙膏体系呈强碱性，该强碱性的条件下，复配o-伞花烃-5-醇势必导致o-伞花烃-5-醇的抑菌活性明显降低。此外，牙膏中的增稠剂通常为高分子化合物，其包含作用也会影响o-伞花烃-5-醇的抑菌活性。另外，碱性环境也会加速CMC、HEC等纤维素及其钠盐的降解过程，导致牙膏的黏度迅速降低，经过长期搁置会促使牙膏分离出水，如何克服竹盐的加入引致的一系列问题，特别是竹盐对o-伞花烃-5-醇的影响，本发明人尝试挖掘适宜的稳定剂，意外发现，常作为食品甜味剂的甘草酸的加入，能克服o-伞花烃-5-醇和竹盐的配伍问题，使制得的牙膏保持显著的杀菌水平。甘草酸为天然皂苷类成分，其水溶液呈酸性，可缓冲竹盐的碱性对o-伞花烃-5-醇的冲击效果，此外，甘草酸具有两亲性结构，具有表面活性剂的性质，对微粒具有较强的亲和力，一部分吸附于微粒表面，另一部分通过分子间作用力相互缠绕，在纳米粒子间形成三维网状结构，这种网状结构可以阻止微粒的聚集，促进包含o-伞花烃-5-醇的粒子在牙膏体系中分散。推断，甘草酸的稳定作用与其发挥的酸碱中和特性、空间稳定特性有关。事实上，本发明也证明，并非任意的酸性物质的加入，均能发挥如甘草酸那般的稳定作用，如柠檬酸的稳定效果并不那么显著。
本发明配方中添加适量的磨擦型二氧化硅作为磨擦剂，在牙刷的压力下剪切破碎牙垢和磨除牙结石，再被表面活性剂乳化呈悬浮液，降低黏性，包括牙菌斑一起离开牙齿表面。通过高清洁性磨擦剂的物理作用，结合木瓜蛋白酶的化学分解作用，达到美白健齿效果。
本发明具有以下有益效果：
本发明提供了一种具有显著抑菌效果，且兼具明显牙齿美白作用的牙膏，该牙膏不含过氧化物类的美白剂，对牙齿刺激性少，也不含西吡氯铵、氯己定等化学杀菌剂，安全性高，牙膏中的竹盐、o-伞花烃-5-醇、酵素、甘草酸均是天然低毒成分，因此，本发明的牙膏是一种天然绿色、安全性高、具有显著美白抑菌效果的功能型牙膏。
具体实施方式
以下实施例是对本发明的进一步说明，而不是对本发明的限制。下述实施例中配方的组分，若无特别说明，均为常规市售产品。
实施例1
一种美白抑菌牙膏，由以下质量百分比计的原料制备而成：竹盐10％、o-伞花烃-5-醇0.1％、木瓜蛋白酶0.5％、甘草酸1.5％、磨擦型二氧化硅20％、增稠型二氧化硅8％、羧甲基纤维素钠0.6％、甘油5％、山梨醇15％、十二烷基硫酸钠3％、薄荷醇0.05％、留兰香香精0.5％，余量为水。
制备步骤：将甘草酸、甘油、山梨醇和水，混合，搅拌溶解，然后加入磨擦型二氧化硅、增稠型二氧化硅、羧甲基纤维素钠、十二烷基硫酸钠，真空搅拌溶解，最后加入竹盐、o-伞花烃-5-醇、木瓜蛋白酶、薄荷醇、留兰香香精，继续搅拌溶解，在真空度≥0.094MPa保持抽泡5min，出料，灌装。
实施例2
一种美白抑菌牙膏，由以下质量百分比计的原料制备而成：竹盐9％、o-伞花烃-5-醇0.08％、木瓜蛋白酶0.4％、甘草酸1％、磨擦型二氧化硅25％、增稠型二氧化硅5％、羧甲基纤维素钠1％、甘油5％、山梨醇10％、十二烷基硫酸钠2％、薄荷醇0.05％、留兰香香精0.5％，余量为水。
制备步骤：将甘草酸、甘油、山梨醇和水，混合，搅拌溶解，然后加入磨擦型二氧化硅、增稠型二氧化硅、羧甲基纤维素钠、十二烷基硫酸钠，真空搅拌溶解，最后加入竹盐、o-伞花烃-5-醇、木瓜蛋白酶、薄荷醇、留兰香香精，继续搅拌溶解，在真空度≥0.094MPa保持抽泡5min，出料，灌装。
