CN112691057B - 一种复方功效型牙膏及其制备方法 - Google Patents
一种复方功效型牙膏及其制备方法 Download PDFInfo
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- CN112691057B CN112691057B CN202011533563.9A CN202011533563A CN112691057B CN 112691057 B CN112691057 B CN 112691057B CN 202011533563 A CN202011533563 A CN 202011533563A CN 112691057 B CN112691057 B CN 112691057B
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Abstract
本发明公开一种复方功效型牙膏及其制备方法，该复方功效型牙膏包括复合摩擦剂、山梨醇液、甘油、羧甲基纤维素钠、黄原胶、苯甲酸钠、焦磷酸钠、植酸钠、十二烷基硫酸钠、功效物质、木糖醇、糖精钠、香精等多种成分。本发明优选复合摩擦剂、保湿剂、胶着剂等成分及合理配比用量，得到的牙膏膏基光洁细腻、均匀稳定，易于分散。本发明还进一步经多次试验筛选得到优质的功效物质成分组合，通过功效成分之间的配伍协同，可有效提高牙膏抑菌性能与修复口疮创面愈合的性能，从而达到改善口腔问题，抑制常见口腔细菌，缓解口腔溃疡，清新口气的效果。
Description
技术领域
本发明涉及日用品技术领域，具体涉及一种复方功效型牙膏及其制备方法。
背景技术
随着经济水平的提高，人们生活方式和饮食结构的改变，蛋糕、饼干等精加工含糖食品及含糖饮料的摄入量增加，我国居民口腔健康现状堪忧，第三次“全国口腔健康流行病学调查”数据显示，约八成人面临牙病的侵扰；2018年09月20日全国爱牙日宣传材料显示，我国能达卫生组织制定的口腔健康标准人群只有0.22％。中国有句俗语：“牙不好，疾病满身跑”，口腔是食物进入人体的首个通道，细菌是引起口腔疾病的主要因素。面对我国口腔健康现状，如何防治口腔疾病，亟须引起重视。
牙膏是人们清洁口腔必备的生活用品，也是口腔疾病防治的第一道关卡，如何在第一道关卡上起到防治的作用，是牙膏研发的核心。随着牙膏市场进入产品细分时代，产品功能化是市场发展的趋势，中草药因含多种有效成分、具有多方位的综合效用、抗菌谱广等特点与优势越来越受消费者青睐，除此之外，本土企业都在推崇产品创新，而中草药牙膏无疑被视作国产品牌打破外资垄断和重新划分格局的重要武器。随着中药现代化技术的发展，利用天然、健康、接受度高的中药活性成分来辅助预防口腔疾病成为了口腔保健护理制品的重要发展方向，然而添加何种中草药、如何添加不影响膏体整体感官评价，达到怎样的效果是本领域在研究复方功效牙膏时的首要考虑因素。
发明内容
鉴于现有技术的不足，本发明的目的在于提供一种具防治口腔疾病的复方功效型牙膏，申请人在改进草果油与艾纳香油提取时，发现使用酶解技术辅助水蒸汽蒸馏法可提高得油率。本发明牙膏通过草果油、艾纳香油与薄荷脑三重促渗透作用，促进中草药功效因子在口腔中的透皮吸收，增强复方药物的抗菌消炎、修复粘膜功能/治疗口腔溃疡的功能，再配以叶绿素铜钠与尿囊素进一步增强抗菌消炎、修复口腔溃疡、除臭功效，最后佐以薄荷与清新柚果香精不仅掩盖中草药不良气味，还能清新口气，口留清爽果香。
