CN111434329A - 一种含花椒提取物的抑菌抗炎保健牙膏 - Google Patents
一种含花椒提取物的抑菌抗炎保健牙膏 Download PDFInfo
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Abstract
一种含四氢小檗碱、香叶木素、石吊兰素等抗炎成分的大红袍花椒提取物及其抗炎抑菌牙膏的制备方法,涉及口腔保健品,特别是牙膏组合物。大红袍花椒在我国素有“中华名椒”盛誉,具有抑菌、抗炎、镇痛等功效。本发明大红袍花椒提取物为挥发油部位和乙醇提取部位的混合组分,经UPLC‑Q‑TOF在大红袍花椒中分析出26种花椒属未见报道的化合物,其中含有多种抑菌、抗炎成分,例如四氢小檗碱、香叶木素、石吊兰素等。以大红袍花椒提取物为原料制备的牙膏组成:磨擦剂18‑24%、增稠剂0.3‑0.7%、保湿剂50‑60%、起泡剂1.8‑2.2%、香料0.5‑1%、防腐剂0.12‑0.15%、甜味剂0.25‑0.35%、花椒提取物3.6%,余量为水。除洁齿外,本发明具有缓解牙痛,减轻牙龈炎、抑菌抗炎、治疗口腔溃疡等作用,且成本低,具有明显的公共卫生价值。
Description
一、技术领域
本发明属于大红袍花椒中化学成分研究技术领域,制备含有四氢小檗碱、香叶木素、石吊兰素等抗炎成分的大红袍花椒提取物,并以此为原料,制备一种新型抗炎抑菌牙膏。
二、背景技术
大红袍花椒在我国素有“中华名椒”盛誉,尤其陕西省韩城大红袍花椒历史悠久,具有抑菌、抗炎、镇痛等功效。本发明经超高效液相色谱-四极杆-飞行时间质谱分析出26种在花椒中首次发现的化合物,其中含有多种抗炎成分,例如四氢小檗碱、香叶木素、石吊兰素等。以大红袍花椒提取物为原料制备牙膏是本发明涉及的大红袍花椒开发的应用形式。
牙膏是一种常见的日常生活用品,是由多种原料混合制成的,如磨擦剂、保湿剂、增稠剂、发泡剂、各类添加剂及水等,用来清洁口腔美白牙齿或防止牙齿和牙周疾病。
按照牙膏的功能来划分,牙膏通常包括两大类:一类是洁齿美白牙膏,主要是为了清洁口腔美白牙齿;另一类是药物牙膏,其基本原理是在牙膏中加入药物成分,从而使牙膏具有止血、防龋齿、防过敏、消炎等功能。近年来,随着人们生活水平不断提高,对牙膏提出了更高的要求,除了洁齿和预防牙齿疾病外,对口腔的护理及功能保健作用和安全性有很高的要求,因此,安全性、功能性口腔护理保健型牙膏成了当下牙膏创新的一个趋势。
因此,我们研发了一款不添加氧化剂的,采用药食同源的天然产物大红袍花椒的主要有效成分来温和抑菌抗炎的牙膏,是牙膏行业内的新创造发明。
三、发明内容
本发明经超高效液相色谱-四极杆-飞行时间质谱联用技术在大红袍花椒中首次发现的26种化合物花椒属植物中未见报道的化合物(如:四氢小檗碱、香叶木素、石吊兰素等),该类化合物成分具有抑制细菌滋生,消除炎症的功能,并针对针对现代社会对口腔的护理及功能保健作用以及安全保障的需求,而研究设计一种含有大红袍花椒提取物的抗炎抑菌牙膏(以下简称“花椒牙膏”),从而有助于口腔的卫生保健。
