WO2020062389A1 - 一种新会柑果皮萃取液制作牙膏的配方及工艺 - Google Patents

一种新会柑果皮萃取液制作牙膏的配方及工艺 Download PDF

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WO2020062389A1
WO2020062389A1 PCT/CN2018/112368 CN2018112368W WO2020062389A1 WO 2020062389 A1 WO2020062389 A1 WO 2020062389A1 CN 2018112368 W CN2018112368 W CN 2018112368W WO 2020062389 A1 WO2020062389 A1 WO 2020062389A1
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toothpaste
xinhui
peel extract
paste
making
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温伟成
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温伟成
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics 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
    • A61K8/9783Angiosperms [Magnoliophyta]
    • A61K8/9789Magnoliopsida [dicotyledons]
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/25Silicon; Compounds thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/34Alcohols
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/34Alcohols
    • A61K8/345Alcohols containing more than one hydroxy group
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/36Carboxylic acids; Salts or anhydrides thereof
    • A61K8/368Carboxylic acids; Salts or anhydrides thereof with carboxyl groups directly bound to carbon atoms of aromatic rings
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/46Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing sulfur
    • A61K8/463Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing sulfur containing sulfuric acid derivatives, e.g. sodium lauryl sulfate
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73Polysaccharides
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73Polysaccharides
    • A61K8/731Cellulose; Quaternized cellulose derivatives
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P1/00Drugs for disorders of the alimentary tract or the digestive system
    • A61P1/02Stomatological preparations, e.g. drugs for caries, aphtae, periodontitis
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P31/00Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
    • A61P31/04Antibacterial agents
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q11/00Preparations for care of the teeth, of the oral cavity or of dentures; Dentifrices, e.g. toothpastes; Mouth rinses
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/80Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/805Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95

Definitions

  • the invention belongs to the technical field of oral care products, and particularly relates to a formula and process for preparing toothpaste from Xinhui mandarin peel extract.
  • Xinhui Citrus also known as Xinhui Guangchen Citrus or Citrus Citrus
  • Citrus Citrus is a famous local specialty in Xinhui District, Jiangmen City, Guangdong province, and a product of Chinese geographical indication.
  • Xinhui mandarin has both skin and flesh as well as the same source of medicine and food. It is an excellent variety selected by Guangchen mandarin farmers from the large red mandarin citrus of the ruta family in the long cultivation history. Its unique quality, popular in the Ming and Qing dynasties, and is listed as "tribute", tribute every year.
  • Citrus peel is the most important by-product remaining after processing of citrus fruits. Except for amino acids, the rest of the citrus peel is higher than the pulp. It is especially rich in functional ingredients such as flavonoids, limonoids, and carotenoids. , Phenolic acid, pectin and dietary fiber. These substances have many physiological activities such as anti-cancer, anti-oxidation, bacteriostasis, etc., and have important health effects on human health. Among them, the flavonoid content in citrus peel is particularly rich, and its content is much higher than that of fruit juice.
  • Flavonoids are a class of polyphenolic compounds with a C 6 -C 3 -C 6 benzene- ⁇ -pyrone structure and are derivatives of chromogen or chroman.
  • flavanones including 3-hydroxyflavanone or dihydroflavanone
  • flavonoids including 3- Hydroxyflavones or flavonols
  • Flavonoids are considered to be one of the most important medicinal ingredients in citrus, and have the ability to maintain normal osmotic pressure of blood vessels, enhance capillary toughness, shorten bleeding time, reduce cholesterol, anti-allergic, anti-viral, anti-inflammatory, and inhibit cancer cell growth and metastasis And other effects.
  • the first object of the present invention is to provide a formula for preparing toothpaste from Xinhui Citrus Peel Extract, which contains Xinhui Citrus Peel Extract and food-grade auxiliary material extracted by the method provided by the present invention.
  • Xinhui Citrus Peel Extract contains Xinhui Citrus Peel Extract and food-grade auxiliary material extracted by the method provided by the present invention.
  • it can also effectively inhibit the growth of harmful bacteria in the oral cavity, sterilization and anti-inflammatory effects.
  • a formula for making toothpaste from Xinhui Citrus Peel Extract contains the following components in mass percentage:
  • the Xinhui citrus peel extract uses carbon dioxide supercritical extraction technology.
  • step 2 2) Add an entrainer and carry out supercritical carbon dioxide extraction of the Xinhui citrus peel powder obtained in step 1).
  • the extraction temperature is 40-60 ° C
  • the extraction pressure is 200-500 BAR
  • the extraction time is 1-3 hours. After being concentrated under pressure, the Xinhui citrus peel extract is obtained.
  • the temperature increase is conducive to the increase of the solute volatility and the diffusion coefficient of the material, which is beneficial to the extraction of flavonoids in the citrus peel.
  • the temperature increase reduces the concentration of carbon dioxide and reduces the carbon dioxide. Density, which leads to a reduction in the ability to dissolve carbon dioxide, is not conducive to extraction.
  • the elevated temperature will destroy the physiological activity of the extracted flavonoids. Therefore, the extraction temperature should not be too high.
  • the increase of pressure increases the density of supercritical carbon dioxide fluid, which is beneficial to the dissolution of flavonoids.
  • the diffusion coefficient of supercritical carbon dioxide fluid also decreases with the increase of pressure, which is not conducive to the dissolution of flavonoids.
