[go: up one dir, main page]
More Web Proxy on the site http://driver.im/

WO2020000771A1 - 一种竹醋牙膏及其制备方法 - Google Patents

一种竹醋牙膏及其制备方法 Download PDF

Info

Publication number
WO2020000771A1
WO2020000771A1 PCT/CN2018/109891 CN2018109891W WO2020000771A1 WO 2020000771 A1 WO2020000771 A1 WO 2020000771A1 CN 2018109891 W CN2018109891 W CN 2018109891W WO 2020000771 A1 WO2020000771 A1 WO 2020000771A1
Authority
WO
WIPO (PCT)
Prior art keywords
toothpaste
bamboo vinegar
add
sodium
silica
Prior art date
Application number
PCT/CN2018/109891
Other languages
English (en)
French (fr)
Inventor
林创有
Original Assignee
三椒口腔健康股份有限公司
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 三椒口腔健康股份有限公司 filed Critical 三椒口腔健康股份有限公司
Publication of WO2020000771A1 publication Critical patent/WO2020000771A1/zh

Links

Classifications

    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9783—Angiosperms [Magnoliophyta]
    • A61K8/9794—Liliopsida [monocotyledons]
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/25—Silicon; Compounds thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73—Polysaccharides
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P1/00—Drugs for disorders of the alimentary tract or the digestive system
    • A61P1/02—Stomatological preparations, e.g. drugs for caries, aphtae, periodontitis
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P31/00—Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
    • A61P31/02—Local antiseptics
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q11/00—Preparations for care of the teeth, of the oral cavity or of dentures; Dentifrices, e.g. toothpastes; Mouth rinses
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/20—Chemical, physico-chemical or functional or structural properties of the composition as a whole
    • A61K2800/26—Optical properties
    • A61K2800/262—Transparent; Translucent