技术方案是:本发明大红袍花椒提取物包括挥发油部位和乙醇提取部位;利用超高效液相色谱-四极杆-飞行时间质谱联用技术,系统分析大红袍花椒提取物,首次发现的26种化合物花椒属植物中未见报道的化合物,包括具有抗炎、抑菌作用的特征性成分四氢小檗碱、香叶木素、石吊兰素等;含有大红袍提取物的一种花椒牙膏,其特征是它由下列重量百分比的原料组成:磨擦剂18-24%、增稠剂0.3-0.7%、保湿剂50-60%、起泡剂1.8-2.2%、香料0.5- 1%、防腐剂0.12-0.15%、甜味剂0.25-0.35%、大红袍花椒提取物2.9-3.3%,余量为水,制作时将上述原料按上述配方进行配料,再把配料后的原料按现有的制作方法混合制得。磨擦剂、保湿剂、起泡剂、香料均为现有牙膏的添加物质,它的种类较多,这里不再多述。但其最佳选择为所述磨擦剂为二氧化硅;增稠剂为非离子瓜尔胶;保湿剂为甘油和70%山梨醇复配;甜味剂为糖精钠;起泡剂为十二烷基硫酸钠;香料为天然薄荷油;甜味剂为糖精;防腐剂为尼泊金乙酯、尼泊金丙酯;功效成分添加剂为花椒提取物。它是本发明的技术核心,在牙膏原料中引入花椒提取物活性成分,该类成分具有抑制细菌滋生,消除炎症的功能,从而有助于口腔的卫生保健。
本发明的优点是:由于在牙膏原料中引入了药食同源花椒的活性成分,即(挥发油、生物碱、黄酮类、香豆素),其中有26种在大红袍花椒中发现的新型成分,主要特征成分在于四氢小檗碱、香叶木素、石吊兰素等新型抗炎、抗菌成分使得它不仅具有抑制细菌滋生,消除炎症的功能,而且还具有安全、天然口腔卫生保健的功能,是一种效果较佳的口腔保健牙膏。
四、具体实施方式
(一)、花椒提取物的制备
取大红袍花椒1kg,加入15倍量去离子水,利用挥发油提取器,加热提取2h,得到花椒中挥发油类成分;收集提取过挥发油的花椒残渣,分别加入8倍量75%乙醇加热回流提取两次,收集乙醇提取液,浓缩至浸膏;将挥发油部位和乙醇提取部位合并即得花椒提取物。
(二)、一种超高效液相色谱-四极杆-静电场轨道阱联用(UPLC-Q-ExactiveOrbitrap-MS)技术对大红袍花椒进行全成分分析,具体步骤如下:
1.仪器与材料
UPLC-Q-Exactive Orbitrap MS四极杆-静电场轨道阱高分辨质谱仪、 Ultimate3000超高效液相色谱系统(赛默飞世尔科技公司,美国);KQ- 250E型超声波清洗器(昆山市超声仪器有限公司);ACQUITY BEH C18 (100mm×2.1mm,1.7μm,Waters美国);色谱乙腈(Fisher公司) 2.色谱条件
以0.1%甲酸-水为流动相A,以乙腈为流动相B,线性梯度洗脱,0~1 min,20%~35%B;1min~5min,35%~80%B;5min~15min,80%~100%B; 15min~17min,100%B;17.1min~20min,20%B,体积流量为0.4 mL/min;柱温为40℃;进样量10μL。
3.质谱条件
正离子检测条件:离子源HESI;毛细管电压3800V;毛细管温度 350℃;源内温度320℃;质谱采集范围m/z 100-1500;分辨率为 70000;S-Lens RF Level为55。负离子检测条件:离子源HESI;毛细管电压 3800;毛细管温度350℃;源内温度320℃;质谱采集范围m/z100- 1500;分辨率为70000;S-Lens RF Level为55。
4.供试品溶液制备
取大红袍花椒提取物0.1g,加入75%色谱甲醇10mL,称定质量,超声处理30min,再次称定质量,用75%色谱甲醇补足减失的质量,滤过,滤液过0.22μm滤膜,即得供试品滤液。
5.化学成分鉴定
取大红袍花椒供试液,按照已述色谱质谱条件进行分析,分别得到正、负离子模式下数据。根据Xcalibur计算出的高分辨精确质量数,据实际测得的相对分子质量与理论相对分子质量二者偏差小于5ppm的原则及同位素丰度比,确定各色谱峰对应化合物的分子式。
