CN113413346A - 一种含有神秘果荷叶提取物的牙膏及其制备方法 - Google Patents
一种含有神秘果荷叶提取物的牙膏及其制备方法 Download PDFInfo
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- CN113413346A CN113413346A CN202110891155.9A CN202110891155A CN113413346A CN 113413346 A CN113413346 A CN 113413346A CN 202110891155 A CN202110891155 A CN 202110891155A CN 113413346 A CN113413346 A CN 113413346A
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- miracle fruit
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- lotus leaf
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Classifications
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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Abstract
本发明涉及牙膏技术领域,尤其涉及一种含有神秘果荷叶提取物的牙膏及其制备方法,按重量份数计包含以下组分:神秘果提取物0.5‑8份;荷叶提取物0.5‑8份;润湿剂10‑30份;摩擦剂15‑45份;发泡剂0.5‑1.5份;粘合剂0.4‑1.6份;稳定剂0.15‑0.3份;甜味剂0.2‑0.8份;适量水及少量食用香精。本发明将神秘果提取物、荷叶提取物作为功效成分加入牙膏中,具有明显的消炎、抑菌、抗过敏作用,可用于防治牙周炎、牙龈炎和口腔炎、口腔溃疡等功效,减少口腔疾病,制备工艺简单,具有明显的公众卫生价值。
Description
技术领域
本发明涉及牙膏技术领域,尤其涉及一种含有神秘果荷叶提取物的牙膏及其制备方法。
背景技术
随着生活节奏的加快、饮食习惯变化和不良的饮食结构,口腔疾病发病率越来越高,包括牙周炎、齿禹病、牙菌斑、牙本质过敏、口臭和口腔溃疡等口腔问题。因此,抑制口腔致病细菌是预防口腔疾病的重要措施。
单纯以清洁牙齿为目的的牙膏已远远不能满足消费者的需求,因此,对口腔疾病具有预防和保健作用的功能型牙膏逐渐兴起。目前市场上具有抗菌作用的口腔护理品大多添加化学合成成分,会对口腔健康造成一定的威胁。
发明内容
本发明目的是针对背景技术中存在的问题,提出一种能有效保护牙齿的含有神秘果荷叶提取物的牙膏及其制备方法。
本发明的技术方案,一种含有神秘果荷叶提取物的牙膏,按重量份数计包含以下组分:神秘果提取物0.5-8份;荷叶提取物0.5-8份;润湿剂10-30份;摩擦剂15-45份;发泡剂0.5-1.5份;粘合剂0.4-1.6份;稳定剂0.15-0.3份;甜味剂0.2-0.8份;适量水及少量食用香精。
优选的,荷叶提取物与神秘果提取物比例为2∶1。
优选的,神秘果提取物的制备步骤如下:
S11、将神秘果枝叶粉碎,清洗后经60℃干燥箱烘干至恒重,粉碎过40目筛,取筛下物,得到神秘果粗粉;
S12、将神秘果粗粉按照质量比1:10加入75%乙醇浸泡8h,100℃加热回流提取2-5h,优选为3h,提取3次,过滤合并提取液,使用旋转蒸发仪(70℃)进行浓缩;过滤,上清液减压蒸馏,冷冻干燥,得枝叶粗提取物干粉溶于水中,经大孔吸附树脂处理,然后用乙醇水溶液洗脱,得到收集液分别进行真空浓缩,浓缩液用活性炭脱色后真空冷冻干燥,冷冻干燥得精制枝叶提取物,真空冷冻干燥的冷阱温度为-40至-65℃,优选为-55℃,真空度为1500-3000Pa,优选为2000Pa,提取物含总酚66.5%,枝提取物含总酚84.1%,即为神秘果提取物。
优选的,乙醇为含水乙醇,为75%乙醇。
优选的,润湿剂为丙二醇、山梨醇、甘油、丙三醇和聚乙二醇中的一种或几种;摩擦剂为磷酸氢钙、二氧化硅、碳酸钙、氢氧化铝、重质碳酸钙和轻质碳酸钙中的一种或几种;发泡剂为十二醇硫酸钠、十二烷基硫酸钠、N-月桂酰肌氨酸钠和甲基椰油酰基牛磺酸钠中的一种或几种;粘合剂包括海藻酸钠、羟甲基纤维素钠、黄原胶、羟乙基纤维素、瓜尔胶、阿拉伯胶和卡拉胶中的一种或几种。
优选的,甜味剂为糖精钠、蔗糖、木糖醇、甜蜜素和阿斯巴甜的一种或几种;食用香精为薄荷脑、留兰香油、青柠油、柠檬香油、橘子油、丁香油、茉莉香油、樱花油和薄荷油中的一种或几种;水为纯净水和去离子水中的一种或两种。
一种上述的含有神秘果荷叶提取物的牙膏的制备方法,包括以下步骤:
S21、将神秘果提取物与荷叶提取物、润湿剂、发泡剂和稳定剂溶解在水中,混合后加热,使制成的胶体呈均匀半透明粘状液态,然后放置,待其溶化膨胀后使用;
S22、将步骤S21所得胶体冷却至50-90℃,依次加入摩擦剂、粘合剂和甜味剂,继续搅拌;
S23、待胶体冷却至45℃以下,加入其余助剂,搅拌,制成膏体;
S24、将膏体研磨,然后真空脱气,静置,灭菌后即得牙膏成品。
优选的,S21中,混合过程在混料机中进行;加热过程在共沸锅中进行,加热至75-100℃,,放置0.5h以上,优选为1-2h。
优选的,S22中,胶体冷却至65-70℃;加入摩擦剂、粘合剂和甜味剂时在搅拌下进行,搅拌的转速为300-320r/min;继续搅拌的时间为0.5h以上,优选为l-2h,转速为350-360r/min。
优选的,S24中,研磨通过研磨机进行,研磨分二次进行,第一次研磨后贮存,第二次研磨后进行真空脱气,脱气到真空度达到-0.093MPa以下为止;静置的时间为2-4h。
与现有技术相比,本发明具有如下有益的技术效果:
本发明将神秘果提取物、荷叶提取物作为功效成分加入牙膏中,具有明显的消炎、抑菌、抗过敏作用,可用于防治牙周炎、牙龈炎和口腔炎、口腔溃疡等功效,减少口腔疾病,制备工艺简单,具有明显的公众卫生价值。
具体实施方式
实施例1
一种含有神秘果荷叶提取物的牙膏,按重量份数计包含以下组分:神秘果提取物1份;荷叶提取物2份;润湿剂20份;摩擦剂20份;发泡剂1.2份;粘合剂1份;稳定剂0.2份;甜味剂0.5份;适量水及少量食用香精。
所述神秘果提取物按照以下步骤制成:
(1)取粉碎后的神秘果,清洗后经60℃干燥箱烘干至恒重,粉碎过40目筛,取筛下物,得到神秘果粗粉;
⑵将神秘果粗粉按照质量比1:10加入75%乙醇浸泡8h,100℃加热回流提取3h,提取3次,过滤合并提取液,使用旋转蒸发仪(70℃)进行浓缩;