本发明方案包括以下方面：
一种复方功效型牙膏，按重量百分比计，包括以下成分：
优选的，所述香精包括柚果香精和薄荷脑；所述山梨醇液的浓度为70wt％；所述复合摩擦剂为磷酸氢钙和二氧化硅；
优选的，所述中草药提取物包括草果油、艾纳香油、凉粉草提取物、鼠尾草提取物和丹皮酚的至少一种。
优选的，所述复方功效型牙膏按重量百分比计，包括以下成分：
优选的，所述复方功效型牙膏，按重量百分比计，包括以下成分：
优选的，所述复方功效型牙膏中的草果油与艾纳香油通过以下步骤制得：
取阴干后的艾纳香枝叶与草果果实，粉碎过筛得粉末，加入蒸馏水、果胶酶、木聚糖酶，调pH，酶解，灭酶，再进行水蒸汽蒸馏提取，得挥发油。
更优选的，草果油与艾纳香油通过以下步骤制得：
S1：取阴干后的艾纳香枝叶与草果果实，粉碎过筛得粉末，加入粉末10倍质量的蒸馏水，加入果胶酶1000U/g粉末以及木聚糖酶2000U/g粉末，调pH至5.5，50℃下酶解2小时，灭酶，再进行水蒸汽蒸馏提取，提取3次，提取时间分别为4小时、3小时、2小时，三次所得的挥发油合并备用。
另一方面，本发明还提供了所述的复方功效型牙膏的制备方法，包括以下步骤：
S1：所有粉末或固体状原料研磨，过筛，备用；
S2：制胶：称取山梨醇和甘油，混合均匀，加入羧甲基纤维素钠和水，搅拌至均匀无透明颗粒，待羧甲基纤维素钠完全溶胀，再加入已用冷水分散均匀的黄原胶，充分搅拌均匀后，在温度70～75℃、转速700～1000rpm条件下搅拌，得胶液；同时将苯甲酸钠、焦磷酸钠、植酸钠与水混合并加热，充分搅拌至完全溶解后，加至胶液中搅拌均匀，静置，待胶液充分溶胀，备用；
S3：制膏：将水加入溶胀后的胶液中，加热至65～70℃时，先加入十二烷基硫酸钠，搅拌均匀；再加入复合摩擦剂，搅拌，得牙膏膏基；
S4：待牙膏膏基温度降至42～45℃，依次加入功效物质、木糖醇、糖精钠与香精，充分搅拌，真空脱气后静置，即得复方功效型牙膏。
优选的，步骤S3，将水加入溶胀后的胶液中，加热至65～70℃时，先加入十二烷基硫酸钠，搅拌均匀；再依次加入复合摩擦剂，搅拌混合后，再1000～1200rpm转速下充分搅拌20min，转速调至500～700rpm再搅拌30min，得牙膏膏基。
优选的，步骤S4，待牙膏膏基温度降至45℃，依次加入功效物质、木糖醇、糖精钠与香精，在转速500rpm条件下充分搅拌30min，真空脱气后静置至少24h，即得复方功效型牙膏。
本发明所取得的有益效果：
(1)本发明采用的复合摩擦剂、保湿剂、胶着剂的配比用量，在多次预实验的基础上，以膏基成形情况、膏体形态、渗水现象，有无过硬颗粒等为感官评价，采用L9(3^4)正交试验筛选牙膏膏基最优配比，得到牙膏膏基光洁细腻、均匀稳定，易于分散。
(2)本发明采用的功效物质基于每种功效成分的生理活性探究，通过多次预实验复配而得。
(3)本发明采用的牙膏香型是经过多种香精的筛选，意外发现薄荷脑香搭配清新柚果香精不仅可以掩盖药效物质的不良气味，还能使牙膏达到清新口气，清爽留香的效果。
(4)本发明公开的复方功效型牙膏，具有抑菌消炎，缓解口腔溃疡，除臭的作用，清新口气，清爽留香，达到防治口腔疾病的效果。