Definitions

  • the invention belongs to the technical field of oral cleaning products, and particularly relates to bamboo vinegar toothpaste and a preparation method thereof.
  • Toothpaste is a cleaning product commonly used in daily life and has a long history. With the continuous development of science and technology, the continuous improvement and improvement of process equipment, various types of toothpaste have come out one after the other, and the quality and grade of products have been continuously improved. Now the type of toothpaste has developed from a single clean toothpaste to a full range and diverse functions. With hundreds of brands of multifunctional toothpaste, it meets the needs of different levels of consumption.
  • Toothpaste is usually prepared with abrasives, humectants, foaming agents, thickeners, adhesives, sweeteners, flavors, and water.
  • Sodium lauryl sulfate is an excellent anionic surfactant.
  • foaming agent As the most commonly used foaming agent in toothpaste, it is one of the important raw materials for toothpaste production. It gives toothpaste a good foaming ability and also emulsifies. And cleaning and decontamination effect.
  • sodium lauryl sulfate has certain irritation to the oral cavity. In order to reduce irritation, technicians generally reduce the amount of sodium lauryl sulfate or do not choose sodium lauryl sulfate, or use more mild compounding properties. Foaming agent (such as sodium lauroyl sarcosinate) to reduce oral irritation. In addition, sodium lauryl sulfate can cause the low-temperature coarsening of silica toothpaste.
  • Existing research indicates that peppermint flavor, propylene glycol, PEG-8, and PEG-32 can solubilize sodium lauryl sulfate, so Can solve the problem of low temperature coarsening of silicon dioxide toothpaste (Liao Hai. Study on low temperature coarsening of silicon dioxide toothpaste [J]. Oral Care Products Industry, 2011, 3: 14-17).
  • bamboo vinegar is a by-product of the pyrolysis of bamboo. It is a dark reddish brown liquid with a special smoky flavor. Its composition is quite complex, up to more than 200 types, and it changes continuously with different collection methods and storage conditions.
  • the main component of bamboo vinegar solution is water (about 80%), followed by organic acids, phenols, ketones, alcohols and so on.
  • the bamboo vinegar stock solution needs to be separated, decolorized and refined to suit different purposes. Due to the complex characteristics of bamboo vinegar solution, bamboo vinegar solution is widely used. At present, bamboo vinegar solution has been used in food, agriculture, medicine and daily chemical fields, including daily necessities such as toothpaste and mouthwash. And research has confirmed that the refined bamboo vinegar solution is safe and reliable in contact with human and animal skin and used orally and nasally.
  • patent document CN104606103A discloses an oral odor-removing toothpaste.
  • the toothpaste contains 70% sorbitol 63-70%, red zeolite powder 0.1-5.0%, bamboo vinegar liquid 2.0-5.0, artemisia oil 0.8-1.0%, friction Type silica 9-13%, thickened silica 2.0%, sodium lauryl sulfate 2.0%, sodium carboxymethyl cellulose 0.95%, polyethylene glycol 0.7%, saccharin sodium 0.30%, sodium benzoate 0.3 %, Sodium dihydrogen phosphate 0.15%, trisodium phosphate 0.25%, pigment 0.0025% and water balance.
  • the toothpaste can improve the breath freshness and extend the breath freshness time.
  • the toothpaste contains bamboo vinegar and artemisinin oil, which complicates the toothpaste system, causing the toothpaste to return to low temperature at the same time.
  • the acidity of the bamboo vinegar is strong, which will also stimulate the mouth .
  • Pullulan is a linear homopolysaccharide composed of glucose residues. It is water-soluble, edible, film-forming, and gas-barrier. Therefore, it is used as an adhesive and capsule material in the pharmaceutical industry and in the food industry. As a film-forming agent, filler, etc., it has a wide range of application prospects.
  • Patent document CN 106420552A discloses a toothpaste including 52-53% sorbitol, 14-16% eggshell powder, 1.5-2.5% glycerol, 1.2-1.4% sodium lauryl sulfate, and xylitol 2.5-3.5%, pullulan polysaccharide 1.4-1.6%, propolis extract 1-1.5%, honeysuckle extract 1.8-2.2%, ethylenediamine tetraacetic acid disodium 0.08-0.12%, sodium benzoate 0.04-0.06%, Nisin 0.08-0.12%, the balance is deionized water.
  • nisin, sodium benzoate and pullulan in the toothpaste forms a multi-functional film of "sterilization + moisturizing + antibacterial", which is attached to the surface layer of teeth and oral mucosa, which reduces the abrasion of dental enamel and oral mucosa during brushing. It also plays an effective role in killing the bacteria that cause infections in the damaged area, thereby playing an anti-caries role.
  • the toothpaste also has a low-temperature coarsening phenomenon, which affects its quality, and the toothpaste has a low transparency.
  • the present invention provides a bamboo vinegar toothpaste, the toothpaste It is safe, mild, and low-irritant, and the paste is transparent, smooth, and delicate, with abundant foam, effective antibacterial, removing oral odor, and has a good oral cleaning and nursing effect.
  • the bamboo vinegar toothpaste provided by the present invention includes the following raw materials in weight percent: humectant 60 to 65%, sucralose 0.01 to 0.1%, friction silica 4 to 6%, thickened silica 8 to 12 %, Sodium carboxymethylcellulose 0.5 to 1%, sodium lauryl sulfate 2 to 3%, betaine 0.1 to 0.4%, bamboo vinegar solution 4 to 6%, pullulan polysaccharide 2 to 5%, xanthan Gum 0.1 to 0.3%, flavor 0.5 to 1%, menthol 0.2 to 0.5%, pigment 0.001%, preservative 0.3%, water 6 to 12%.
  • the bamboo vinegar toothpaste of the present invention is prepared from the following weight percentages of raw materials: humectant 62%, sucralose 0.05%, friction silica 5%, thickened silica 10 %, Sodium carboxymethylcellulose 1%, sodium lauryl sulfate 2%, betaine 0.3%, bamboo vinegar solution 5%, pullulan polysaccharide 3%, xanthan gum 0.2%, flavor 0.8%, menthol 0.3%, pigment 0.001%, preservative 0.3%, the balance is water.
  • the humectant is a combination of polyethylene glycol and sorbitol.
  • the polyethylene glycol is polyethylene glycol-400.
  • the fragrance is a bamboo fragrance.
  • the preservative is sodium benzoate.
  • the pigment is a fruit green pigment.
  • the bamboo vinegar solution is a refined bamboo vinegar solution.
  • the present invention also provides a method for preparing the bamboo vinegar toothpaste, which specifically includes the following steps:
  • premix solution A Take the formula amount of water and add it to premix pot A, and then add the formula amount of pullulan, sucralose, betaine, and bamboo vinegar solution, stir until completely dissolved, and prepare premix solution A for use;
  • the obtained paste is subjected to vacuum degassing, the degree of vacuum is -0.098 MPa, and the time is 45 to 65 min. After the degassing, the paste is left for 2 days and divided into packages to obtain bamboo vinegar toothpaste.
  • composition of the present invention is as follows: during the research, the inventor found that the existing toothpaste containing bamboo vinegar liquid will return to a low temperature when it is stored at a low temperature of 15 ° C, even if mint flavor, propylene glycol and polyethylene glycol are used Such problems still exist as a solubilizer. At the same time, the addition of bamboo vinegar solution also reduces the amount of foam in the toothpaste. It is speculated that this is due to the complex composition of the bamboo vinegar solution and the strong acidity, which leads to the decline in toothpaste stability and foam. The amount is reduced.