  • the molecular structure of carbon dioxide determines that it has certain limitations for certain separation processes: it has a good ability to dissolve hydrocarbons and weakly polar fat-soluble substances, but it needs to increase the extraction pressure or strongly polar organic compounds or Entrainment is used to achieve separation.
  • Carbon dioxide is a non-polar substance. Pure supercritical carbon dioxide fluid can only extract lipophilic substances with lower polarity. Flavonoids are generally more polar. Only a small amount of volatile small molecules can be obtained without an entrainer. The yield of flavonoids is extremely low. Therefore, it is necessary to increase the extraction rate of flavonoids by adding an entrainer.
  • the entraining agent is 70% ethanol, 95% ethanol, absolute ethanol, or methanol; preferably, the entraining agent is methanol.
  • step 2) the entrainer is first added according to the material-liquid ratio g / mL of 1: (0.5-2), the extraction is statically performed for 20 min, and then the entrainer is added at 0.2-0.6 mL / min. Extraction is performed for 2h; preferably, the entrainer is added according to the material-liquid ratio of 1: 1, static extraction is performed for 20min, and then the entrainer is added at 0.4mL / min, and dynamic extraction is performed for 2h.
  • the extraction rate is the highest when the amount of entrainer is about 0.4 mL / min.
  • the amount of entrainer it is beneficial to the dissolution of flavonoids in citrus peel and increase the extraction rate; however, if the amount is too large, the contact time between flavones in citrus peel and the entrainer becomes shorter, resulting in The use of entrainer is reduced.
  • the longer the time the higher the extraction rate of flavonoids. But after 120min, the total flavonoids leaching amount is very small, because generally, if the extraction time is too short, the supercritical carbon dioxide fluid and the solute do not reach a good contact, the extraction amount is small; after a certain period of extraction, the supercritical fluid and flavonoids The compound gradually approaches the equilibrium of dissolution, and the extraction time is increased, the extraction yield is limited, and the energy consumption of supercritical extraction is increasing with time.
  • the total flavonoid content of the Xinhui mandarin peel extract is greater than 10%.
  • the humectant is at least one of glycerin, sorbitol, polyethylene glycol, and propylene glycol; and the friction agent is one of calcium carbonate, calcium hydrogen phosphate, calcium pyrophosphate, silicon dioxide, and aluminum hydroxide.
  • the surfactant is at least one of sodium lauryl sulfate, sodium 2-acyloxy bond sulfonate
  • the thickener is carboxymethyl cellulose, carboxyethyl cellulose, antlers At least one of pectin, xanthan gum, and guar gum
  • the sweetener is xylitol or sodium saccharin
  • the preservative is potassium sorbate or sodium benzoate
  • the flavor is menthol or fruit Class of spices.
  • the humectant is glycerin and sorbitol
  • the friction agent is silicon dioxide
  • the surfactant is sodium lauryl sulfate
  • the thickener is carboxymethyl cellulose and xanthan gum
  • the sweetener is xylitol
  • the preservative is sodium benzoate
  • the flavor is menthol.
  • glycerin and sorbitol as humectants can prevent toothpaste from curing and hardening in the hose, and make the paste have luster and other effects; using silicon dioxide as a friction agent, has strong tooth selling ability, good physical properties, and stable chemical properties It has the advantages of good compatibility with other ingredients in the toothpaste paste.
  • the specific surface area of silicon dioxide is large, and the ability to adsorb spices is strong, so that the aroma of the toothpaste becomes soft and lasting, the gloss of the paste is improved, and the taste is more Is delicate; choosing carboxymethyl cellulose and xanthan gum as thickeners can improve and increase the viscosity of the paste, maintain the stability of the paste, and improve the physical properties of the paste, and make the taste of toothpaste more Choosing xylitol as a sweetener has the advantages of high safety, good taste, high stability, good water solubility, etc., and the price is reasonable; choosing sodium benzoate as a preservative can delay microbial growth or chemical changes Corruption is more conducive to maintaining the active ingredients in the toothpaste; choosing menthol as a flavor makes the toothpaste have a minty fragrance and cool taste.
  • a second object of the present invention is to provide a process for preparing toothpaste from Xinhui mandarin peel extract, which is simple and quick to prepare.
  • a process for making toothpaste from Xinhui mandarin peel extract includes the following steps:
  • step S2 Add the Xinhui citrus peel extract prepared in step S1 to an appropriate amount of the deionized water, and then add the thickener provided in step S1. Leave it to swell completely and dissolve, and add it to the toothpaste paste making machine. ;
  • step S3 The humectant, the sweetener, the preservative, and the remaining deionized water provided in step S1 are stirred and dissolved, and then added to the toothpaste paste making machine in step S2, and the toothpaste The paste machine is stirred at low speed and evacuated. When the vacuum reaches -0.09MPa, turn off the vacuum pump;
  • step S4 The toothpaste paste making machine described in step S3 is stirred at high speed, and the friction agent and the surfactant provided in step S1 are sequentially sucked into the toothpaste paste making machine using the vacuum pump, and the vacuum pump is turned on. , When the vacuum degree of the mixed environment reaches -0.09 ⁇ -0.095MPa, continue to homogenize for 20 ⁇ 30min to make the paste compact, then turn off the vacuum pump, and inhale the flavor provided in step S1 to the vacuum pump through the vacuum pump Toothpaste machine
  • a toothpaste formulation for Xinhui citrus peel extract provided by the present invention.
  • the carbon dioxide supercritical extraction technology is used to extract the Xinhui citrus peel.