⑶将浓缩液用活性炭脱色后真空冷冻干燥,冷阱温度为-55℃,真空度为2000Pa,干燥后即得神秘果提取物。
上述的含有神秘果荷叶提取物的牙膏制备步骤为:
(1)将神秘果提取物1份、荷叶提取物2份、丙二醇20份、十二醇硫酸钠1.2份、焦磷酸钠0.2份用去离子水溶解,在混料机中搅拌均匀后,投入共沸锅中,加热至85℃,使制成的胶体呈均匀半透明粘状液态,然后放置2h,让其充分溶化膨胀后使用;
(2)将步骤⑴所得胶体冷却至65℃,将共沸锅放到搅拌器上,边搅拌(转速320r/min)边按顺序加入磷酸氢钙20份、海藻酸钠1份、糖精钠0.5份,继续搅拌2h(转速360r/min),使各种物料混合均匀;
(3)待胶体冷却至45℃以下,加入薄荷脑少量,通过机械混合搅拌均匀,制成具有一定粘性、稠度适当的膏体;
⑷将膏体经过研磨机研磨,将过粗、过硬的颗粒磨细,使膏体细腻、均匀、稳定,研磨分二次进行,第一次磨后贮存陈化lh,第二次研磨后进行真空脱气,直到真空度达到-0.093MPa为止,时间为60min;
(5)膏体脱气静置4h,灭菌后装入软管中并进行封口即得成品神秘果提取物荷叶提取物牙膏。
本实施例制备得到的牙膏的主要质量指标评价和抑菌效果试验如下:
1.牙膏外观、理化指标、卫生指标测定
取试样牙膏4支,1支样品室温保存,另3支样品放入-8℃±1℃的冰箱内,8h后取出,随即放入45℃±1℃恒温培养箱内,8h后取出,恢复室温,开盖观察,膏体没有溢出管口;将牙膏管体倒置,10s内无液体从管口滴出;膏体挤出后与室温保存样品相比较,其香味、色泽应正常。无过硬颗粒,pH值为7.98,泡沫量170mm,稠度26mm,牙膏的菌落的总数71cfu/g<国标的500cfu/g,致病菌未检出,铅、碑未超标,均符合牙膏质量国家标准GB8372-2008及《化妆品卫生规范》。
2.牙膏体外抑菌试验如下
采用滤纸片法测定所制牙膏的抑菌能力,选用的菌种为:牙龈卟啉单胞菌、黏性放线菌、内氏放线菌、具核梭杆菌;具体方法如下:将细菌培养液均匀交叉涂于培养皿的培养基上,将培养皿置于37℃的恒温培育箱中24h;分别取5μL经过稀释的不同浓度的牙膏药液、灭菌去热原水浸湿直径为6mm的无菌圆滤纸片,将小圆滤纸片均匀对称地贴附于培养基上的中央区域,将培养皿置37℃恒温培养箱中培养24h,分别测量抑菌圈直径,以抗菌区域直径的大小来初步评估分析实验牙膏的抗菌潜力,“-”表示抑菌圈小于1mm,样品没有抑菌能力,其中膏体的稀释浓度分别为20、40、80、160、320mg/ml,实验结果见表1。
表1:牙膏的体外抑菌试验结果
3.牙膏药效试验如下
随机选25名患者进行试牙膏药效学试验,受试者均是口腔炎症患者,男女不限,年龄22岁至48岁之间,使用周期为25天,对全部受试者进行刷牙方法指导。受试者使用统一的牙刷及指定的牙膏,要求用巴氏刷牙法每天刷牙2次(早7:00-9:00、晚7:30-9:30),每次至少2分钟,刷牙时使用牙膏膏体以2克为准。要求试验过程中不使用其它任何口腔卫生用品,如其它种类的牙膏、漱口水、牙线等。对饮食不限制,统计结果见表2。
表2:含神秘果提取物荷叶提取物牙膏药效学试验结果
实施例2
实施例2与实施例1的不同之处在于:在牙膏制备过程中,各组分的种类或含量有所不同,以及某些制作参数有所不同,具体为:
(1)将神秘果提取物1.25份,荷叶提取物2.5份、山梨醇25份、十二烷基硫酸钠1.0份、焦磷酸钠0.3份用去离子水溶解,在混料机中搅拌均匀后,投入共沸锅中,加热至90℃,使制成的胶体呈均匀半透明粘状液态,然后放置1.5h,让其充分溶化膨胀后使用;
(2)将步骤⑴所得胶体冷却至70℃,将共沸锅放到搅拌器上,边搅拌(转速300r/min)边按顺序加入二氧化硅25份、稜甲基纤维素钠1.2份、木糖醇0.6份,继续搅拌1.5h(转速350r/min),使各种物料混合均匀;
(3)待胶体冷却至45℃以下,加入薄荷脑与橘子油少量,通过机械混合搅拌均匀,制成具有一定粘性、稠度适当的膏体;
(4)将膏体经过研磨机研磨,将过粗、过硬的颗粒磨细,使膏体细腻、均匀、稳定,研磨分二次进行,第一次磨后贮存陈化2h,第二次研磨后进行真空脱气,直到真空度达到-0.096MPa为止,时间为50min;
(5)膏体脱气静置3h,灭菌后装入软管中并进行封口即得成品皂角刺提取物牙膏。
本实施例制备得到的牙膏的主要质量指标评价和抑菌效果试验如下:
1.牙膏外观、理化指标、卫生指标测定
取试样牙膏4支,1支样品室温保存,另3支样品放入-8℃±1℃的冰箱内,8h后取出,随即放入45℃±1℃恒温培养箱内,8h后取出,恢复室温,开盖观察,膏体没有溢出管口;将牙膏管体倒置,10s内无液体从管口滴出;膏体挤出后与室温保存样品相比较,其香味、色泽应正常。无过硬颗粒,pH值为8.05,泡沫量175mm,稠度28mm,牙膏的菌落的总数90cfu/g<国标的500cfu/g,致病菌未检出,铅、碑未超标,均符合牙膏质量国家标准GB8372-2008及《化妆品卫生规范》。
2.牙膏体外抑菌试验如下
采用滤纸片法测定所制牙膏的抑菌能力,选用的菌种为:牙龈卟啉单胞菌、黏性放线菌、内氏放线菌、具核梭杆菌;具体方法如下:将细菌培养液均匀交叉涂于培养皿的培养基上,将培养皿置于37℃的恒温培育箱中24h;分别取5μ1经过稀释的不同浓度的牙膏药液、灭菌去热原水浸湿直径为6mm的无菌圆滤纸片,将小圆滤纸片均匀对称地贴附于培养基上的中央区域,将培养皿置37℃恒温培养箱中培养24h,分别测量抑菌圈直径,以抗菌区域直径的大小来初步评估分析实验牙膏的抗菌潜力,“-”表示抑菌圈小于1mm,样品没有抑菌能力,其中膏体的稀释浓度分别为20、40、80、160、320mg/ml,实验结果见表3。
表3:牙膏的体外抑菌试验结果
3.牙膏药效试验如下
随机选25名患者进行试牙膏药效学试验,受试者均是口腔炎症患者,男女不限,年龄22岁至48岁之间,使用周期为25天,对全部受试者进行刷牙方法指导。受试者使用统一的牙刷及指定的牙膏,要求用巴氏刷牙法每天刷牙2次(早7:00-9:00、晚7:30-9:30),每次至少2分钟,刷牙时使用牙膏膏体以2克为准。要求试验过程中不使用其它任何口腔卫生用品,如其它种类的牙膏、漱口水、牙线等。对饮食不限制,统计结果见表4。
表4:含神秘果提取物荷叶提取物牙膏药效学试验结果
实施例3
实施例3与实施例1在制备牙膏过程中各组分和含量有所不同,以及某些制作参数有所不同,具体为:
⑴将神秘果提取物3份,荷叶提取物6份、甘油20份、甲基可可酯基牛磺酸钠1.5份、焦磷酸钠0.3份用去离子水溶解,在混料机中搅拌均匀后,投入共沸锅中,加热至100℃,使制成的胶体呈均匀半透明粘状液态,然后放置lh,让其充分溶化膨胀后使用;