  • the inventor introduced pullulan polysaccharide in the toothpaste, using the long-chain molecular structure of pullulan polysaccharide , Attached to the oral mucosa and tooth surface, thereby reducing the irritation of the oral cavity by sodium lauryl sulfate.
  • the amount of pullulan in toothpaste needs to be higher than 1% to have a more obvious anti-irritant effect, but the introduction of pullulan alone without bamboo vinegar solution will cause a paste at 1%
  • the decrease in transparency affects the appearance of the toothpaste. It is speculated that this is due to the highly ordered structure of the pullulan polysaccharide molecule itself. At the same time, these macromolecules form a cross-network structure and repeatedly wrap the particles in the toothpaste, causing a decrease in transparency.
  • the inventor introduced pullulan polysaccharide and bamboo vinegar solution into the silica toothpaste at the same time. It was unexpectedly found that after the blend of pullulan polysaccharide and bamboo vinegar liquid, the toothpaste had excellent transparency, and the paste was smooth and delicate, and it became a strip. Good performance, rich foam volume, and no low temperature back to coarse, and can effectively reduce toothpaste irritation to the mouth. It is speculated that this is due to the network structure formed by pullulan macromolecules combined with the network structure formed by silica, which makes it difficult for the microparticles to move around, which significantly enhances the stability of the system and solves the low temperature return of silica toothpaste.
  • pullulan has the function of stabilizing foam.
  • pullulan After foaming agent foaming, pullulan can effectively improve foam stability and restrict the defoaming effect of bamboo vinegar solution; bamboo vinegar liquid on the one hand brings antibacterial and refreshing oral effects, on the other hand it also plays a regulating role, making the paste transparent and moderate viscosity.
  • the bamboo vinegar toothpaste of the present invention can effectively reduce the oral irritation caused by the foaming agent sodium lauryl sulfate and bamboo vinegar solution, protect the oral mucosa, be safe, mild, and low irritant, can effectively antibacterial, remove oral odor,
  • the mouth is refreshing and has good oral cleaning and nursing effects.
  • the light green paste is transparent, smooth, delicate, moderate in consistency, rich in foam, and has a light bamboo fragrance, which can bring consumers a pleasant sense and use experience.
  • the raw materials of the bamboo vinegar toothpaste of the invention are easy to obtain, the formula is simple, the system is stable, and the shelf life is long; the preparation process is stable, the conditions are controllable, the production cost is low, it can be industrialized and can be promoted and applied.
  • the raw materials mentioned in the present invention are all conventional commercial products.
  • refined bamboo vinegar solution was purchased from Jiangyin Zhongju Biological Technology Co., Ltd .
  • bamboo fragrance essence was purchased from Guangzhou Tufu Spice Technology Co., Ltd., article number: TF10193 (commercial name: refreshing bamboo fragrance).
  • Flavor Fruit green pigment was purchased from Xiaolan Guanqiu Trading Co., Ltd., trade name: Fruit Green.
  • Example 1 Example 2
  • Example 3 Example 4 70% sorbitol 58kg 60kg 60kg 60kg PEG-400 4kg 3kg 2kg 2kg Sucralose 0.01kg 0.1kg 0.05kg 0.05kg Friction silica 4kg 6kg 5kg 5kg Thickened silica 12kg 8kg 10kg 10kg Sodium carboxymethyl cellulose 0.5kg 1kg 1kg 1kg Sodium dodecyl sulfate 2kg 2kg 2kg 2kg 2kg Betaine 0.1kg 0.4kg 0.3kg 0.3kg Refined bamboo vinegar 4kg 6kg 4kg 5kg Pullulan 2kg 5kg 5kg 3kg Xanthan Gum 0.1kg 0.3kg 0.2kg 0.2kg
  • the method for preparing bamboo vinegar toothpaste of Examples 1 to 4 is as follows:
  • premix solution A Take the formula amount of water and add it to premix pot A, and then add the formula amount of pullulan, sucralose, betaine, and refined bamboo vinegar solution, stir until completely dissolved to prepare premix solution A, and set aside;
  • Premix B Take the formulated amount of 70% sorbitol and polyethylene glycol-400 and add it to the premixing pot B, then add the formulated amounts of sodium methylcellulose sodium and xanthan gum, and stir until completely dissolved and dispersed to obtain Premix B, ready for use;
  • the obtained paste is subjected to vacuum degassing, the degree of vacuum is -0.098 MPa, and the time is 60 minutes. After degassing, the paste is allowed to stand for 2 days and then divided into packages to obtain bamboo vinegar toothpaste.
  • Test example 1 physical and chemical index detection of bamboo vinegar toothpaste of the present invention
  • the bamboo vinegar toothpaste of Examples 1 to 4 all meet the requirements of GB / T8372 toothpaste standard, and the light green paste is transparent, smooth, delicate, moderate in consistency, rich in foam, with a light bamboo fragrance, and can bring Consumers' pleasing senses and feelings of use; At the same time, the bamboo vinegar toothpaste of Examples 1 to 4 of the present invention has shown good stability through low-temperature and high-temperature tests. It does not show coarseness at low temperatures and no water separation at high temperatures Phenomenon, appearance, pH value, consistency and other physical and chemical indicators are all normal.
  • Test Example 2 Study on the in vitro cytotoxicity of the bamboo vinegar toothpaste of the present invention
  • Examples 1 to 4 and toothpastes of Comparative Examples 1-3; human oral mucosal fibroblasts (homf), Shanghai Baili Biotechnology Co., Ltd .; DMEM / F12 cell culture solution (with 10% fetal bovine serum, 100U / mL penicillin , 100U / mL streptomycin), phosphate buffer solution (PBS, pH 7.4), trypsin, MTT (3- (4,5-dimethylthiazole-2) -2,5-diphenyltetrazolium Bromide), dimethyl sulfoxide (DMSO).
  • trypsin MTT (3- (4,5-dimethylthiazole-2) -2,5-diphenyltetrazolium Bromide
  • DMSO dimethyl sulfoxide
  • RGR relative cell proliferation rate
  • the MTT method was used to test the cytotoxicity of various toothpaste extracts.
  • the OD values obtained from the test of each group of toothpaste extracts, and the calculated RGR values and cytotoxicity grade results are shown in Table 5 below.
  • Toothpaste extract OD value RGR value (%, x ⁇ s) Cytotoxic grade Example 1 0.771 ⁇ 0.068 87.25 ⁇ 5.92 1
  • Example 2 0.763 ⁇ 0.060 86.32 ⁇ 6.64 1
  • Example 3 0.796 ⁇ 0.063 90.07 ⁇ 6.83 1
  • Example 4 0.821 ⁇ 0.065 92.86 ⁇ 6.90 1 Comparative Example One 0.101 ⁇ 0.053 10.60 ⁇ 4.21 4 Comparative Example Two 0.075 ⁇ 0.044 8.37 ⁇ 5.36 4 Comparative Example Three 0.842 ⁇ 0.062 95.27 ⁇ 7.12 1 Negative control 0.883 ⁇ 0.067 100 0
  • the cytotoxicity of the bamboo vinegar toothpaste extracts of Examples 1 to 4 of the present invention is grade 1, suggesting that the toothpaste of the present invention is less toxic to oral cells, and therefore has less irritation to human oral mucosa.
  • the RGR value of Example 4 is the highest, so Example 4 is the best embodiment of the present invention.
  • Comparative Example 1 does not contain pullulan and bamboo vinegar solution (that is, a general toothpaste formula), and Comparative Example 2 contains only bamboo vinegar solution.
  • the cytotoxicity of both toothpaste extracts is Level 4 reflects that the toothpaste has greater irritation to the oral mucosa; Comparative Example 3 only contains pullulan polysaccharide, and the cytotoxicity of the toothpaste extract is Grade 1, suggesting that pullulan can effectively reduce Oral cells are toxic, which reduces the irritation of oral mucosa by toothpaste.