  • the total flavonoid content of the extract is greater than 10%.
  • coli have different degrees of inhibition, and can be used as a natural antibacterial active substance; by selecting the most The combination of good content and food-grade accessories, in addition to the basic functions of cleaning teeth, removing odor and dirt from the oral cavity, can also effectively inhibit the growth of harmful bacteria in the oral cavity, sterilization and anti-inflammatory effects, and can effectively relieve gingivitis, periodontal Swelling, bleeding, and pain caused by inflammation and oral ulcers have significant prevention and relief effects on common oral diseases.
  • FIG. 1 is a process flow chart of manufacturing toothpaste from Xinhui Citrus Peel Extract.
  • the invention discloses a formula for producing toothpaste from Xinhui mandarin peel extract, which comprises the following components in mass percentage:
  • the humectant is at least one of glycerin, sorbitol, polyethylene glycol, and propylene glycol;
  • the friction agent is at least one of calcium carbonate, calcium hydrogen phosphate, calcium pyrophosphate, silicon dioxide, and aluminum hydroxide;
  • surface The active agent is at least one of sodium lauryl sulfate and sodium 2-acyloxy bond sulfonate;
  • the thickener is carboxymethyl cellulose, carboxyethyl cellulose, staghorn pectin, xanthan gum, guar At least one of the gums;
  • the sweetener is xylitol or sodium saccharin;
  • the preservative is potassium sorbate or sodium benzoate;
  • the flavor is menthol or fruit flavor.
  • test instruments and reagents are commercially available products and are all commercially available.
  • step S2 Add the Xinhui citrus peel extract provided in step S1 to an appropriate amount of deionized water, and then add the carboxymethyl cellulose and xanthan gum provided in step S1. Leave it to swell and dissolve, and add toothpaste to make a paste.
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  • step S3 Stir the glycerin, sorbitol, xylitol, sodium benzoate and remaining deionized water provided in step S1 and dissolve it, and then add it to the toothpaste paste making machine in step S2.
  • the toothpaste paste making machine is stirred at low speed and evacuated. Turn off the vacuum pump when the vacuum reaches -0.09MPa;
  • step S4 The toothpaste paste making machine in step S3 is stirred at high speed, and the silicon dioxide and sodium lauryl sulfate provided in step S1 are sequentially sucked into the toothpaste paste making machine by a vacuum pump.
  • the vacuum pump is turned on, and the vacuum degree of the mixing environment reaches -0.095 At MPa, continue to homogenize for 25 minutes to make the paste compact, then turn off the vacuum pump, and suck the menthol provided in step S1 into the toothpaste paste making machine through the vacuum pump;
  • step S2 Add the Xinhui citrus peel extract prepared in step S1 to an appropriate amount of deionized water, and then add the carboxyethyl cellulose and guar gum provided in step S1. Leave to swell and dissolve, and add toothpaste to make the paste.
  • Aircraft
  • step S3 Stir and dissolve the polyethylene glycol, propylene glycol, sodium saccharin, potassium sorbate, and the remaining deionized water in step S1, and then add it to the toothpaste paste machine in step S2.
  • the toothpaste paste machine is stirred at low speed and pumped. Vacuum, turn off the vacuum pump when the vacuum reaches -0.09MPa;
  • step S4 The toothpaste paste making machine in step S3 is stirred at high speed, and the aluminum hydroxide and sodium 2-acyloxy bond sulfonate provided in step S1 are sequentially sucked into the toothpaste paste making machine by using a vacuum pump, the vacuum pump is turned on, and the vacuum of the mixed environment is turned on.
  • the degree reaches -0.095 MPa continue to homogenize for 20 minutes to make the paste compact, then turn off the vacuum pump, and suck the orange flavor flavor provided in step S1 into the toothpaste paste making machine through the vacuum pump;
  • test strain suspension inoculate 6 test strains into solid broth culture medium and incubate at 37 ° C for 24h; use the inoculation hook to pick the surface of the culture medium that has undergone slant activation of the strain
  • the bacterial mass was added with sterile physiological saline, and was uniformly ground in a tissue mill, and the concentration of the bacterial suspension was adjusted to 1 ⁇ 10 6 -6 ⁇ 10 6 cfu / mL.
  • Level 1 Painless ulcers, erythema, or mild pain, without pain medication
  • Grade 2 Pain with erythema, edema, or prickly ulcers, moderate pain, need analgesics, but patients can eat solid food;
  • Level 3 Pain with erythema, edema, or flaky ulcers. Strong analgesics are required. Patients cannot eat solid food, which affects rest.
  • Grade 4 Large-scale mucosal ulcers, severe pain, inability to eat, and need parenteral or enteral nutritional support.
  • the five groups of patients with oral ulcers respectively selected the toothpaste prepared in Example 1, the toothpaste prepared in Example 2, the toothpaste prepared in Example 3, the toothpaste prepared in Example 4, and the ordinary toothpaste on the market in the control group (excluding The active ingredients of the present invention) are used for tooth brushing, once in the morning and evening, and continued to be used for 3 months without additional treatment.
  • the incidence of oral ulcer and the classification of oral ulcer are detected at different time points after treatment.
  • the toothpaste prepared in Examples 1-4 of the present invention has a significant effect on the treatment of oral ulcers, and its treatment effect is significantly better than that of the control example.