附图说明
图1：牙膏实物图，图中A代表空白牙膏(白色膏体)，图中B代表样品牙膏(绿色膏体)。
具体实施方式
为了更好理解本发明技术内容，下面提供具体实施例，对本发明做进一步的说明。
草果果实购自安徽亳州批发市场，经鉴定为姜科豆蔻属植物草果的成熟果实；
艾纳香枝叶采自中国热带农业科学院热带作物品种资源研究所艾纳香种质资源圃；
凉粉草提取物与尾草提取物通过网上店铺直接购买，质量要求为醇提(20:1)
果胶酶：食品级，迈德丰生物科技有限公司，100000U/g；
木聚糖酶：食品级，信得利生物科技有限责任公司，40000U/g；
其他牙膏辅料按质量要求均通过网上店铺购买。
实施例1牙膏功效物质的提取
方法1：分别取阴干后的艾纳香枝叶与成熟干草果果实，用粉碎机粉碎至40目后，加入粉末10倍质量的蒸馏水；分别加入果胶酶1000U/g粉末和木聚糖酶2000U/g粉末，调pH至5.5，50℃下酶解2小时，加热至100℃灭活酶10分钟，再进行水蒸汽蒸馏提取，提取3次，提取时间分别为4小时，3小时，2小时，三次所得的挥发油合并即得艾纳香挥发油1与草果挥发油1，重复三次，计算挥发油得率(挥发油得率＝挥发油质量/原料质量×100％)，取平均值。
方法2：分别取阴干后的艾纳香枝叶与成熟干草果果实，用粉碎机粉碎至40目后，加入粉末10倍质量的蒸馏水浸泡2小时，进行水蒸汽蒸馏提取，提取3次，提取时间分别为4小时，3小时，2小时，三次所得的挥发油合并即得艾纳香挥发油2与草果挥发油2，重复三次，计算挥发油得率，取平均值。结果表见1，结果表明酶解技术辅助水蒸汽蒸馏法可以提高挥发油收得率。
表1不同提取方法挥发油收得率
| 原料 | 挥发油收得率1(方法1) | 挥发油收得率(方法2) |
| 草果挥发油 | 3.42％ | 2.31％ |
| 艾纳香挥发油 | 0.04％ | 0.015％ |
实施例2复方功效型牙膏的制备工艺研究
2.1牙膏基础配方优选工艺
2.1.1牙膏基础配方成分的选择
摩擦剂是牙膏的主要成分，摩擦剂的选择既不能损伤牙面及牙周组织，又要有一定的摩擦作用。磷酸氢钙性能稳定，是一种洁齿力温和、不伤牙齿的磨料，不但与牙釉质的组成元素相似，能对病损牙产生良好的再矿化修复作用，还能改善膏体的分水现象，制成膏体光洁细腻；二氧化硅性质稳定，不与牙膏其他成分发生反应，具有良好的触变性和耐磨度，在美白牙齿的同时，将牙齿磨损程度降到最低。
采用对膏体稳定性好的复合摩擦剂优于单一摩擦剂，根据摩擦剂的特点，选用磨擦力适中，稳定性较好的磷酸氢钙与二氧化硅复合摩擦剂；保湿剂以山梨醇为代表，吸湿性较甘油差，但保湿性能良好，口感甚佳。二元醇类的保湿剂如丙二醇、二甘醇、和聚乙二醇的各种性能比较接近，但口感不如甘油，而且甘油还具有抗菌性能、适口的甜味和稳定牙膏粘度的作用。因此采用无色透明的山梨醇复配甘油作为保湿剂，增加膏体的稳定性，牙膏中使用的是70％浓度的液体山梨醇。增稠剂采用常用的羧甲基纤维素钠，与黄原胶复配，进一步增强抗盐、抗酶性能，并使膏体更加细腻、光亮；十二烷基硫酸钠在牙膏体系中具有去污、乳化和优异的发泡力。由于发泡剂在搅拌过程中会产生气泡，会影响膏基感官评价，因此不在膏基处进行筛选，具体膏基配方见表2。
表2牙膏基础配方
| 原料名称 | 质量要求 |
| 磷酸氢钙 | 食品级 |