(2)将步骤⑴所得胶体冷却至65℃,将共沸锅放到搅拌器上,边搅拌(转速310r/min)边按顺序加入方解石粉35份、瓜尔胶0.8份、甜蜜素0.7份,继续搅拌lh(转速350r/min),使各种物料混合均匀;
(3)待胶体冷却至45℃以下,加入薄荷脑与柠檬香油少量,通过机械混合搅拌均匀,制成具有一定粘性、稠度适当的膏体;
(4)将膏体经过研磨机研磨,将过粗、过硬的颗粒磨细,使膏体细腻、均匀、稳定,研磨分二次进行,第一次磨后贮存陈化3h,第二次研磨后进行真空脱气,直到真空度达到-0.096MPa为止,时间为40min;
(5)膏体脱气静置2h,灭菌后装入软管封口即得成品。
本实施例制备的牙膏,质量指标和抑菌效果如下
1.膏体外观,理化指标,卫生指标
取试样牙膏4支,1支样品室温保存,另3支样品放入-8℃±1℃的冰箱内,8h后取出,随即放入45℃±1℃恒温培养箱内,8h后取出,恢复室温,开盖观察,膏体没有溢出管口;将牙膏管体倒置,10s内无液体从管口滴出;膏体挤出后与室温保存样品相比较,其香味、色泽应正常。无过硬颗粒,pH值为8.05,泡沫量175mm,稠度28mm,牙膏的菌落的总数90cfu/g<国标的500cfu/g,致病菌未检出,铅、碑未超标,均符合牙膏质量国家标准GB8372-2008及《化妆品卫生规范》。
2.牙膏抑菌试验如下
选用的菌种为:牙龈卟啉单胞菌、黏性放线菌、内氏放线菌、具核梭杆菌;去热原水浸湿直径为6mm的无菌圆滤纸片,将小圆滤纸片均匀对称地贴附于培养基上的中央区域,将培养皿置37℃恒温培养箱中培养24h,分别测量抑菌圈直径,以抗菌区域直径的大小来初步评估分析实验牙膏的抗菌潜力,“-”表示抑菌圈小于1mm,样品没有抑菌能力,其中膏体的稀释浓度分别为20、40、80、160、320mg/ml,实验结果见表5。
表5:牙膏的体外抑菌试验结果
3.牙膏药效试验如下
随机选25名患者进行试牙膏药效学试验,受试者均是口腔炎症患者,男女不限,年龄22岁至48岁之间,使用周期为25天,对全部受试者进行刷牙方法指导。受试者使用统一的牙刷及指定的牙膏,要求用巴氏刷牙法每天刷牙2次(早7:00-9:00、晚7:30-9:30),每次至少2分钟,刷牙时使用牙膏膏体以2克为准。要求试验过程中不使用其它任何口腔卫生用品,如其它种类的牙膏、漱口水、牙线等。对饮食不限制,统计结果见表6。
表6:含神秘果提取物荷叶提取物牙膏药效学试验结果
由上可见,本发明制得的牙膏对牙菌斑、牙龈肿痛、口腔异味有显著的改善作用。因此,本发明的牙膏可用于防治牙周炎、牙龈炎和口腔炎、口腔溃疡等,从而减少口腔疾病。
神秘果的果肉含有大量的醣蛋白存在,同时其中的维生素C、KI、柠檬酸、琥珀酸、草酸等营养物质非常丰富,对于人体有好处,而且在神秘果的种子中也是含有天然固醇等成分存在的,神秘果的叶子中含有大量的钠、钾、钙、镁等微量矿物元素,对于人体非常重要。
荷叶相对其它常见中草药对抑制龋病及牙周病相关的细菌具有更好的效能以及更低的成本。牙周病通常被视为一种慢性炎症性疾病,多种细菌在疾病形成中发挥作用。这些细菌较常见的包括伴放线放线杆菌、黏性放线菌、牙龈卟啉单胞菌、具核梭杆菌、内氏放线菌等。研究发现荷叶中多种成分能不同程度地抑制牙周常见致病菌。首先荷叶醇类提取物对于牙周致病菌具有较稳定的抑制作用。荷叶醇类提取物黄酮中的槲皮素、金丝桃苷、紫云英苷能有效抑制上述五种常见牙周致病菌,确定其能有效治疗牙龈炎、牙周炎等口腔疾病。
