CN114917169B - 一种含富锌糙米发酵液的牙膏及其制备方法 - Google Patents
一种含富锌糙米发酵液的牙膏及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种含富锌糙米淘米水发酵液的牙膏,该含富锌糙米发酵液的牙膏包括质量份数如下的成分:富锌糙米发酵液1‑2份、改性TiO24‑8份、TiO24‑8份、SiO220‑30份、山梨醇25‑35份、甘油15‑25份、助剂和水;其中,所述改性TiO2为表面接枝花生四烯酸酯的TiO2;所述改性TiO2和TiO2,均经过NaOH表面预处理。本发明还涉及有关该含富锌糙米发酵液的牙膏的制备方法,包括富锌糙米发酵液的制备方法和改性TiO2的制备方法。本发明实现了高效口腔清洁和牙齿美白的技术效果,有效改善了口腔卫生环境,具有良好的应用前景。
Description
技术领域
本发明属于口腔清洁用品技术领域,具体涉及一种含富锌糙米发酵液的牙膏及其制备方法。
背景技术
牙膏是日常生活中必不可少的清洁用品,其具有维持并改善口腔卫生的作用,并且还能美白牙齿、去除菌斑,对维持个人形象发挥着重要作用。
牙菌斑是一种细菌性生物膜,是口腔内包裹基质表面、或粘附牙面、牙齿间或修复体表面的软而未矿化的细菌性群体,仅通过水洗很难将其去除。牙菌斑含有三个阶段的生长,即牙面获得性薄膜的形成、细菌的黏附和共聚、细菌大量繁殖产生牙菌斑。在口腔护理领域中,Hanke在上世纪40年代首先发现含锌化合物具有抗牙菌斑的作用,能帮助防龋。随后,柠檬酸锌等化合物开始被加入牙膏中,以实现清洁牙菌斑、缓解牙龈出血、以及抗牙结石等功能。按美国食品药品监督管理局对控制牙菌斑和缓解牙龈炎功效成分的分类,柠檬酸锌安全等级为I,功效等级为Ⅲ,是牙膏中一种安全有效的功效成分。但当前的柠檬酸锌牙膏对牙齿美白、减小刺激性以及活性物质利用率方面还存在不足。
近年来,富锌糙米因其较高的锌元素含量和丰富的营养价值受到市场的关注,是一种天然、绿色、零危害的理想锌元素来源。而作为富锌糙米副产品的淘米水中也含有蛋白质、脂肪、维生素、锌等营养成分,大量淘米水被直接倒掉不仅浪费了水资源,还损失了众多营养物质。此外,淘米水通过微生物发酵后,得到进一步富集的锌元素具有更好的生物相容性以及活性,能被人体更高效的吸收、利用,实现了变废为宝的转换,具有良好的经济价值。然而,目前尚未出现将富锌糙米衍生产物应用于改善牙膏性能的功能性产品。
综上,本发明的目的在于开发一种含有富锌糙米淘米水发酵液成分的牙膏,以实现高效口腔清洁、牙齿美白的技术效果。
发明内容
为解决上述现有技术问题,本发明开发了一种含富锌糙米淘米水发酵液的牙膏,其实现了高效清洁牙菌斑和牙齿美白的技术效果,有效改善了口腔卫生环境,具有良好的应用前景。
本发明的一个目的在于,提供一种含富锌糙米发酵液的牙膏,所述含富锌糙米发酵液的牙膏包括质量份数如下的成分:
助剂
水;
其中,
所述改性TiO2为表面接枝花生四烯酸酯的TiO2;
所述改性TiO2和TiO2,均经过NaOH表面预处理。
进一步地,所述助剂选自CAPB、CMC、卡拉胶、木糖醇、烷基糖苷和香精中的一种或多种。
进一步地,所述水的质量份数为10-20份。
进一步地,所述SiO2的粒度为300-400目。
本发明的另一个目的在于,提供上述含富锌糙米发酵液的牙膏的制备方法,所述含富锌糙米发酵液的牙膏的制备方法包括如下步骤:
(1)富锌糙米发酵液的制备方法:
S1.将富锌糙米加入水中,搅拌后,过滤,将所得滤液灭菌,得到发酵基质;
S2.将乳酸菌菌液接种至所述发酵基质中,发酵培养后,将所得发酵液灭菌,得到所述富锌糙米发酵液;
(2)改性TiO2的制备方法:
L1.将TiO2焙烧后,浸泡于NaOH溶液中,超声、洗涤、干燥、研磨后,得到预处理后的TiO2;
L2.将部分所述预处理后的TiO2加入花生四烯酸溶液中,超声反应后,离心、洗涤、干燥,得到所述改性TiO2。
TiO2经过预处理后,有效除去了TiO2的有机修饰,并清洗干净了表层铝/硅的惰性包膜,促进其表面羟基化,提高了TiO2与花生四烯酸的反应效率。