| 二氧化硅 | 食品级 |
| 70％山梨醇液 | 食品级，≥70％ |
| 甘油 | 纯度:99.9％ |
| CMC-Na | 食品级，耐酸高粘 |
| 黄原胶 | 食品级 |
| 苯甲酸钠 | 食品级 |
| 焦磷酸钠 | 食品级 |
| 植酸钠 | 食品级 |
| 去离子水 |
膏基配方特点：保湿剂多，水量较少，由于主摩擦剂磷酸氢钙通常以二水合物(CaHPO4·2H2O)的形式存在，在空气中稳定，在水溶液或加热时易水解生成磷灰石和磷酸，使牙膏稠度增大，甚至硬化，为了减缓这些影响，增大保湿剂中甘油的量并添加焦磷酸钠作为稳定剂，防止磷酸氢钙脱水，通过预实验发现，焦磷酸钠用量以0.5％～1％为宜，不宜超过1％，因为用量多膏体增稠，用量少膏体偏软；同时添加植酸钠可以起到螯合钙离子的作用。此外，甘油用量若大些，吸水量会增大，CMC-Na用量就要相应少；
膏基制备工艺：S1：所有粉末或固体状原料，先研磨成极细粉末，再过150目筛，备用；S2：制胶：黄原胶先用一定量的冷水分散均匀备用；按比例称取保湿剂，混合均匀，加入CMC-Na和少量水，搅拌至均匀无透明颗粒，待CMC-Na完全溶胀，再加入预分散好的黄原胶，充分搅拌均匀后，在温度70～75℃、转速700-1000rpm条件下，搅拌约30min，制胶完成，搅拌过程中注意防止水分蒸发；同时按比例称取苯甲酸钠、焦磷酸钠、植酸钠放入烧杯中，加入一定比例的水进行加热，充分搅拌至完全溶解后，加至胶液中搅拌均匀，结束后，静止放置12h左右，待胶液充分溶胀，备用。S3：制膏基：将剩余的去离子水加入溶胀后的胶液中，加热至70℃时，依次加入二氧化硅与磷酸氢钙，手动搅拌与胶液基本混合后，保持温度先1000rpm转速下充分搅拌30min后，转速调至500～700rpm再搅拌30min，使充分搅拌均匀，陈化24h，即得牙膏膏基。
2.1.2膏基配方用量的确定
感官评价：感官指标是评价牙膏膏质最为直观的指标，根据牙膏新国家标准对膏体的要求，本实验采用5级100分评分法进行感官评价，评价方法如下：
(1)成形情况：将制备好的膏体装入裱花袋，剪成牙膏管口大小的口径，将牙膏从裱花袋中挤出一条在易吸水的滤纸上，轻微用力挤出，若挤压力较大，不易将膏体挤出，说明牙膏太稠，否则，说明膏体太稀，稠稀适中，拉丝明显；挤出的膏体是否易切断。
(2)膏体形态：将牙膏挤出两条放在黑纸上，观察膏体是否洁净、均匀、细腻，是否水分分离，色泽是否正常或有无杂质；整体是否向下塌陷；膏体放置一段时间，是否很快干燥。在一条膏体表面用别形针划0.5～1cm的槽，观察该槽在适当的时间内是否保持其形状不变，若正常，表明膏体正常。
(3)看渗水现象：挤点牙膏放在毛边纸上，用手指均匀摊开，看纸的反面有无渗水，质好牙膏渗水很少；
(4)看有无过硬颗粒：将少许牙膏涂抹在载波片上，用手指摊均匀捺压，洗净看玻片有无划痕，如有会在刷牙时划伤牙；
表3感官评分指标
2.2正交试验优选牙膏基础配方
根据上述膏基辅料的筛选，确定牙膏摩擦剂为磷酸氢钙与二氧化硅，保湿剂为70％山梨醇液与甘油，胶着剂为CMC-Na与汉生胶的复配体系，为进一步优化牙膏膏基配方，采用正交实验设计，按感官评分体系标准筛选最佳配方工艺，结果如下：
表4正交因素水平表
| A(磷酸氢钙:二氧化硅) | B(70％山梨醇液:甘油) | C(CMC-Na:汉生胶) | |