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Abstract

本发明公开了一种新会柑果皮萃取液制作牙膏的配方,其包含以下质量百分比的组分:40.0-60.0%的保湿剂、15.0-25.0%的摩擦剂、10.0-15.0%的新会柑果皮萃取液、1.0-3.0%的表面活性剂、1.0-2.0%的增稠剂、0.8-1.4%的香精、0.1-0.2%的甜味剂、0.1-0.2%的防腐剂、以及适量的去离子水。本发明还公开了一种新会柑果皮萃取液制作牙膏的工艺。对于本发明,采用二氧化碳超临界萃取技术对新会柑果皮进行萃取,并将最佳的新会柑果皮萃取液含量结合食品级辅料,除具有洁牙护齿、去除口腔异味和渍垢的基本功能外,还能够有效抑制口腔牙齿有害细菌滋生、杀菌消炎等功效,能够有效缓解因牙龈炎、牙周炎、口腔溃疡导致的牙齿肿胀、出血、疼痛等症状,对常见口腔疾病具有显著的预防和缓解效果。

Description

一种新会柑果皮萃取液制作牙膏的配方及工艺 技术领域
本发明属于口腔护理用品技术领域,具体涉及一种新会柑果皮萃取液制作牙膏的配方及工艺。
背景技术
新会柑,又称新会广陈柑或陈皮柑,广东省江门市新会区著名土特产,中国地理标志产品。新会柑,皮肉兼用,药食同源,是广陈柑农在漫长种植历史中,从芸香科柑橘属大红柑中筛选出来的优秀品种。其品质独特,在明清就风行各地,并被列为“贡品”,年年进贡。
柑橘果皮是柑橘果实加工后余留的最主要的副产品,其所含营养成分除氨基酸外,其余均高于果肉,尤其富含一定功能性成分,如类黄酮、类柠檬苦素、类胡萝卜素、酚酸、果胶和膳食纤维等物质。这些物质具有抗癌、抗氧化、抑菌等诸多生理活性,对人体健康具有重要保健作用。其中,柑果皮中的类黄酮含量尤为丰富,其含量远高于果汁。
类黄酮是一类具有C 6-C 3-C 6苯-γ-吡喃酮结构的多酚类化合物,是色原酮或色原烷的衍生物。目前,已从柑橘属植物中分离鉴定出60多种单体黄酮类化合物,主要分为三类:黄烷酮(包括3-羟基黄烷酮或二氢黄烷酮)、黄酮(包括3-羟基黄酮或黄酮醇)和花色苷。类黄酮被认为是柑橘中最重要的药效成分之一,具有维持血管正常渗透压、增强毛细血管韧性、缩短出血时间、降低胆固醇、抗过敏、抗病毒、抗炎症、抑制癌细胞增长和转移等作用。
现有技术中,曾见金花茶、野菊茶、绿茶、小藻球、普洱茶等天然物质被用于牙膏中用来预防口腔疾病的报道,但未见将新会柑果皮萃取液应用于牙膏中的相关报道。
发明内容
为了克服上述技术缺陷,本发明的第一目的是提供了一种新会柑果皮萃取液制作牙膏的配方,其含有本发明所提供的方法提取得到的新会柑果皮萃取液以及 食品级辅料,除具有洁牙护齿、去除口腔异味和渍垢的基本功能外,还能够有效抑制口腔牙齿有害细菌滋生、杀菌消炎等功效。
为了解决上述问题,本发明按以下技术方案予以实现的:
一种新会柑果皮萃取液制作牙膏的配方,包含以下质量百分比的组分:
Figure PCTCN2018112368-appb-000001
进一步的,包含以下质量百分比的组分:
Figure PCTCN2018112368-appb-000002
进一步的,所述新会柑果皮萃取液采用二氧化碳超临界萃取技术。
进一步的,所述新会柑果皮萃取液的制备方法为:
1)将新鲜的新会柑果皮切成细条状,于50-60℃热风干燥,磨成粉,过筛;
2)加入夹带剂,对步骤1)所制得的新会柑果皮粉末进行二氧化碳超临界萃取,萃取温度为40-60℃,萃取压力为200-500BAR,萃取时间为1-3h,再经过减压浓缩后,即得所述新会柑果皮萃取液。
当温度低于50℃时,黄酮提取率随着温度的升高而升高,但温度高于50℃后,黄酮提取率反而减少,这是因为萃取温度对萃取效果具有双重的影响。一方面,温度升高有利于溶质挥发性的增加和提高物料的扩散系数,有利于柑果皮中黄酮类化合物的萃出;另一方面,温度升高又降低了二氧化碳的浓度,减少了二氧化碳的密度,从而导致二氧化碳溶解能力的降低,不利于萃取。此外,温度升高也会破坏萃取的黄酮类化合物的生理活性。因此,萃取的温度不宜过高。
压力的增大,使超临界二氧化碳流体的密度增大,有利于黄酮类成分的溶出,但是,超临界二氧化碳流体的扩散系数也随压力的增大而减小,又不利于黄酮类成分的溶出;当压力在200-300BAR时,提取率随压力上升而增加,而从300BAR开始,提取率随压力的上升而减少。因此,萃取的压力不宜过高。