根据中药材化学成分数据库及相关文献,快速确证可能的化学成分。最终采用UPLC-Q-Exactive Orbitrap-MS的方法推断出30种化学成分,其中文献中报道在花椒属中发现的化合物:羟基-β-山椒、花椒油素2种在正离子模式下分析获得;3,5,6-三羟基-7,4′-二甲氧基黄酮和黄连素β-D-葡萄糖苷2 种化合物在负离子模式下分析获得,其余26种化合物未曾在花椒属植物中发现,例如:四氢小檗碱、香叶木素、石吊兰素等,通过本次实验研究首次推测获得。正离子模式下被推断的15种化学成分的相对保留时间、相对分子质量、分子式、一级质谱数据及二级质谱碎片离子见表1,其提取离子流图如图1;负离子模式下被推断的15种化学成分的相对保留时间、相对分子质量、分子式、一级质谱数据及二级质谱碎片离子见表2,其提取离子流图如图2。
附图说明
图1正离子模式下15种化学成分的提取离子流图
图2负离子模式下15种化学成分的提取离子流图
表1正离子模式下15种化学成分的相对保留时间、相对分子质量、分子式、一级质谱及二级质谱碎片离子
表2负离子模式下15种化学成分的相对保留时间、相对分子质量、分子式、一级质谱及二级质谱碎片离子
(三)、本发明牙膏组合物及制备
本发明的一种含花椒提取物的抑菌抗炎保健牙膏,其特征是各组份内容及所占重量百分比为:摩擦剂二氧化硅,其重量百分比为18-24%;增稠剂为非离子瓜尔胶,其重量百分比为0.3-0.7%;保湿剂为甘油和70%山梨醇复配,其重量百分比为50-60%;起泡剂为十二烷基硫酸钠,其重量百分比为 1.8-2.2%;香料为天然薄荷油,其重量百分比为0.5-1%;甜味剂为糖精,其重量百分比为25-0.35%;防腐剂为尼泊金乙酯、尼泊金丙酯,其重量百分比为0.12-0.15%;含大红袍花椒提取物的牙膏,其重量百分比为3.6%;其余为去离子水。制作时将上述原料通过搅拌、碾磨并真空脱气,获得牙膏膏体。
(四)、二甲苯致小鼠耳肿胀实验
动物:昆明种小鼠50只
药物及试剂:去离子水,二甲苯(分析纯,北京化工厂),云南白药牙膏(云南白药集团股份有限公司),花椒提取物(相当于同质量花椒牙膏中配方中添加药量3.3%),花椒牙膏,空白基质牙膏,均为本实验室自制。
1.二甲苯致小鼠耳肿胀实验
取昆明种小鼠50只,随机分成5组,每组10只,分别为模型组、牙膏空白基质组、阳性组(云南白药牙膏)、花椒牙膏组、花椒提取物组。于小鼠右耳两面涂以二甲苯,毎只50μL致炎,左耳不加处理作自身空白对照, 30min后牙膏空白基质组、阳性组、花椒牙膏组分别在右耳涂以相对应的牙膏约每只0.1g;花椒提取物组在右耳涂以花椒提取物每只约为33mg。模型组致炎90min后脱颈椎处死小鼠;其他组涂药Ih后脱颈椎处死小鼠,擦净耳部所涂药物,沿耳廓基线剪下两耳,用6.5mm打孔器冲下左右两耳同一部位的圆片,于分析天平称重,精确到0.0001g。用右耳片重量减去左耳片重量为肺胀度,比较药物的抗炎作用,计算肿胀抑制率。
肿胀抑制率=(空白对照组平均肿胀度-给药组平均肿胀度)/空白对照组平均肿胀度×100%
2.结果如下表:
组别 | 剂量(/只) | 肿胀度/mg | 抑制率/% |
模型组 | — | 8.36±1.54 | — |
云南白药牙膏组 | 0.1g | 4.52±2.31 | 45.9 |
花椒牙膏组 | 0.1g | 3.69±2.64 | 55.9 |
花椒提取物组 | 33mg | 3.21±2.68 | 61.6 |
牙膏空白基质组 | 0.1g | 8.15±3.37 | 2.5 |
3.结果表明:
花椒牙膏组、云南白药牙膏组、花椒提取物组与模型组相比,均能抑制二甲苯引起肿胀的作用(P<0.01),其中花椒提取物组抗炎效果优于云南白药牙膏组,花椒牙膏组略高于云南白药牙膏组;牙膏空白基质组与模型组相比,无显著性差异(P>0.01);花椒牙膏组与牙膏空白基质组相化,具有显著的差异(P<0.01)。
(五)、花椒牙膏对口腔5种主要致病菌抑菌作用实验
仪器:HH-B11-600电热恒温培养箱(上海市跃进农场医疗器械厂), YXO-LS-SII立式压力蒸汽灭菌器(上海博讯实业有限公司医疗设备厂),超净台(上海博讯实业公司),24孔细胞培养板(美国Corning公司),2.5L 厌氧产气袋(英国Oxoid公司),2.5L厌氧培养袋(青岛精科仪器试剂有限公司)
供试样品:云南白药牙膏(云南白药集团股份有限公司)、花椒提取物、牙膏空白基质组(批号20170701)、花椒牙膏(化号:2017001),均为实验室自制。
实验菌株:金黄色葡萄球菌由北京中医药大学基础医学院免疫病研究中心提供,口腔变形链球菌,变形链球菌,嗜酸乳杆菌,黏性性放线菌购均来自北京中医药大学生命科学院。
培养基:胰酪胨大豆琼脂培养基(TSA,批号:13279327)、胰酪胨大豆肉汤培养基(TSA,批号:1352765)、脑心浸液肉汤培养基(BHI,批号:1333387)、脑心浸液琼脂培养基(BHIA,批号:12575645购于英国Oxford 公司、营养肉汤培养基(批号:20170720)购于北京化学试剂公司、胰蛋白大豆肉汤(批号:20170720)购于北京双旋微生物培养基制品厂。TSA、TSB培养基用于口腔变形链球菌培养BHI、BHIA培养基用于变形链球菌、嗜酸乳杆菌、黏性放线菌的培养;营养肉汤和营养琼脂用于金黃龟葡萄球菌的培养。
1.花椒牙膏对口腔5种主要致病菌抑菌作用实验
采用厌氧血平板培养基。厌氧培养18h(90%N2,5%CO2,37℃)和2~3d 专性厌氧菌培养(75%N2,15%H2,5%CO2,37℃)。保存之细菌复苏,经生化鉴定后接种于相应琼脂平板。挑取琼脂表面的单个菌落混悬于相应液体培养基(胰蛋白大豆肉汤)中(1个1mm菌落/ml)培养,培养相应时间(18h)后使菌液浓度呈105~106CFU/ml备用。
有效浓度筛选采用微量液体稀释法检测最小抑菌浓度(minimum inhibitoryconcentration,MIC)和最小杀菌浓度(minimum bactericidal concentration, MBC)。MIC测定:用无菌微量加样器吸取呈梯度稀释的各种样品50μl于无菌 96孔微孔板中,再加入等量菌液,混和。放置适宜培养条件下孵育,18h后测定结果。肉眼观察,以没有发生浑浊现象的最高稀释微孔的药物浓度为 MIC。MBC测定:依次取未发生浑浊现象的微孔培养液涂布于琼脂平板上,培养12h后计算菌落数,微孔内的活菌数/起始活菌数≤0.1%的孔内药物浓度为MBC。阳性对照:不加各种药品,只加菌液和等量液体培养基。阴性对照: 不加菌液,只加各种药品和等量液体培养基。
2.结果如下表:
表5各液体稀释法测定实验抗菌液的MIC
mg/ml
表6各液体稀释法测定实验抗菌液的MBC
mg/ml
3.结果表明:
由表2与表3结果可知各组的最小杀菌浓度与最小杀菌浓度一样,牙膏空白基质组并未检测到有抑菌杀菌能力,本花椒牙膏在对5种实验菌口腔变形链球菌、黏性放线菌、变形链球菌、嗜酸乳酸菌、金黄色葡萄球菌抑菌作用上要高于云南白药牙膏,但是含花椒提取物的牙膏与空白牙膏相比对5种实验菌口腔变形链球菌、黏性放线菌、变形链球菌、嗜酸乳酸菌、金黄色葡萄球菌抑菌作用良好,花椒提取物的抑菌作用很好,进一步说明添加此含量的花椒提取物具有不错的抑菌作用。
(六)、花椒牙膏使用效果测试