| 1 | 2:1 | 2:1 | 1:1 |
| 2 | 3:1 | 3:1 | 2:1 |
| 3 | 4:1 | 4:1 | 3:1 |
表5正交实验结果
| 实验号 | A | B | C | 感官评价 |
| 1 | 1 | 1 | 1 | 79.5 |
| 2 | 1 | 2 | 2 | 84.5 |
| 3 | 1 | 3 | 3 | 81.4 |
| 4 | 2 | 1 | 2 | 87.4 |
| 5 | 2 | 2 | 3 | 89.3 |
| 6 | 2 | 3 | 1 | 85.5 |
| 7 | 3 | 1 | 3 | 80.5 |
| 8 | 3 | 2 | 1 | 84.5 |
| 9 | 3 | 3 | 2 | 82.5 |
| 均值1 | 81.800 | 82.467 | 83.167 | |
| 均值2 | 87.400 | 86.100 | 84.800 | |
| 均值3 | 82.500 | 83.133 | 83.733 | |
| 极差 | 5.600 | 3.633 | 1.633 |
表6方差分析
| 因素 | 偏差平方和 | 自由度 | F比 | F临界值 | 显著性 |
| A | 55.860 | 2 | 40.274 | 19.000 | * |
| B | 22.447 | 2 | 16.184 | 19.000 | |
| C | 4.127 | 2 | 2.975 | 19.000 | |
| 误差 | 1.39 | 2 |
*P＜0.05
通过正交试验直观与方差分析，结果表明，各因素对牙膏膏基的影响大小为A＞B＞C，即复合摩擦剂的配比对膏基的整体影响最大，其次是保湿剂，其中因素A对牙膏膏基配方的影响具有统计学意义。根据分析结果，优选牙膏膏基用量配比为：磷酸氢钙：二氧化硅＝3:1，70％山梨醇液:甘油＝3:1，CMC-Na:汉生胶＝2:1。
2.2.2其他成分用量筛选
通过预实验发现发泡剂的添加会影响膏基整体感官评价的判断，故发泡剂放在基础膏基配方确定后再筛选其用量，发泡剂用K12(十二烷基硫酸钠)；由于中草药等功能添加剂味苦或涩，特别草果油的添加量较大时，口感会辣并且冲鼻，影响牙膏的口感，经过多次预实验，确定木糖醇与糖精钠复配作为甜味剂；薄荷脑与精新柚果油复配作为香精，改善牙膏口感，本实验在最优膏基配方基础上再设计9个配方如表7所示，调整功效物质、发泡剂、甜味剂与香精的用量，其中功效物质的用量取1.7％(草果油0.05％、艾纳香油0.2％、凉粉草提取物0.5％、鼠尾草提取物0.5％、丹皮酚0.2％、叶绿素铜纳0.05％、尿囊素0.2％)、2.98％(草果油0.1％、艾纳香油0.3％、凉粉草提取物1％、鼠尾草提取物1％、丹皮酚0.25％、叶绿素铜纳0.08％、尿囊素0.25％)、5.6％(草果油0.15％、艾纳香油0.5％、凉粉草提取物2％、鼠尾草提取物2％、丹皮酚0.4％、叶绿素铜纳0.15％、尿囊素0.4％)。
牙膏起泡量的测定：预先量称45℃、20mL的水，称取待测牙膏1g于烧杯中，加入少量水溶解膏体，将溶解后的膏体倒入具塞量筒，用剩余水清洗烧杯，再倒入量筒，盖好瓶塞，按紧瓶塞，用最大力度摇匀量筒中的溶液，目测膏体完全溶解后停止，将量筒放置于操作台上静置5min，以目测量筒泡沫分布最集中的位置为准，记录起泡量。