二氧化碳的分子结构决定了它对一定的分离过程有一定的局限性:对于烃类和弱极性的脂溶性物质的溶解能力较好,但对于强极性的有机化合物则需加大萃取压力或使用夹带剂来实现分离。二氧化碳是非极性物质,单纯的超临界二氧化碳流体只能萃取极性较低的亲脂性物质,黄酮类物质一般极性较大,在不加夹带剂的条件下只能得到少量易挥发的小分子物质,黄酮类化合物的得率极低,因此,需要通过加入夹带剂来提高黄酮类化合物的提取率。
进一步的,在步骤2)中,所述夹带剂为70%乙醇、95%乙醇、无水乙醇或甲醇;优选的,所述夹带剂为甲醇。
在选择夹带剂时,选取70%乙醇、95%乙醇和无水乙醇,由于有机溶剂中,甲醇的极性大于乙醇,而且甲醇的沸点比无水乙醇的沸点低。因此,选择甲醇可能会更有利于黄酮类化合物的萃取及分离。
进一步的,在步骤2)中,先按料液比g/mL为1:(0.5-2)加入所述夹带剂,静态萃取20min,再按0.2-0.6mL/min添加所述夹带剂,动态萃取2h;优选的,先按料液比为1:1加入所述夹带剂,静态萃取20min,再按0.4mL/min添加所述夹带剂,动态萃取2h。
动态萃取时,夹带剂加入量为0.4mL/min左右时,提取率最高。随着夹带剂用量的增大,有利于柑果皮中的黄酮类化合物的溶出,使提取率升高;但是,用量过大,柑果皮中的黄酮类化合物与夹带剂的接触时间变短,导致夹带剂使用效率降低。
动态萃取时,时间越长,黄酮类化合物的提取率越高。但120min后,总黄酮浸出量很少,这是因为一般情况下,如果萃取时间太短,超临界二氧化碳流体与溶质未达到良好接触,萃取量少;萃取一定时间后,超临界流体与黄酮类化合物逐渐接近溶解平衡,再增加萃取时间,萃取得率增加有限,而且随着时间的延长,超临界萃取的能耗也在增加。
进一步的,所述新会柑果皮萃取液的总黄酮含量大于10%。
进一步的,所述保湿剂为甘油、山梨醇、聚乙二醇、丙二醇中的至少一种;所述摩擦剂为碳酸钙、磷酸氢钙、焦磷酸钙、二氧化硅、氢氧化铝中的至少一种;所述表面活性剂为十二醇硫酸钠、2-酰氧基键磺酸钠中的至少一种;所述增稠剂为羧甲基纤维素、羧乙基纤维素、鹿角果胶、黄原胶、瓜尔胶中的至少一种;所述甜味剂为木糖醇或糖精钠;所述防腐剂为山梨酸钾盐或苯甲酸钠;所述香料为薄荷醇或水果类香料。
进一步的,所述保湿剂为甘油和山梨醇;所述摩擦剂为二氧化硅;所述表面活性剂为十二醇硫酸钠;所述增稠剂为羧甲基纤维素和黄原胶;所述甜味剂为木糖醇;所述防腐剂为苯甲酸钠;所述香料为薄荷醇。
选用甘油和山梨醇作为保湿剂,可防止牙膏在软管中固化变硬,并使膏体具有光泽等效能;选用二氧化硅作为摩擦剂,具有沽齿能力强、物理性能好、化学性质稳定、与牙膏膏体中其它配料的相容性好的优点,而且,二氧化硅的比表面大,对香料的吸附能力强,使牙膏的香气变得柔和持久,提高膏体光泽度,口感更为细腻;选择羧甲基纤维素和黄原胶作为增稠剂,能够改善和增加膏体的粘稠度,保持膏体的稳定性,以及改善膏体的物理性状,并使得牙膏的口感更佳;选择木糖醇作为甜味剂,具有安全性高、引起味觉良好、稳定性高、水溶性好等优点,并且价格合理;选择苯甲酸钠作为防腐剂,能够延迟微生物生长或化学变化引起的腐败,更利于保持牙膏中的有效成分;选择薄荷醇作为香料,使得牙膏具有薄荷味的清香,口感清凉。
为了克服上述技术缺陷,本发明的第二目的是提供了一种新会柑果皮萃取液制作牙膏的工艺方法,该方法制备简单快捷。
为了解决上述问题,本发明按以下技术方案予以实现的:
一种新会柑果皮萃取液制作牙膏的工艺方法,包括以下步骤:
S1、配料:配备包含以下质量百分比的原料组分:40.0-60.0%的保湿剂、15.0-25.0%的摩擦剂、10.0-15.0%的新会柑果皮萃取液、1.0-3.0%的表面活性剂、1.0-2.0%的增稠剂、0.8-1.4%的香精、0.1-0.2%的甜味剂、0.1-0.2%的防腐剂、以及适量的去离子水;
S2、将步骤S1所配备的所述新会柑果皮萃取液加入适量所述去离子水,再加入步骤S1所配备的增稠剂,静置待其溶胀完全后溶解,加入牙膏制膏机中;
S3、将步骤S1所配备的所述保湿剂、所述甜味剂、所述防腐剂和剩余所述去离子水搅拌溶解,再加入到步骤S2所述的牙膏制膏机中,所述牙膏制膏机低速搅拌并抽真空,待真空度达到-0.09MPa时关闭真空泵;
S4、使步骤S3所述的牙膏制膏机高速搅拌,将步骤S1所配备的所述摩擦剂、所述表面活性剂依次利用所述真空泵吸入到所述牙膏制膏机中,开启所述真空泵,混合环境的真空度达到-0.09~-0.095MPa时继续均质20~30min,使膏体达到紧致状态,然后关闭所述真空泵,将步骤S1所配备的香精通过所述真空泵吸入到所述牙膏制膏机中;