Landscapes

  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Veterinary Medicine (AREA)
  • Public Health (AREA)
  • General Health & Medical Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • Birds (AREA)
  • Chemical & Material Sciences (AREA)
  • Epidemiology (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Medicinal Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oncology (AREA)
  • Microbiology (AREA)
  • Botany (AREA)
  • Mycology (AREA)
  • Communicable Diseases (AREA)
  • Biotechnology (AREA)
  • Inorganic Chemistry (AREA)
  • Oral & Maxillofacial Surgery (AREA)
  • Bioinformatics & Cheminformatics (AREA)
  • Cosmetics (AREA)

Abstract

本发明属于口腔清洁用品技术领域，具体涉及一种竹醋牙膏，该牙膏包括以下重量百分比计的制备原料：保湿剂60～65％、三氯蔗糖0.01～0.1％、磨擦型二氧化硅4～6％、增稠型二氧化硅8～12％、羧甲基纤维素钠0.5～1％、十二烷基硫酸钠2～3％、甜菜碱0.1～0.4％、竹醋液4～6％、普鲁兰多糖2～5％、黄原胶0.1～0.3％、香精0.5～1％、薄荷脑0.2～0.5％、色素0.001％、防腐剂0.3％、水6～12％。本发明牙膏安全、温和、低刺激，且膏体透明、光洁、细腻，泡沫量丰富，有效抗菌、去除口腔异味，具有良好的口腔清洁护理效果。