表7牙膏其他成分用量筛选
根据综上筛选，得出牙膏其他成分用量为配方4，最终得出复方功效型牙膏优选配方如下：
表8复方功效型牙膏配方比
| 牙膏成分 | 原料质量要求 | 百分比％ |
| 磷酸氢钙 | 30％ | |
| 二氧化硅 | 食品级 | 10％ |
| 70％山梨醇液 | 食品级，≥70％ | 24％ |
| 甘油 | 纯度:99.9％ | 8％ |
| CMC-Na | 食品级，耐酸高粘 | 1％ |
| 黄原胶 | 食品级 | 0.5％ |
| 苯甲酸钠 | 食品级 | 0.1％ |
| 焦磷酸钠 | 食品级 | 0.55％ |
| 植酸钠 | 食品级 | 0.35％ |
| K12(十二烷基硫酸钠) | 工业级 | 2.5％ |
| 艾纳香油 | 纯精油 | 0.3％ |
| 草果油 | 纯精油 | 0.1％ |
| 凉粉草提取物 | 醇提(20:1) | 1％ |
| 鼠尾草提取物 | 醇提(20:1) | 1％ |
| 丹皮酚 | 水溶，≥99％ | 0.25％ |
| 叶绿素铜纳 | 食品级 | 0.08％ |
| 尿囊素 | 医药级，≥99％ | 0.25％ |
| 木糖醇 | 食品级 | 0.25％ |
| 糖精钠 | 食品级 | 0.3％ |
| 薄荷脑 | 医药级 | 0.6％ |
| 清新柚果香精 | 果香型 | 0.1％ |
| 去离子水 | 28％ |
在实际生产中，发泡剂需先加到溶胀后的胶液中，加热至70℃时，搅拌均匀，因为发泡剂此时加入可以起到消泡作用，降低搅拌过程中大量泡沫产生；再依次加入二氧化硅与磷酸氢钙(摩擦剂粉末此时加入再次起到消泡作用)，先手动搅拌与胶液充分混合后，在温度保持1000rpm转速下充分搅拌20min后，转速调至500～700rpm再搅拌30min，使其充分搅拌均匀，得牙膏膏基；待牙膏膏基温度降至约45℃，依次加入功效物质、木糖醇、糖精钠与香精，在转速500rpm条件下充分搅拌30min，抽真空后静止放置24h，即得复方功效型牙膏。将所制得的复方功效型牙膏重复试验三次，并装三次样品牙膏进行稳定性考察，结果其稠度、ph值稳定，膏体没有分水，脱壳等现象，且香味、色泽正常。
实施例3复方功效型牙膏抑菌性能检测
3.1试验材料与介绍
菌种：变形链球菌标准株(Streptococcus mutans,SM)，ATCC25175；牙龈卟啉单胞菌标准株(Porphyromonas gingivalis,PG)，ATCC33277；菌株均由成都里来生物科技有限公司分子生物检验室提供。其中变形链球菌是口腔占比最大的链球菌属中的一种，是龈齿发病的主要致病菌；牙龈卟啉单胞菌是慢性与侵袭性牙周炎、牙龈脓肿和牙周感染主要的致病菌，因此主要对这两种菌的抑菌性能进行检测。
培养基：兔血脑心浸出液肉汤(BHI)培养基(上海源叶生物科技有限公司)，厌氧肉肝汤(北京索莱宝科技有限公司)。
空白牙膏(无添加功效物质与香精)与样品牙膏1(功效物质1.7％)、样品牙膏2(功效物质2.98％)、样品牙膏3(功效物质5.6％)以及样品牙膏4(功效物质不含叶绿素铜钠与尿囊素，其他与样品牙膏2配比一样)
3.2试验方法