S5、开启所述真空泵继续均质10~20min,得到具有一定粘性的、稀稠适当的膏体,经质量检验合格后进行灌装、包装,即可制得所需的牙膏成品。
与现有技术相比,本发明的有益效果是:
(1)本发明提供的一种新会柑果皮萃取液制作牙膏的配方,采用二氧化碳超临界萃取技术对新会柑果皮进行萃取,其萃取液的总黄酮含量大于10%,该黄酮类化合物对金黄色葡萄球菌、溶血性链球菌、乳杆菌、厌氧扩菌、嗜酸乳杆菌、大肠杆菌具有不同程度的抑制,可作为一种天然抗菌活性物质;通过选取新会柑果皮萃取液的最佳含量与食品级辅料结合,除具有洁牙护齿、去除口腔异味和渍垢的基本功能外,还能够有效抑制口腔牙齿有害细菌滋生、杀菌消炎等功效,能够有效缓解因牙龈炎、牙周炎、口腔溃疡导致的牙齿肿胀、出血、疼痛等症状,对常见口腔疾病具有显著的预防和缓解效果。
(2)本发明所述的新会柑果皮萃取液制作牙膏的工艺方法,该方法制备简便快捷。
附图说明
下面结合附图对本发明的具体实施方式作进一步详细的说明,其中:
图1为本发明所述新会柑果皮萃取液制作牙膏的工艺流程图。
具体实施方式
以下结合附图对本发明的优选实施例进行说明,应当理解,此处所描述的优选实施例仅用于说明和解释本发明,并不用于限定本发明。
本发明公开了一种新会柑果皮萃取液制作牙膏的配方,包含以下质量百分比的组分:
Figure PCTCN2018112368-appb-000003
其中,保湿剂为甘油、山梨醇、聚乙二醇、丙二醇中的至少一种;摩擦剂为碳酸钙、磷酸氢钙、焦磷酸钙、二氧化硅、氢氧化铝中的至少一种;表面活性剂为十二醇硫酸钠、2-酰氧基键磺酸钠中的至少一种;增稠剂为羧甲基纤维素、羧乙基纤维素、鹿角果胶、黄原胶、瓜尔胶中的至少一种;甜味剂为木糖醇或糖精钠;防腐剂为山梨酸钾盐或苯甲酸钠;香料为薄荷醇或水果类香料。
各种试验仪器与试剂均为市售商品,均为可通过商业途径购买获得。
实施例1
(一)新会柑果皮萃取液的制备:
1)将新鲜的新会柑果皮切成细条状,于55℃热风干燥,磨成粉,过筛;
2)取出100g干粉加入100mL甲醇,在萃取温度为50℃,萃取压力为300BAR的条件下,静态萃取20min,再按0.4mL/min添加甲醇,动态萃取2h,再经过减压浓缩后,即得22.2g新会柑果皮萃取液。
(二)一种新会柑果皮萃取液制作牙膏的配方,包含以下质量的组分:
Figure PCTCN2018112368-appb-000004
(三)新会柑果皮萃取液制作牙膏的工艺方法,包括以下步骤:
S1、配料:配备包含以下质量百分比的原料组分:25.0g的甘油、25.0g的山梨醇、20.0g的二氧化硅、12.0g的新会柑果皮萃取液、2.0g的十二醇硫酸钠、0.75g的羧甲基纤维素、0.75g的黄原胶、1.0g的薄荷醇、0.15g的木糖醇、0.15g的苯甲酸钠、以及13.2g的去离子水;
S2、将步骤S1所配备的新会柑果皮萃取液加入适量去离子水,再加入步骤S1所配备的羧甲基纤维素、黄原胶,静置待其溶胀完全后溶解,加入牙膏制膏机中;
S3、将步骤S1所配备的甘油、山梨醇、木糖醇、苯甲酸钠和剩余去离子水搅拌溶解,再加入到步骤S2的牙膏制膏机中,牙膏制膏机低速搅拌并抽真空,待真空度达到-0.09MPa时关闭真空泵;
S4、使步骤S3的牙膏制膏机高速搅拌,将步骤S1所配备的二氧化硅、十二醇硫酸钠依次利用真空泵吸入到牙膏制膏机中,开启真空泵,混合环境的真空度达到-0.095MPa时继续均质25min,使膏体达到紧致状态,然后关闭真空泵,将步骤S1所配备的薄荷醇通过真空泵吸入到牙膏制膏机中;
S5、开启真空泵继续均质15min,得到具有一定粘性的、稀稠适当的膏体,经质量检验合格后进行灌装、包装,即可制得所需的牙膏成品。
实施例2
(一)新会柑果皮萃取液的制备:
1)将新鲜的新会柑果皮切成细条状,于50℃热风干燥,磨成粉,过筛;
2)取出100g干粉加入50mL甲醇,在萃取温度为40℃,萃取压力为200BAR的条件下,静态萃取20min,再按0.2mL/min添加甲醇,动态萃取2h,再经过减压浓缩后,即得20.1g新会柑果皮萃取液。
(二)一种新会柑果皮萃取液制作牙膏的配方,包含以下质量的组分:
Figure PCTCN2018112368-appb-000005
(三)新会柑果皮萃取液制作牙膏的工艺方法与实施例1相同。
实施例3
(一)新会柑果皮萃取液的制备:
1)将新鲜的新会柑果皮切成细条状,于60℃热风干燥,磨成粉,过筛;
2)取出100g干粉加入200mL甲醇,在萃取温度为60℃,萃取压力为500BAR的条件下,静态萃取20min,再按0.6mL/min添加甲醇,动态萃取2h,再经过减压浓缩后,即得21.3g新会柑果皮萃取液。