Description

一种竹醋牙膏及其制备方法 技术领域
本发明属于口腔清洁用品技术领域，具体涉及一种竹醋牙膏及其制备方法。
背景技术
牙膏是日常生活中常用的清洁用品，有着很悠久的历史。随着科学技术的不断发展，工艺装备的不断改进和完善，各种类型的牙膏相继问世，产品的质量和档次不断提高，现在牙膏品种已由单一的清洁型牙膏，发展成为品种齐全、功能多样，上百个品牌的多功能型牙膏，满足了不同层次消费水平的需要。
牙膏通常是以磨擦剂、保湿剂、发泡剂、增稠剂、粘合剂、甜味剂、香精和水等制备而成。十二烷基硫酸钠是一种优良的阴离子表面活性剂，作为牙膏中最常用的发泡剂，是牙膏生产的重要原料之一，其赋予牙膏具有良好的发泡能力，同时也起到乳化和清洁去污的作用。
但是，十二烷基硫酸钠对口腔有一定的刺激，为了降低刺激性，技术人员一般会减少十二烷基硫酸钠的用量或不选用十二烷基硫酸钠，或复配选用性能更温和的发泡剂(如月桂酰肌氨酸钠)，以减轻对口腔的刺激。此外，十二烷基硫酸钠还会引起二氧化硅牙膏的低温返粗现象，现有研究指出薄荷香精、丙二醇、PEG-8、PEG-32对十二烷基硫酸钠有增溶作用，因而可以解决二氧化硅牙膏的低温返粗现象(廖海.二氧化硅牙膏低温返粗的研究[J].口腔护理用品工业，2011,3：14-17)。
竹醋液是竹材热解得到的副产品，是一种有特殊烟熏味的深红褐色液体，其成分相当复杂，多达200多种，并且随收集方法，贮存条件等不同而不断变化。竹醋液的主要成分是水(约占80％)，其次是有机酸、酚类、酮类、醇类等。竹醋原液需进行分离脱色精制，以合适不同的用途。由于竹醋液成分复杂的特征决定了竹醋液的用途相当广泛。目前，竹醋液已应用于食品、农业、医药和日化领域中，具体包括牙膏、漱口水等日用品。并且研究证实了精制竹醋液接触人和动物皮肤及经口、鼻使用是安全可靠的，因此，含精制竹醋液的漱口水有着良好的应用前景。如专利文献CN104606103A公开了一种除口腔异味牙膏，该牙膏含有70％山梨醇63-70％、红辉沸石粉0.1-5.0％、竹醋液2.0-5.0、青蒿油0.8-1.0％、磨擦型二氧化硅9-13％、增稠型二氧化硅2.0％、十二醇硫酸钠2.0％、羧甲基纤维素钠0.95％、聚乙二醇0.7％、糖精钠0.30％、苯甲酸钠0.3％、磷酸二氢钠0.15％、磷酸三钠0.25％、色素0.0025％ 和水余量。该牙膏能提高口气清新度及延长口气清新时间，可是该牙膏由于含有竹醋液和青蒿油，造成牙膏体系复杂，导致牙膏低温返粗，同时竹醋液的酸性较强，同样会刺激口腔。
普鲁兰多糖是由葡萄糖残基组成的直链状同型多聚糖，具有水溶性、可食用性、成膜性、阻气性，因此在医药行业作为胶黏剂、胶囊材料，在食品行业作为成膜剂、填充剂等，具有广泛的应用前景。专利文献CN 106420552A公开了一种牙膏，该牙膏包括山梨(糖)醇52-53％、蛋壳粉14-16％、甘油1.5-2.5％、月桂醇硫酸酯钠1.2-1.4％、木糖醇2.5-3.5％、普鲁兰多糖1.4-1.6％、蜂胶提取物1-1.5％、忍冬花提取物1.8-2.2％、乙二胺四乙酸二钠0.08-0.12％、苯甲酸钠0.04-0.06％、乳链菌肽0.08-0.12％，余量为去离子水。该牙膏中乳链菌肽、苯甲酸钠和普鲁兰多糖联合，形成了“杀菌+保湿+抗菌”的多重功效薄膜，附着在牙齿和口腔黏膜表层，既降低了刷牙时对牙釉质和口腔黏膜的磨损，对引起破损处感染的细菌也起到有效杀灭的作用，从而起到抗龋的作用。然而该牙膏也存在低温返粗现象，影响了其品质，并且该牙膏的透明度较低。
发明内容
为了解决现有技术存在的问题(如表面活性剂十二烷基硫酸钠对口腔的刺激性大，膏体稳定性较差、透明度低等)，本发明提供了一种竹醋牙膏，该牙膏安全、温和、低刺激，且膏体透明、光洁、细腻，泡沫量丰富，有效抗菌、去除口腔异味，具有良好的口腔清洁护理效果。
本发明提供的竹醋牙膏包括以下重量百分比计的制备原料：保湿剂60～65％、三氯蔗糖0.01～0.1％、磨擦型二氧化硅4～6％、增稠型二氧化硅8～12％、羧甲基纤维素钠0.5～1％、十二烷基硫酸钠2～3％、甜菜碱0.1～0.4％、竹醋液4～6％、普鲁兰多糖2～5％、黄原胶0.1～0.3％、香精0.5～1％、薄荷脑0.2～0.5％、色素0.001％、防腐剂0.3％、水6～12％。
作为本发明优选的实施方式，本发明竹醋牙膏由以下重量百分比计的原料制备而成：保湿剂62％、三氯蔗糖0.05％、磨擦型二氧化硅5％、增稠型二氧化硅10％、羧甲基纤维素钠1％、十二烷基硫酸钠2％、甜菜碱0.3％、竹醋液5％、普鲁兰多糖3％、黄原胶0.2％、香精0.8％、薄荷脑0.3％、色素0.001％、防腐剂0.3％，余量为水。
优选地，所述保湿剂为聚乙二醇和山梨醇的组合物。
优选地，所述聚乙二醇为聚乙二醇-400。
优选地，所述香精为竹香香精。
优选地，所述防腐剂为苯甲酸钠。
优选地，所述色素为果绿色素。
优选地，所述竹醋液为精制竹醋液。
相应地，本发明还提供了上述竹醋牙膏的制备方法，具体包括以下步骤：
S1、取配方量的水加入到预混锅A中，接着加入配方量的普鲁兰多糖、三氯蔗糖、甜菜碱和竹醋液，搅拌至完全溶解，制得预混液A，备用；
S2、取配方量的保湿剂加入到预混锅B中，接着加入配方量的羟甲基纤维素钠、黄原胶，搅拌至完全溶解、分散，制得预混液B，备用；
S3、往预混液A中加入预混液B，搅拌至均匀，再加入配方量的磨擦型二氧化硅、增稠型二氧化硅，搅拌至均匀，最后加入配方量的十二烷基硫酸钠、香精、薄荷脑、色素和防腐剂，搅拌至均匀，制得膏体；
S4、所得膏体进行真空脱气，真空度为-0.098MPa，时间为45～65min，脱气后膏体静置2天，分装，即得竹醋牙膏。
本发明的组方构思如下：发明人在研究时发现，现有含有竹醋液的牙膏，在低温15℃下贮存时会出现低温返粗现象，即使使用了薄荷香精、丙二醇和聚乙二醇等作为增溶剂，仍会存在这样的问题，同时，竹醋液的加入也使得牙膏的泡沫量降低，推测这是由于竹醋液的成分复杂，以及酸性较强，导致牙膏稳定性下降，泡沫量减少。
另一方面，为了降低十二烷基硫酸钠对口腔的刺激性，同时不影响牙膏的清洁去污能力，发明人在牙膏中引入了普鲁兰多糖，利用普鲁兰多糖的长链分子结构，附着于口腔黏膜和牙齿表面，从而降低十二烷基硫酸钠对口腔的刺激性。普鲁兰多糖在牙膏中的用量需高于1％才有较明显的降刺激效果，但是在不含竹醋液的情况下单独引入普鲁兰多糖，在1％用量下会引起了膏体透明度下降，影响了牙膏外观，推测这是由于普鲁兰多糖分子自身的结构高度有序，同时这些大分子之间形成交叉网状结构，并且反复包裹牙膏中的微粒，引起透明度的下降。
于是，发明人在二氧化硅牙膏中同时引入了普鲁兰多糖和竹醋液，意外地发现，普鲁兰多糖和竹醋液复配后，牙膏透明度极好，膏体光洁细腻，成条性好，泡沫量丰富，并且不会发生低温返粗现象，还能有效降低牙膏对口腔的刺激。推测这是由于普鲁兰多糖大分子形成的网状结构结合二氧化硅形成的网状结构，使包裹的微粒难以发生位置移动，显著增强了体系稳定性，解决了二氧化硅牙膏的低温返粗现象，同时普鲁兰多糖大分子的网状结构具有稳泡的作用，发泡剂发泡后，普鲁兰多糖能有效提高泡沫稳定性，制约竹醋液带来的消泡作用；而竹醋液一方面带来抗菌、清新口腔的效果，另一方面也起到调节作用，使膏体透明，粘稠 度适中。
因此，与现有技术相比，本发明的优势在于：
(1)本发明竹醋牙膏能够有效降低发泡剂十二烷基硫酸钠与竹醋液带来的口腔刺激，保护口腔黏膜，安全、温和、低刺激，能有效抗菌、去除口腔异味，使口腔清爽，具有良好的口腔清洁护理效果；同时浅绿色的膏体透明、光洁、细腻，稠度适中，泡沫量丰富，带有淡淡的竹子清香，能够给消费者带来愉悦的感官和使用感受。