菌液制备：将低温保存的标准菌株变形链球菌、牙龈卟啉单胞菌，各取50μL接种至兔血BHI培养基中，划线使其能形成单个菌落，将接种平板放至厌氧箱中(80％ N2，10％ H2，10％CO2)培养3d活化。然后挑取平板菌落接种至厌氧肉肝汤中培养72h，紫外分光光度计测定菌液浓度OD600为0.5～1.0之间，检验纯度后用相应的培养液将菌液稀释成1×107CFU/mL的菌悬液备用。
抑菌样品的制备：分别取称三种试样牙膏3.0g，加入10mL去离子水搅拌均匀得样品溶液，将灭菌滤纸片(d＝6mm)浸泡于配置好的样品溶液中5min，提取出平放于灭菌好的平皿中，自室温下干燥后备用，得样品牙膏1、样品牙膏2、样品牙膏3、样品牙膏4。
阴性对照样品1的制备
称取空白(无添加功效物质与香精)牙膏3.0g，加入10ml去离子水搅拌均匀，得阴性对照样品，将灭菌滤纸片(d＝6mm)浸泡于配置好的样品溶液中5min，提出平放于灭菌好的平皿中，自室温下干燥后备用。
阴性对照样品2的制备
将灭菌滤纸片(d＝6mm)浸泡于10ml无菌蒸馏水中，提出平放于灭菌好的平皿中，自室温下干燥后备用。
试验菌接种
用移液枪取备好的菌悬液50μl分别置于相应培养基平板上，瓶用涂布棒在培养基平皿内表面均匀涂抹3次，每涂抹一次转动60度，最后将涂布棒绕平板边缘涂抹一周，盖好平皿。将浸泡过的滤纸片按间隔贴于含菌平板上，并用无菌镊子轻压样片，使其紧贴于平板表面，每平板等间距放置3片，每个样品做3个平行实验，盖好平皿，瓶用封口膜封住，放置37℃恒温培养箱中培养24h后，观察并记录抑菌圈的有无，选择均匀而完全无菌生长的抑菌环，用游标卡尺准确测量其直径大小，求平均值。
评价标准
抑菌环直径大于7mm判为有抑菌作用，小于或等于7mm者判为无抑菌作用；3次同一重复试验均有抑菌作用者，抑菌试验结果有效。
结果表明样品三种样品牙膏对变形链球菌与牙龈卟单胞菌均有抑菌效果，其中功效物质添加的量最大时，抑菌效果越明显，与样品牙膏4对比，表明增加叶绿素铜纳与尿囊素，可以提高其抑菌性能，结合功效物质对牙膏膏体的影响，最终筛选样品牙膏2功效物质作为最优配方比，具体见表9，如下：
表9复方功效型牙膏抑菌性能检测
实施例4复方功效型牙膏口腔溃疡修复性能检测
4.1实验耗材
动物：SD大鼠9只，SPF级，6周龄，体质量(180±20)g，购于长沙市天勤生物技术有限公司。
空白牙膏(无添加功效物质与香精)与样品牙膏2中最终配方自制
水合氯醛(北京索莱宝科技有限公司)
甲基紫精溶液(上海将来实业股份有限公司)
4.2实验方法
实验动物分组及给药
取SD大鼠9只，在1周适应性饲养，正常后随机均分为3组，即溃疡自然愈合组，空白牙膏组以及样口牙膏组。这3组大鼠进行口腔溃疡模型的造模，其中溃疡自然愈合组不给药，让其自然愈合，其余2组大鼠造模后24h起每日涂沫空白牙膏与样品牙膏，每次涂抹0.1g，一天3次。
口腔溃疡动物模型建立
采用改良后的陈谦明法构建口腔溃疡动物模型，首先在大鼠腹腔注射10％水合氯醛(3mL/kg)麻醉大鼠，将其固定于手术台，取仰卧位，用止血钳撑开上下颌，用平齿镊拉出一侧颊囊，再用5号皮试针缓慢均匀扇形注射10mmol/L甲基紫精溶液0.25mL于颊囊黏膜下层约8mm处，并用预制温度为100℃、直径约为5mm铁钉于注射处触烫3s，手电观察即可见该处有约5mm的白色损害；24h肉眼观察颊囊处有直径约为5mm的溃疡形成，表面有黄色假膜覆盖，周围组织充血水肿，并有炎性分泌物渗出，大鼠口腔内唾液分泌量增加。