实施例3
一种美白抑菌牙膏，由以下质量百分比计的原料制备而成：竹盐12％、o-伞花烃-5-醇0.05％、木瓜蛋白酶0.2％、甘草酸2％、磨擦型二氧化硅20％、增稠型二氧化硅10％、羧甲基纤维素钠0.5％、甘油5％、山梨醇15％、十二烷基硫酸钠3％、薄荷醇0.05％、留兰香香精0.5％，余量为水。
制备步骤：将甘草酸、甘油、山梨醇和水，混合，搅拌溶解，然后加入磨擦型二氧化硅、增稠型二氧化硅、羧甲基纤维素钠、十二烷基硫酸钠，真空搅拌溶解，最后加入竹盐、o-伞花烃-5-醇、木瓜蛋白酶、薄荷醇、留兰香香精，继续搅拌溶解，在真空度≥0.094MPa保持抽泡5min，出料，灌装。
实施例4
一种美白抑菌牙膏，由以下质量百分比计的原料制备而成：竹盐10％、o-伞花烃-5-醇0.07％、木瓜蛋白酶0.1％、甘草酸1.5％、磨擦型二氧化硅15％、增稠型二氧化硅7％、羟乙基纤维素0.6％、甘油10％、山梨醇20％、十二酰基肌氨酸钠2％、木糖醇0.1％、留兰香香精1％，余量为水。
制备步骤：将甘草酸、甘油、山梨醇和水，混合，搅拌溶解，然后加入磨擦型二氧化硅、增稠型二氧化硅、羟乙基纤维素、十二酰基肌氨酸钠，真空搅拌溶解，最后加入竹盐、o-伞花烃-5-醇、木瓜蛋白酶、木糖醇、留兰香香精，继续搅拌溶解，在真空度≥0.094MPa保持抽泡3min，出料，灌装。
对比例1-4
对比例1-4的美白抑菌牙膏，由以下质量百分比计的原料制备而成：
上述对比例1-4的美白抑菌牙膏的制备步骤参考实施例1。
实施例5毒理评价
1、急性经口毒性试验
依据卫生部颁发的《化妆品卫生规范》2007年版中的急性经口毒性试验方法，用KM小白鼠试验，连续观察14天，结果显示，实施例1-4制得的美白抑菌牙膏均满足LD50＞40g/kg的要求，表明本发明提供的美白抑菌牙膏安全性高。
2、口腔黏膜刺激试验
依据YY/T0127.3-2009，口腔医疗器械生物学评价，第二单元试验方法，口腔粘膜刺激试验要求，结果显示，实施例1-4制得的美白抑菌牙膏的刺激指数均为0，对口腔粘膜比较安全。
实施例6抑菌效果评价
按照QB/T2738-2012《日化产品抗菌抑菌效果的评价方法》中的抑菌型日化产品的抑菌效果检验方法(悬液定量法)，测试实施例1-4和对比例1-4制得的美白抑菌牙膏对变异链球菌(ATCC35668)、牙龈卟啉单胞菌(ATCC33277)、白色念珠菌(ATCC10231)的抑菌率，重复3次实验，取平均值，结果见表1。
表1抑菌效果检测结果
结果显示，实施例1-4制得的美白抑菌牙膏对变异链球菌、牙龈卟啉单胞菌、白色念珠菌等常见的口腔病原菌均具有良好的抑菌效果，抑菌率均达到94％以上，效果优于对比例1-4的制得牙膏。
实施例7美白效果评价
取50块经酸蚀处理的牛牙釉质块放入37℃染色液浸泡一周(染色液为红茶、胃粘蛋白、氯化铁和水的混合液)，取出后用烟草烟熏处理30min，得到染色的牛牙釉质块。然后固定于L8-II十字刷牙机上，随机分成5组，每组10块，分别采用实施例1-4制得的牙膏、以及某市售酵素小苏打美白牙膏进行模拟刷牙8000次，清洗晾干。采用色差仪测定刷牙前后牙釉质的色彩，刷牙前记为L0，刷牙后记为L1。增白率％＝(L1-L0)/L0×100％，取平均值，结果见表2。