(2)本发明竹醋牙膏的原料易得，配方简单，体系稳定，货架期长；制备工艺稳定，条件可控，生产成本较低，能工业化生产，可推广应用。
具体实施方式
下面通过具体实施例对本发明做进一步的详细说明。
本发明所述原料均为常规市售商品，例如精制竹醋液购自江阴中炬生物科技有限公司；竹香香精购自广州途富香料科技有限公司，货号：TF10193(商品名：清爽竹香香精)；果绿色素购自小榄冠球贸易有限公司，商品名：果绿。
实施例1～4、本发明竹醋牙膏及其制备
实施例1～4竹醋牙膏的配方如下表1：
表1
原料 实施例1 实施例2 实施例3 实施例4
70％山梨醇 58kg 60kg 60kg 60kg
聚乙二醇-400 4kg 3kg 2kg 2kg
三氯蔗糖 0.01kg 0.1kg 0.05kg 0.05kg
磨擦型二氧化硅 4kg 6kg 5kg 5kg
增稠型二氧化硅 12kg 8kg 10kg 10kg
羧甲基纤维素钠 0.5kg 1kg 1kg 1kg
十二烷基硫酸钠 2kg 2kg 2kg 2kg
甜菜碱 0.1kg 0.4kg 0.3kg 0.3kg
精制竹醋液 4kg 6kg 4kg 5kg
普鲁兰多糖 2kg 5kg 5kg 3kg
黄原胶 0.1kg 0.3kg 0.2kg 0.2kg
竹香香精 1kg 0.5kg 0.8kg 0.8kg
薄荷脑 0.2kg 0.5kg 0.4kg 0.3kg
果绿色素 0.001kg 0.001kg 0.001kg 0.001kg
苯甲酸钠 0.3kg 0.3kg 0.3kg 0.3kg
水 补足100kg 补足100kg 补足100kg 补足100kg
实施例1～4竹醋牙膏的制备方法如下：
S1、取配方量的水加入到预混锅A中，接着加入配方量的普鲁兰多糖、三氯蔗糖、甜菜碱和精制竹醋液，搅拌至完全溶解，制得预混液A，备用；
S2、取配方量的70％山梨醇、聚乙二醇-400加入到预混锅B中，接着加入配方量的羟甲基纤维素钠、黄原胶，搅拌至完全溶解、分散，制得预混液B，备用；
S3、往预混液A中加入预混液B，搅拌至均匀，再加入配方量的磨擦型二氧化硅、增稠型二氧化硅，搅拌至均匀，最后加入配方量的十二烷基硫酸钠、果绿色素、薄荷脑、竹香色素和苯甲酸钠，搅拌至均匀，制得膏体；
S4、所得膏体进行真空脱气，真空度为-0.098MPa，时间为60min，脱气后膏体静置2天，分装，即得竹醋牙膏。
对比例一～三的配方如下表2：
表2
原料 对比例一 对比例二 对比例三
70％山梨醇 60kg 60kg 60kg
聚乙二醇-400 2kg 2kg 2kg
三氯蔗糖 0.05kg 0.05kg 0.05kg
磨擦型二氧化硅 5kg 5kg 5kg
增稠型二氧化硅 10kg 10kg 10kg
羧甲基纤维素钠 1kg 1kg 1kg
十二烷基硫酸钠 2kg 2kg 2kg
甜菜碱 0.3kg 0.3kg 0.3kg
精制竹醋液 / 5kg /
普鲁兰多糖 / / 3kg
黄原胶 0.2kg 0.2kg 0.2kg
竹香香精 0.8kg 0.8kg 0.8kg
薄荷脑 0.3kg 0.3kg 0.3kg
果绿色素 0.001kg 0.001kg 0.001kg
苯甲酸钠 0.3kg 0.3kg 0.3kg
水 补足100kg 补足100kg 补足100kg
对比例一～三的制备方法参考实施例1～4。
试验例一、本发明竹醋牙膏的理化指标检测
根据GB/T 8372牙膏标准对实施例1～4和对比例一～三牙膏进行考察，并加检稠度和发泡量指标，具体结果见下表3。
表3各牙膏的理化指标检测结果
Figure PCTCN2018109891-appb-000001
Figure PCTCN2018109891-appb-000002
由上表3可知：
(1)实施例1～4竹醋牙膏均符合GB/T 8372牙膏标准要求，并且浅绿色的膏体透明、光洁、细腻，稠度适中，泡沫量丰富，带有淡淡的竹子清香，能够带给消费者愉悦的感官和使用感受；同时本发明实施例1～4竹醋牙膏通过低温和高温试验考察，表现出良好的稳定性，在低温时没有出现返粗现象，在高温时没有出现分水现象，外观、pH值、稠度等理化指标均表现正常。
(2)与对比例一相比，对比例二牙膏引入含竹醋液，其泡沫量显著降低，并且出现低温返粗现象；而对比例三牙膏引入普鲁兰多糖，其膏体透明度下降，同时膏体粘稠度较高。
试验例二、本发明竹醋牙膏的体外细胞毒性研究
(一)试验试剂：
实施例1～4和对比例一～三的牙膏；人口腔黏膜成纤维细胞(homf)，上海拜力生物科技有限公司；DMEM/F12细胞培养液(加入10％胎牛血清、100U/mL青霉素、100U/mL链霉素)、磷酸缓冲液(PBS，pH＝7.4)、胰蛋白酶，MTT(3-(4,5-二甲基噻唑-2)-2,5-二苯基四氮唑溴盐)，二甲亚砜(DMSO)。
(二)试验方法：
1、牙膏浸提液的制备：取实施例1～4和对比例一～三的牙膏，分别称取3.0g每种牙膏样品于10mLPBS中，摇晃混匀，常温下静置过夜，吸取上清液，用微孔滤器过滤除菌，得到牙膏浸提液。
2、使用MTT法测定牙膏浸提液的细胞毒性：将人口腔成纤维细胞制备成1×10 5个/mL的细胞悬液，按每孔200μL接种于96孔细胞培养板中，置于5％CO 2，37℃细胞培养箱内培养24h，弃去原培养液，每孔加180μL培养液和20μL牙膏浸提液，设3个平行孔，以加等量PBS作阴性对照，继续培养20h。然后每孔加5g/L的MTT溶液20μL，继续在37℃下培养4h后，吸弃原培养液。每孔加入200μLDMSO，室温下振荡10min后，用酶标仪在490nm波长下检测每孔的OD值，计算细胞相对增殖率(RGR)，公式如下：RGR＝实验组OD值/阴性对照组OD值×100％。
使用表4中的分级标准，根据RGR值对牙膏浸提液的细胞毒性进行分级。
表4细胞相对增殖率与细胞毒性分级的关系
Figure PCTCN2018109891-appb-000003
(三)试验结果：
使用MTT法对各种牙膏浸提液的细胞毒性进行测试，各组牙膏浸提液测试得到的OD值，进而计算得到的RGR值以及细胞毒性分级结果如下表5所示。
表5各种牙膏浸提液的检测结果
牙膏浸提液 OD值 RGR值(％，x±s) 细胞毒性分级
实施例1 0.771±0.068 87.25±5.92 1
实施例2 0.763±0.060 86.32±6.64 1
实施例3 0.796±0.063 90.07±6.83 1
实施例4 0.821±0.065 92.86±6.90 1
对比例一 0.101±0.053 10.60±4.21 4
对比例二 0.075±0.044 8.37±5.36 4
对比例三 0.842±0.062 95.27±7.12 1
阴性对照 0.883±0.067 100 0
由上表5可知：
(1)本发明实施例1～4竹醋牙膏浸提液的细胞毒性为1级，提示本发明牙膏对口腔细胞的毒性较小，因而对人口腔黏膜的刺激性较低。实施例1～4中，以实施例4的RGR值最高，因此实施例4为本发明的最佳实施例。
(2)与实施例4相比，对比例一不含有普鲁兰多糖和竹醋液(即为一般牙膏配方)，对比例二仅含竹醋液，两种牙膏浸提液的细胞毒性均为4级，反映该牙膏对口腔黏膜有较大的刺激性；对比例三仅含普鲁兰多糖，其牙膏浸提液的细胞毒性为1级，提示普鲁兰多糖可有效减轻牙膏原料对口腔细胞的毒性，从而降低牙膏对口腔黏膜的刺激。
以上内容是结合具体的优选实施方式对本发明所作的进一步详细说明，不能认定本发明的具体实施只局限于这些说明。对于本发明所属技术领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干简单推演或替换，都应当视为属于本发明的保护范围。