进一步地,步骤S2中,所述乳酸菌选自嗜热链球菌、保加利亚乳杆菌、嗜酸乳杆菌和乳双歧杆菌中的一种或多种。
进一步地,步骤S2中,所述发酵培养的时间为36-72h。
进一步地,步骤L1中,所述焙烧的温度为500-550℃,时间为0.5-1h。
进一步地,步骤L2中,所述花生四烯酸与所述预处理后的TiO2的摩尔比为(2-5):1。
进一步地,步骤L2中,所述超声反应的时间为6-8h。
本发明具有以下有益效果:
1.本发明中含有表面高活性的羟基与花生四烯酸中的羧基通过酯化反应相连形成的改性TiO2,其表面被花生四烯酸修饰后,其亲油性大大增强,能够稳定均匀分散于牙膏中,并且其比表面积大大增加,通过填充在SiO2颗粒之间增强了产品的摩擦和吸附性能,提高了对牙菌斑的去除效果;
2.本发明中同时还含有未接枝花生四烯酸酯的、仅经过NaOH表面预处理的TiO2,其表面含有大量的羟基,能在TiO2相互之间,或者与SiO2成分的表面羟基之间产生氢键,形成网状结构,由此二者能够发挥协同作用,显著提升研磨性能,同时促进发酵液中的活性成分均匀分布,进一步增强产品清洁牙齿、护理口腔的效果;
3.本发明中的富锌糙米发酵液中含有大量锌元素,其具有较高活性,生物相容性好,能够抑制细菌生长、阻止沉积物形成,达到了减少牙菌斑、牙齿美白的效果;并且富锌糙米发酵液的原料为淘米水,有效节约了资源,实现绿色、可持续生产。
具体实施方式
为了更清楚地说明本发明的技术方案,列举如下实施例。实施例中所出现的原料、反应和后处理手段,除非特别声明,均为市面上常见原料,以及本领域技术人员所熟知的技术手段。
本发明实施例中的富锌糙米购买自当地市场。
本发明实施例中的SiO2粒度为300目。
本发明实施例中的TiO2牌号为:杜邦R706,原级尺寸100-300nm,金红石型。
本发明实施例中富锌糙米发酵液的制备方法为:
S1.将100g富锌糙米加入500mL水中,搅拌30min后,过滤,将所得滤液120℃灭菌20min,得到发酵基质;
S2.将保加利亚乳杆菌CICC 20271斜面培养活化后,接种于MRS液体培养基中培养24h,离心、重悬,得到菌液;
将所述菌液接种至所述发酵基质中,发酵培养48h后,将所得发酵液120℃灭菌20min,得到所述富锌糙米发酵液。
本发明实施例中改性TiO2的制备方法为:
L1.将TiO2在500℃下焙烧0.5h后,浸泡于2mol/L的NaOH溶液中,超声处理1h后,洗涤至洗液呈中性,干燥后研磨得到预处理后的TiO2;
L2.将0.1mol所述预处理后的TiO2加入0.3mol花生四烯酸中,80℃超声反应8h后,离心、洗涤、干燥,得到所述改性TiO2。
本发明实施例中的TiO2为经上述步骤L1预处理后的TiO2。
实施例1-3中含富锌糙米发酵液的牙膏的各个成分和相应质量份数,如表1所示。
表1实施例1-3含富锌糙米发酵液的牙膏中各成分及其质量份数
实施例1-3的含富锌糙米发酵液的牙膏的制备方法均为:按上述质量份数,将水、甘油、山梨醇、木糖醇、TiO2、改性TiO2和SiO2加入容器中搅拌,均质后,将混合液加入制膏锅中,然后将富锌糙米发酵液、CAPB、CMC、卡拉胶、烷基糖苷和香精加入制膏锅中,抽至真空后,搅拌研磨5min,然后在常温常压下陈化2h,得到所述含富锌糙米发酵液的牙膏。
基于实施例1,设置其对比例。对比例的成分如表2所示。
表2实施例1、对比例1-2的含富锌糙米发酵液的牙膏中各成分及其质量份数
对比例1-2的制备方法与实施例1的区别在于:将富锌糙米发酵液和改性TiO2组分对应地进行替换,其他步骤与实施例1相同。
测试例1
牙菌斑去除能力测试
测试方法:随机选取60名志愿者,将其分为3组,每组20人,分别使用本发明实施例1、对比例1、对比例2制备的牙膏产品,每日早晚各进行一次刷牙,每次使用牙膏2g,持续30天,测定每组人员在测试前后的菌斑指数(PLI)平均值,根据PLI数值差异分析牙膏的牙菌斑去除能力。
PLI检测方法:用探针轻划牙面,根据菌斑的量和厚度记分。每颗牙检查4个牙面,即近中颊面、正中颊面、远中颊面以及舌面。每颗牙的记分为4个牙面记分之和除以4,个人记分为每颗牙记分之和除以受检牙数。(评分标准:0=龈缘区无菌斑;1=龈缘区的牙面有薄的菌斑,但视诊不可见,若用探针尖刮牙面可见牙菌斑;2=在龈缘或邻面可见中等量菌斑;3=龈沟内或龈缘区及邻面有大量软垢。)