选择400名受试者进行效果测试。选择标准:按医疗常规认定的诊断标准选择病例。受试者年龄:20-60岁;性别:男50名,女50名;
使用方法:用花椒牙膏每天早晚各使用一次,每次3-5分钟,使用期间,不加用其他药物。疗效标准:a、效果显著:症状基本消失;b、有效:症状好转;c、无效:无明显效果。疗效观察结果:观察5-14天,结果见表 4。
表7本发明牙膏试用结果
病症 | 受试人数 | 显效 | 有效 | 无效 | 有效率% |
牙痛 | 100 | 80 | 16 | 4 | 96 |
牙龈炎 | 100 | 92 | 4 | 4 | 96 |
口腔溃疡 | 100 | 84 | 8 | 8 | 92 |
口臭 | 100 | 88 | 3 | 9 | 91 |
Claims (6)
1.大红袍花椒提取物包括大红袍花椒中的挥发油提取部位和大红袍花椒中乙醇提取部位的混合组分。
2.根据权利要求1所述的大红袍花椒提取物,其特征成分在于主要含有抗炎、抑菌成分四氢小檗碱、香叶木素、石吊兰素等。
3.根据权利要求1所述的大红袍花椒提取物的应用为含大红袍花椒提取物的牙膏,包括摩擦剂、增稠剂、保湿剂、起泡剂、香料、甜味剂以及防腐剂,其特征是牙膏中具有总重量百分比为3.6%的大红袍花椒提取物。
4.根据权利要求3所述的含大红袍花椒提取物的牙膏,其特征是各组份内容及所占重量百分比为:
摩擦剂二氧化硅,其重量百分比为18-24%;
增稠剂为非离子瓜尔胶,其重量百分比为0.3-0.7%;
保湿剂为甘油和70%山梨醇复配,其重量百分比为50-60%;
起泡剂为十二烷基硫酸钠,其重量百分比为1.8-2.2%;
香料为天然薄荷油,其重量百分比为0.5-1%;
甜味剂为糖精,其重量百分比为0.25-0.35%;
防腐剂为尼泊金乙酯、尼泊金丙酯,其重量百分比为0.12-0.15%;
其余为去离子水。
5.如权利要求3所述的含大红袍花椒提取物的牙膏的制备方法,其特征是按所述重量百分比将大红袍花椒提取物、摩擦剂、增稠剂、保湿剂、起泡剂、香料、甜味剂以及防腐剂混合,通过搅拌、碾磨并真空脱气,获得牙膏膏体。
6.根据权利要求5所述的含大红袍花椒提取物的牙膏的制备方法,其特征是优选的方法为按所述重量百分比:
(1)将大红袍花椒提取物、保湿剂和糖精2%、放入去离子水中搅拌制成的去离子水溶液,与摩擦剂、增稠剂、起泡剂以及防腐剂混合,搅拌、碾磨并真空脱气;
(2)加入香精,搅拌、碾磨并真空脱气,获得牙膏膏体。
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CN117338670A (zh) * | 2023-11-22 | 2024-01-05 | 广州市盛龙口腔清洁用品有限公司 | 一种含青花椒提取物的牙膏及其制备方法 |
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CN115569092A (zh) * | 2022-05-11 | 2023-01-06 | 青岛中鑫诺生物科技有限公司 | 一种修复牙膏膏剂及其制备方法 |
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CN117338670A (zh) * | 2023-11-22 | 2024-01-05 | 广州市盛龙口腔清洁用品有限公司 | 一种含青花椒提取物的牙膏及其制备方法 |
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