Claims (8)

  1. 一种竹醋牙膏，其特征在于，包括以下重量百分比计的制备原料：保湿剂60～65％、三氯蔗糖0.01～0.1％、磨擦型二氧化硅4～6％、增稠型二氧化硅8～12％、羧甲基纤维素钠0.5～1％、十二烷基硫酸钠2～3％、甜菜碱0.1～0.4％、竹醋液4～6％、普鲁兰多糖2～5％、黄原胶0.1～0.3％、香精0.5～1％、薄荷脑0.2～0.5％、色素0.001％、防腐剂0.3％、水6～12％。
  2. 根据权利要求1所述竹醋牙膏，其特征在于，由以下重量百分比计的原料制备而成：保湿剂62％、三氯蔗糖0.05％、磨擦型二氧化硅5％、增稠型二氧化硅10％、羧甲基纤维素钠1％、十二烷基硫酸钠2％、甜菜碱0.3％、竹醋液5％、普鲁兰多糖3％、黄原胶0.2％、香精0.8％、薄荷脑0.3％、色素0.001％、防腐剂0.3％，余量为水。
  3. 根据权利要求1或2所述竹醋牙膏，其特征在于，所述保湿剂为聚乙二醇和山梨醇的组合物。
  4. 根据权利要求1所述竹醋牙膏，其特征在于，所述聚乙二醇为聚乙二醇-400。
  5. 根据权利要求1或2所述竹醋牙膏，其特征在于，所述香精为竹香香精。
  6. 根据权利要求1或2所述竹醋牙膏，其特征在于，所述防腐剂为苯甲酸钠。
  7. 根据权利要求1或2所述竹醋牙膏，其特征在于，所述色素为果绿色素。
  8. 根据权利要求1～7任一所述竹醋牙膏的制备方法，其特征在于，包括以下步骤：
    S1、取配方量的水加入到预混锅A中，接着加入配方量的普鲁兰多糖、三氯蔗糖、甜菜碱和竹醋液，搅拌至完全溶解，制得预混液A，备用；
    S2、取配方量的保湿剂加入到预混锅B中，接着加入配方量的羟甲基纤维素钠、黄原胶，搅拌至完全溶解、分散，制得预混液B，备用；
    S3、往预混液A中加入预混液B，搅拌至均匀，再加入配方量的磨擦型二氧化硅、增稠型二氧化硅，搅拌至均匀，最后加入配方量的十二烷基硫酸钠、香精、薄荷脑、色素和防腐剂，搅拌至均匀，制得膏体；
    S4、所得膏体进行真空脱气，真空度为-0.098MPa，时间为45～65min，脱气后膏体静置2天，分装，即得竹醋牙膏。
PCT/CN2018/109891 2018-06-29 2018-10-11 一种竹醋牙膏及其制备方法 WO2020000771A1 (zh)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN201810714378.6A CN108743502B (zh) 2018-06-29 2018-06-29 一种竹醋牙膏及其制备方法
CN201810714378.6 2018-06-29