表2牙齿美白效果检测结果
结果显示，实施例1-4制得的美白抑菌牙膏具有明显的牙齿美白效果，对牙齿的增白效果与某市售酵素小苏打美白牙膏相当。
实施例8稳定性评价
将实施例1-4、对比例3-4制得的美白抑菌牙膏在室温下放置24个月，分别在放置3、6、12、18、24个月时观察膏体的变化，结果见表3。
表3牙膏稳定性考察结果
结果显示，实施例1-4制得的美白抑菌牙膏具有较佳的稳定性，在室温下放置24个月膏体没有出现分水现象。对比例3的牙膏不含甘草酸，在室温下放置6个月，膏体出现分水，放置12个月，膏体严重分水，表明在不含甘草酸的情况，竹盐的碱性会加速CMC-Na的降解，促进牙膏分离出水。对比例4的牙膏以柠檬酸取代甘草酸，在室温下放置18个月，膏体出现分水，放置24个月，膏体严重分水，表明柠檬酸的稳定作用要差于甘草酸，若以柠檬酸作为稳定剂，制得牙膏并不能满足牙膏2～3年的保质期要求。
以上仅是本发明的优选实施方式，应当指出的是，上述优选实施方式不应视为对本发明的限制，本发明的保护范围应当以权利要求所限定的范围为准。对于本技术领域的普通技术人员来说，在不脱离本发明的精神和范围内，还可以做出若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。
Claims (9)
1.一种美白抑菌牙膏，其特征在于，由以下质量百分比计的原料制备而成：竹盐9～12％、o-伞花烃-5-醇0.05～0.1％、酵素0.1～0.5％、甘草酸1～2％、磨擦型二氧化硅15～25％、增稠型二氧化硅5～10％、增稠剂0.5～1％、保湿剂15～30％、发泡剂2～3％、清凉剂0.05～0.1％、香精0.5～1％，余量为水。
2.根据权利要求1所述的美白抑菌牙膏，其特征在于，所述的酵素为木瓜蛋白酶、葡糖氧化酶或乳过氧化物酶。
3.根据权利要求2所述的美白抑菌牙膏，其特征在于，所述的酵素为木瓜蛋白酶。
4.根据权利要求1所述的美白抑菌牙膏，其特征在于，所述的增稠剂为羧甲基纤维素钠、黄原胶、卡波姆、羟乙基纤维素中的一种或其组合。
5.根据权利要求1所述的美白抑菌牙膏，其特征在于，所述的保湿剂为甘油、山梨醇、丙二醇、聚乙二醇中的一种或其组合。
6.根据权利要求1所述的美白抑菌牙膏，其特征在于，所述的发泡剂为十二烷基硫酸钠、十二酰基肌氨酸钠、泊洛沙姆、椰油酰胺丙基甜菜碱中的一种或其组合。
7.根据权利要求1所述的美白抑菌牙膏，其特征在于，所述的清凉剂为薄荷醇、赤藓醇、木糖醇中的一种或其组合。
8.根据权利要求1所述的美白抑菌牙膏，其特征在于，所述的香精为食用香精。
9.一种权利要求1-8任一项所述的美白抑菌牙膏的制备方法，其特征在于，包括以下步骤：
将甘草酸、保湿剂和水，混合，搅拌溶解，然后加入磨擦型二氧化硅、增稠型二氧化硅、增稠剂、发泡剂，真空搅拌溶解，最后加入竹盐、o-伞花烃-5-醇、酵素、清凉剂、香精，继续搅拌溶解，在真空度≥0.094MPa保持抽泡3～5min，出料，灌装。
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