上面对本发明的实施方式作了详细说明,但是本发明并不限于此,在所属技术领域的技术人员所具备的知识范围内,在不脱离本发明宗旨的前提下还可以作出各种变化。
Claims (10)
1.一种含有神秘果荷叶提取物的牙膏,其特征在于,按重量份数计包含以下组分:
神秘果提取物0.5-1份;荷叶提取物0.5-1份;润湿剂10-30份;摩擦剂15-45份;发泡剂0.5-1.5份;粘合剂0.4-1.6份;稳定剂0.15-0.3份;甜味剂0.2-0.8份。
2.根据权利要求1所述的一种含有神秘果荷叶提取物的牙膏,其特征在于,荷叶提取物与神秘果提取物比例为2∶1。
3.根据权利要求1所述的一种含有神秘果荷叶提取物的牙膏,其特征在于,神秘果提取物的制备步骤如下:
S11、将神秘果枝叶粉碎,得提取原料;
S12、加入乙醇水溶液,回流提取2~5小时,过滤,上清液减压蒸馏,冷冻干燥,得枝叶粗提取物干粉溶于水中,经大孔吸附树脂处理,然后用乙醇水溶液洗脱,得到收集液分别进行真空浓缩,冷冻干燥得精制枝叶提取物,提取物含总酚66.5%,枝提取物含总酚84.1%,即为神秘果提取物。
4.根据权利要求3所述的一种含有神秘果荷叶提取物的牙膏,其特征在于,乙醇为含水乙醇,为75%乙醇。
5.根据权利要求1-4任一项所述的一种含有神秘果荷叶提取物的牙膏,其特征在于,润湿剂为丙二醇、山梨醇、甘油、丙三醇和聚乙二醇中的一种或几种;摩擦剂为磷酸氢钙、二氧化硅、碳酸钙、氢氧化铝、重质碳酸钙和轻质碳酸钙中的一种或几种;发泡剂为十二醇硫酸钠、十二烷基硫酸钠、N-月桂酰肌氨酸钠、甲基椰油酰基牛磺酸钠中的一种或几种;粘合剂包括海藻酸钠、羟甲基纤维素钠、黄原胶、羟乙基纤维素、瓜尔胶、阿拉伯胶和卡拉胶中的一种或几种。
6.根据权利要求1所述的一种含有神秘果荷叶提取物的牙膏,其特征在于,甜味剂为糖精钠、蔗糖、木糖醇、甜蜜素和阿斯巴甜中的一种或几种。
7.一种根据权利要求1所述的含有神秘果荷叶提取物的牙膏的制备方法,其特征在于,包括以下步骤:
S21、将神秘果提取物与荷叶提取物、润湿剂、发泡剂和稳定剂溶解在水中,混合后加热,使制成的胶体呈均匀半透明粘状液态,然后放置,待其溶化膨胀后使用;
S22、将步骤S21所得胶体冷却至50-90℃,依次加入摩擦剂、粘合剂和甜味剂,继续搅拌;
S23、待胶体冷却至45℃以下,加入其余助剂,搅拌,制成膏体;
S24、将膏体研磨,然后真空脱气,静置,灭菌后即得牙膏成品。
8.根据权利要求7所述的一种含有神秘果荷叶提取物的牙膏的制备方法,其特征在于,S21中,混合过程在混料机中进行;加热过程在共沸锅中进行,加热至75-100℃,放置1-2h。
9.根据权利要求8所述的一种含有神秘果荷叶提取物的牙膏的制备方法,其特征在于,S22中,胶体冷却至65-70℃;加入摩擦剂、粘合剂和甜味剂时在搅拌下进行,搅拌的转速为300-320r/min;继续搅拌的时间为l-2h,转速为350-360r/min。
10.根据权利要求7-9任一项所述的一种含有神秘果荷叶提取物的牙膏的制备方法,其特征在于,S24中,研磨通过研磨机进行,研磨分二次进行,第一次研磨后贮存,第二次研磨后进行真空脱气,脱气到真空度达到-0.093MPa以下为止;静置的时间为2-4h。
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