Publications (1)

Publication Number Publication Date
WO2020000771A1 true WO2020000771A1 (zh) 2020-01-02

Family

ID=63975660

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/CN2018/109891 WO2020000771A1 (zh) 2018-06-29 2018-10-11 一种竹醋牙膏及其制备方法

Country Status (2)

Country Link
CN (1) CN108743502B (zh)
WO (1) WO2020000771A1 (zh)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110840788B (zh) * 2019-11-27 2022-04-19 广东盐业健康产业发展有限公司 一种牙膏配方
CN111821218A (zh) * 2020-08-04 2020-10-27 安徽克菱保健科技有限公司 一种咀嚼发泡缓释牙膏片

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2012116768A (ja) * 2010-11-29 2012-06-21 Kao Corp 液体口腔用組成物
CN104606103A (zh) * 2015-01-26 2015-05-13 柳州师范高等专科学校 除口腔异味牙膏
CN104606102A (zh) * 2015-01-26 2015-05-13 柳州师范高等专科学校 除口臭牙膏
CN106176299A (zh) * 2016-09-18 2016-12-07 天津北洋百川生物技术有限公司 一种含聚谷氨酸的口腔护理牙膏及其制备方法
CN106420552A (zh) * 2016-08-31 2017-02-22 福建省梦娇兰日用化学品有限公司 一种含多种天然来源成分的儿童专用牙膏
CN108186491A (zh) * 2018-03-05 2018-06-22 三椒口腔健康股份有限公司 一种含竹醋液的漱口水及其制备方法

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105267234A (zh) * 2015-10-29 2016-01-27 山东省药学科学院 一种缓解口干症状的组合物及其制备方法

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2012116768A (ja) * 2010-11-29 2012-06-21 Kao Corp 液体口腔用組成物
CN104606103A (zh) * 2015-01-26 2015-05-13 柳州师范高等专科学校 除口腔异味牙膏
CN104606102A (zh) * 2015-01-26 2015-05-13 柳州师范高等专科学校 除口臭牙膏
CN106420552A (zh) * 2016-08-31 2017-02-22 福建省梦娇兰日用化学品有限公司 一种含多种天然来源成分的儿童专用牙膏
CN106176299A (zh) * 2016-09-18 2016-12-07 天津北洋百川生物技术有限公司 一种含聚谷氨酸的口腔护理牙膏及其制备方法
CN108186491A (zh) * 2018-03-05 2018-06-22 三椒口腔健康股份有限公司 一种含竹醋液的漱口水及其制备方法

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
LIU, SHAOYING ET AL.: "Effects of Pullulan on Rheological Properties of Toothpaste", FOOD AND DRUG, vol. 18, no. 06, 20 November 2016 (2016-11-20), pages 407 - 410, ISSN: 1672-979X *

Also Published As

Publication number Publication date
CN108743502A (zh) 2018-11-06
CN108743502B (zh) 2019-03-22

Similar Documents

Publication Publication Date Title
Abd Rahim et al. Comparative studies on the effect of crude aqueous (CA) and solvent (CM) extracts of clove on the cariogenic properties of Streptococcus mutans
TWI355945B (zh)
KR20140118279A (ko) 발효 포공영 추출물-함유 복합 생약재 추출물을 유효성분으로 함유하는 구강세정용 조성물
JP2000512660A (ja) 口腔衛生用製品のための抗菌剤
WO2020000771A1 (zh) 一种竹醋牙膏及其制备方法
EP3195870B1 (en) Agent for promoting growth of nonpathogenic oral indigenous bacteria and composition for oral use
KR101450098B1 (ko) 푸코이단을 유효성분으로 포함하는 구강 세정용 조성물
JPH03240721A (ja) 口腔用組成物
CN111956682A (zh) 一种用于口腔炎、牙龈炎等炎症的丁硼乳膏及其制备方法和应用
JP2018058795A (ja) 口腔用組成物、及びその製剤変色及び液分離の抑制方法
KR20120050104A (ko) 매스틱 추출물을 함유하는 치약 조성물 및 그 제조방법
WO2020087763A1 (zh) 一种6-氟咪唑并吡啶衍生物的用途
CN113101243B (zh) 口腔软组织细胞修复促进剂、口腔护理组合物及应用
US20040265247A1 (en) Mouth rinse composition
KR101295242B1 (ko) 구맥 추출물을 유효성분으로 함유하는 구강세균 억제용 항균 조성물
CN110840788B (zh) 一种牙膏配方
CN109044916A (zh) 一种蒲地蓝牙膏及其制备方法
KR101773227B1 (ko) 치마제 조성물
KR20190057727A (ko) 기호성이 향상된 기관지 건강 약리 조성물
WO2021079921A1 (ja) 口腔内の病原性細菌に対する生育抑制剤、口腔内の菌叢改善剤及び口腔用組成物
JP2001302480A (ja) チコリから活性化合物を溶媒抽出する方法
KR101011049B1 (ko) 알파-하이드록시산을 포함하며 가글 후 응고물이 형성되는 구강용 액상 조성물 및 치과구강용 제품
CN111617021A (zh) 抗口腔幽门螺杆菌的牙膏
WO2024016109A1 (zh) 茶活性物质口腔护理组合物及其制备方法
US11771644B1 (en) Whitening toothpaste capable of effectively removing dental plaque and tartar

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 18924483

Country of ref document: EP

Kind code of ref document: A1

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 18924483

Country of ref document: EP

Kind code of ref document: A1