结果显示，溃疡自然愈合组在第7天开始出现愈合，第11天全部痊愈，平均愈合天数为9.33天；空白牙膏组在第6天开始出现愈合，第10天全部痊愈，平均愈合时间为8.5天；样品牙膏组在第3天开始出现愈合，第6天全部痊愈，平均愈合时间为6天。
表10复方功效型牙膏溃疡性能检测
| 实验组 | 平均愈合天数(d) |
| 溃疡自然愈合组 | 9.33 |
| 空白牙膏 | 8.5 |
| 样品牙膏 | 5.17 |
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。
Claims (6)
1.一种复方功效型牙膏，其特征在于，按重量百分比计，包括以下成分：
所述的复方功效型牙膏的制备方法，包括以下步骤：
S1：所有粉末或固体状原料研磨，过筛，备用；
S2：制胶：称取山梨醇和甘油，混合均匀，加入羧甲基纤维素钠和水，搅拌至均匀无透明颗粒，待羧甲基纤维素钠完全溶胀，再加入已用冷水分散均匀的黄原胶，充分搅拌均匀后，在温度70～75℃、转速700～1000rpm条件下搅拌，得胶液；同时将苯甲酸钠、焦磷酸钠、植酸钠与水混合并加热，充分搅拌至完全溶解后，加至胶液中搅拌均匀，静置，待胶液充分溶胀，备用；
S3：制膏：将水加入溶胀后的胶液中，加热，先加入十二烷基硫酸钠，搅拌均匀；再加入复合摩擦剂，搅拌，得牙膏膏基；其中，所述复合摩擦剂为磷酸氢钙和二氧化硅；
S4：待牙膏膏基温度降至42～45℃，依次加入功效物质、木糖醇、糖精钠与香精，充分搅拌，真空脱气后静置，即得复方功效型牙膏；其中，所述功效物质为草果油、艾纳香油、凉粉草提取物、鼠尾草提取物、丹皮酚、叶绿素铜钠和尿囊素，所述香精为柚果香精和薄荷脑。
2.根据权利要求1所述复方功效型牙膏，其特征在于，按重量百分比计，包括以下成分：
3.根据权利要求1所述复方功效型牙膏，其特征在于，草果油与艾纳香油通过以下步骤制得：
取阴干后的艾纳香枝叶与草果果实，粉碎过筛得粉末，加入蒸馏水、果胶酶、木聚糖酶，调pH，酶解，灭酶，再进行水蒸汽蒸馏提取，得挥发油。
4.根据权利要求1所述复方功效型牙膏，其特征在于，草果油与艾纳香油通过以下步骤制得：
取阴干后的艾纳香枝叶与草果果实，粉碎过筛得粉末，加入粉末10倍质量的蒸馏水，加入果胶酶1000U/g粉末以及木聚糖酶2000U/g粉末，调pH至5.5，50℃下酶解2小时，灭酶，再进行水蒸汽蒸馏提取，提取3次，提取时间分别为4小时、3小时、2小时，三次所得的挥发油合并备用。
5.根据权利要求1所述的复方功效型牙膏，其特征在于，步骤S3，将水加入溶胀后的胶液中，加热至70℃时，先加入十二烷基硫酸钠，搅拌均匀；再加入复合摩擦剂，混合后，再1000～1200rpm转速下充分搅拌20min，转速调至500～700rpm再搅拌30min，得牙膏膏基。
6.根据权利要求1所述的复方功效型牙膏，其特征在于，步骤S4，待牙膏膏基温度降至45℃，依次加入功效物质、木糖醇、糖精钠与香精，在转速500rpm条件下充分搅拌30min，真空脱气后静置至少24h，即得复方功效型牙膏。
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