测试结果如表3所示:
表3牙菌斑去除能力测试结果
根据表3可以得出,本发明的含富锌糙米发酵液的牙膏具有良好的牙菌斑去除能力,在一个月的测试中PLI降低率可达70%以上,而使用传统添加剂柠檬酸锌和未改性TiO2的对比例2和对比例3,因其摩擦能力、生物相容性相对较差,因此对牙菌斑的去除能力低于实施例1。
测试例2
牙齿美白能力测试
测试方法:采用文献“黄秀娟,李毅苹.一种复合型系统美白牙膏的开发研究[J].口腔护理用品工业,2019,29(2):15-18.”中3.2中的测试方法对实施例1和对比例1-2的美白能力进行评价。
测试结果如表4所示:
表4牙齿美白能力测试结果
组别 | L*刷牙前 | L*刷牙后 | ΔL* |
实施例1 | 41.62 | 55.49 | 13.87 |
对比例1 | 42.87 | 53.60 | 10.73 |
对比例2 | 41.38 | 51.97 | 10.59 |
根据表4可以得出,本发明实施例1制备的含富锌糙米发酵液的牙膏具有较强牙齿美白能力,其有效去除了牙釉质外源性色斑,美白效果比使用普通柠檬酸锌和未改性TiO2的对比例更为显著,具有良好的应用前景。
对于本领域技术人员而言,显然本发明不限于上述示范性实施例的细节,而且在不背离本发明的精神或基本特征的情况下,能够以其他的具体形式实现本发明。因此,无论从哪一点来看,均应将实施例看作是示范性的,而且是非限制性的,本发明的范围由所附权利要求而不是上述说明限定,因此旨在将落在权利要求的等同要件的含义和范围内的所有变化囊括在本发明内。
此外,应当理解,虽然本说明书按照实施方式加以描述,但并非每个实施方式仅包含一个独立的技术方案,说明书的这种叙述方式仅仅是为清楚起见,本领域技术人员应当将说明书作为一个整体,各实施例中的技术方案也可以经适当组合,形成本领域技术人员可以理解的其他实施方式。
Claims (6)
1.一种含富锌糙米发酵液的牙膏,其特征在于,所述含富锌糙米发酵液的牙膏由质量份数如下的成分构成:
富锌糙米发酵液 1份
改性TiO2 5份
TiO2 6份
SiO2 22份
山梨醇 35份
甘油 15份
椰油酰胺丙基甜菜碱 2份
羧甲基纤维素 1.5份
卡拉胶 0.4份
木糖醇 1份
烷基糖苷 2份
香精 1份
水 15份;
其中,
所述改性TiO2为表面接枝花生四烯酸酯的TiO2;
所述改性TiO2和TiO2,均经过NaOH表面预处理;
所述含富锌糙米发酵液的牙膏的制备方法包括如下步骤:
(1)富锌糙米发酵液的制备方法:
S1. 将富锌糙米加入水中,搅拌后,过滤,将所得滤液灭菌,得到发酵基质;
S2. 将乳酸菌菌液接种至所述发酵基质中,发酵培养后,将所得发酵液灭菌,得到所述富锌糙米发酵液;
(2)改性TiO2的制备方法:
L1. 将TiO2焙烧后,浸泡于NaOH溶液中,超声、洗涤、干燥、研磨后,得到预处理后的TiO2;
L2. 将部分所述预处理后的TiO2加入花生四烯酸溶液中,超声反应后,离心、洗涤、干燥,得到所述改性TiO2;
步骤S2中,所述发酵培养的时间为36-72 h。
2.根据权利要求1所述含富锌糙米发酵液的牙膏,其特征在于,所述SiO2的粒度为300-400目。
3.根据权利要求1所述含富锌糙米发酵液的牙膏,其特征在于,步骤S2中,所述乳酸菌选自嗜热链球菌、保加利亚乳杆菌、嗜酸乳杆菌和乳双歧杆菌中的一种或多种。
4.根据权利要求1所述含富锌糙米发酵液的牙膏,其特征在于,步骤L1中,所述焙烧的温度为500-550℃,时间为0.5-1 h。
5.根据权利要求1所述含富锌糙米发酵液的牙膏,其特征在于,步骤L2中,所述花生四烯酸与所述预处理后的TiO2的摩尔比为(2-5):1。
6.根据权利要求1所述含富锌糙米发酵液的牙膏,其特征在于,步骤L2中,所述超声反应的时间为6-8 h。
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