(二)一种新会柑果皮萃取液制作牙膏的配方,包含以下质量的组分:
Figure PCTCN2018112368-appb-000006
Figure PCTCN2018112368-appb-000007
(三)新会柑果皮萃取液制作牙膏的工艺方法与实施例1相同。
实施例4
(一)新会柑果皮萃取液的制备方法与实施例1相同。
(二)一种新会柑果皮萃取液制作牙膏的配方,包含以下质量的组分:
Figure PCTCN2018112368-appb-000008
(三)新会柑果皮萃取液制作牙膏的工艺方法,包括以下步骤:
S1、配料:配备包含以下质量百分比的原料组分:25.0g的聚乙二醇、25.0g的丙二醇、20.0g的氢氧化铝、12.0g的新会柑果皮萃取液、2.0g的2-酰氧基键磺酸钠、0.75g的羧乙基纤维素、0.75g的瓜尔胶、1.0g的橘子味香精、0.15g的糖 精钠、0.15g的山梨酸钾盐、以及13.2g的去离子水;
S2、将步骤S1所配备的新会柑果皮萃取液加入适量去离子水,再加入步骤S1所配备的羧乙基纤维素、瓜尔胶,静置待其溶胀完全后溶解,加入牙膏制膏机中;
S3、将步骤S1所配备的聚乙二醇、丙二醇、糖精钠、山梨酸钾盐和剩余去离子水搅拌溶解,再加入到步骤S2的牙膏制膏机中,牙膏制膏机低速搅拌并抽真空,待真空度达到-0.09MPa时关闭真空泵;
S4、使步骤S3的牙膏制膏机高速搅拌,将步骤S1所配备的氢氧化铝、2-酰氧基键磺酸钠依次利用真空泵吸入到牙膏制膏机中,开启真空泵,混合环境的真空度达到-0.095MPa时继续均质20min,使膏体达到紧致状态,然后关闭真空泵,将步骤S1所配备的橘子味香精通过真空泵吸入到牙膏制膏机中;
S5、开启真空泵继续均质10min,得到具有一定粘性的、稀稠适当的膏体,经质量检验合格后进行灌装、包装,即可制得所需的牙膏成品。
理化指标及稳定性测定
将实施例1-4所制得的牙膏进行理化指标及稳定性测定,测试结果如表1所示。
表1理化指标及稳定性测定结果
Figure PCTCN2018112368-appb-000009
Figure PCTCN2018112368-appb-000010
由表1可知,本发明的实施例1-4所制得的牙膏各项指标均符合国家标准(GB8372-2017和QB2966-2014)。
效果试验例1
新会果皮萃取液中类黄酮的抗菌效果试验:
(1)供试菌株悬浮液制备:将6种供试菌种分别接种于固体肉汤培养基中,于37℃恒温培养24h;用接种钩挑取已进行菌种斜面活化的培养基表面的菌块,加入无菌生理盐水,在组织研磨器中研磨均匀,并将菌悬液的浓度调节到1×10 6-6×10 6cfu/mL。
(2)抑菌试验:配制LB固体培养基,将固体培养基熔化倒入培养皿中冷却、凝固后,用无菌棉拭子分别蘸取各试验菌的菌悬液,均匀涂布培养基表面,制成含菌平板。采用滤纸片法,将直径5mm的滤纸圆片,经高压灭菌处理后干燥,滴加10μL 10%本发明实施例1-4所制得的新会柑果皮萃取液作为试验样片,滴加DMSO液作为阴性对照,用无菌镊子将试验样片和阴性对照样片贴放于每个培养皿表面,盖好培养皿,于37℃培养24h。试验结果如表2所示。
表2新会柑果皮萃取液对6种受试菌的抗菌活性测试结果
Figure PCTCN2018112368-appb-000011
注:“—”:无抑菌活性;抑菌圈直径:以mm计。
由表2可知,本发明的实施例1-4所制得的新会柑果皮萃取液对金黄色葡萄球菌、溶血性链球菌、乳杆菌、厌氧扩菌、嗜酸乳杆菌、大肠杆菌具有不同程度 的抑制作用。
效果试验例2
使用本发明的实施例1-4所制得的牙膏及市面上的普通牙膏(不含本发明的活性成分)进行临床实验。具体如下:
(1)按照临床诊断口腔溃疡的标准,共选入100名患者,分成5个实验组,每组20名。各组在年龄、性别、疾病种类和溃疡级别等方面需要具备无显著差异(P>0.05),具有可比性;其中,每组中口腔溃疡1级5名,口腔溃疡2级5名,口腔溃疡3级5名,口腔溃疡4级5名。
口腔溃疡分级:
1级:无痛性溃疡、红斑或轻微疼痛,不需止痛药;
2级:疼痛伴红斑、水肿或点状溃疡,中度疼痛、需用止痛剂,但患者能进食固体食物;
3级:疼痛伴红斑、水肿或片状溃疡,需用较强止痛剂,患者不能进食固体食物,影响休息;
4级:粘膜大面积溃疡,剧痛,不能进食,需要肠外或肠内营养支持。
(2)实验方法:
5组口腔溃疡患者分别选用实施例1制得的牙膏、实施例2制得的牙膏、实施例3制得的牙膏、实施例4制得的牙膏、对照组的市面上的普通牙膏(不含本发明的活性成分)进行刷牙,早晚各一次,持续使用3个月,不进行额外处理,选取治疗后不同时间点进行口腔溃疡发生率检测及口腔溃疡发生分级的检测。
(3)评定指标:
详细检查治疗结束时溃疡的发生情况,及溃疡大小、深度、形状及周围粘膜登记情况。以溃疡疼痛消失及所有溃疡创面愈合为指标判断愈合时间。试验结果如表3所示。
表3不同时间口腔溃疡愈合例数情况
Figure PCTCN2018112368-appb-000012
Figure PCTCN2018112368-appb-000013
由表3可知,本发明的实施例1-4所制得的牙膏对治疗口腔溃疡具有显著的功效,其治疗效果明显优于对照例。
以上所述,仅是本发明的较佳实施例而已,并非对本发明作任何形式上的限制,故凡是未脱离本发明技术方案内容,依据本发明的技术实质对以上实施例所作的任何修改、等同变化与修饰,均仍属于本发明技术方案的范围内。

Claims (10)

  1. 一种新会柑果皮萃取液制作牙膏的配方,其特征在于,包含以下质量百分比的组分:
    Figure PCTCN2018112368-appb-100001
  2. 根据权利要求1所述的新会柑果皮萃取液制作牙膏的配方,其特征在于,包含以下质量百分比的组分:
    Figure PCTCN2018112368-appb-100002
  3. 根据权利要求1所述的新会柑果皮萃取液制作牙膏的配方,其特征在于:所述新会柑果皮萃取液采用二氧化碳超临界萃取技术。
  4. 根据权利要求3所述的新会柑果皮萃取液制作牙膏的配方,其特征在于,所述新会柑果皮萃取液的制备方法为:
    1)将新鲜的新会柑果皮切成细条状,于50-60℃热风干燥,磨成粉,过筛;
    2)加入夹带剂,对步骤1)所制得的新会柑果皮粉末进行二氧化碳超临界 萃取,萃取温度为40-60℃,萃取压力为200-500BAR,萃取时间为1-3h,再经过减压浓缩后,即得所述新会柑果皮萃取液。
  5. 根据权利要求4所述的新会柑果皮萃取液制作牙膏的配方,其特征在于:在步骤2)中,所述夹带剂为70%乙醇、95%乙醇、无水乙醇或甲醇。
  6. 根据权利要求4所述的新会柑果皮萃取液制作牙膏的配方,其特征在于:在步骤2)中,先按料液比g/mL为1:(0.5-2)加入所述夹带剂,静态萃取20min,再按0.2-0.6mL/min添加所述夹带剂,动态萃取2h。
  7. 根据权利要求4所述的新会柑果皮萃取液制作牙膏的配方,其特征在于:所述新会柑果皮萃取液的总黄酮含量大于10%。
  8. 根据权利要求1所述的新会柑果皮萃取液制作牙膏的配方,其特征在于:所述保湿剂为甘油、山梨醇、聚乙二醇、丙二醇中的至少一种;所述摩擦剂为碳酸钙、磷酸氢钙、焦磷酸钙、二氧化硅、氢氧化铝中的至少一种;所述表面活性剂为十二醇硫酸钠、2-酰氧基键磺酸钠中的至少一种;所述增稠剂为羧甲基纤维素、羧乙基纤维素、鹿角果胶、黄原胶、瓜尔胶中的至少一种;所述甜味剂为木糖醇或糖精钠;所述防腐剂为山梨酸钾盐或苯甲酸钠;所述香料为薄荷醇或水果类香料。
  9. 根据权利要求8所述的新会柑果皮萃取液制作牙膏的配方,其特征在于:所述保湿剂为甘油和山梨醇;所述摩擦剂为二氧化硅;所述表面活性剂为十二醇硫酸钠;所述增稠剂为羧甲基纤维素和黄原胶;所述甜味剂为木糖醇;所述防腐剂为苯甲酸钠;所述香料为薄荷醇。
  10. 一种根据权利要求1~9任一项所述的新会柑果皮萃取液制作牙膏的工艺方法,其特征在于,包括以下步骤:
    S1、配料:配备包含以下质量百分比的原料组分:40.0-60.0%的保湿剂、15.0-25.0%的摩擦剂、10.0-15.0%的新会柑果皮萃取液、1.0-3.0%的表面活性剂、1.0-2.0%的增稠剂、0.8-1.4%的香精、0.1-0.2%的甜味剂、0.1-0.2%的防腐剂、以及适量的去离子水;
    S2、将步骤S1所配备的所述新会柑果皮萃取液加入适量所述去离子水,再加入步骤S1所配备的增稠剂,静置待其溶胀完全后溶解,加入牙膏制膏机中;
    S3、将步骤S1所配备的所述保湿剂、所述甜味剂、所述防腐剂和剩余所述 去离子水搅拌溶解,再加入到步骤S2所述的牙膏制膏机中,所述牙膏制膏机低速搅拌并抽真空,待真空度达到-0.09MPa时关闭真空泵;
    S4、使步骤S3所述的牙膏制膏机高速搅拌,将步骤S1所配备的所述摩擦剂、所述表面活性剂依次利用所述真空泵吸入到所述牙膏制膏机中,开启所述真空泵,混合环境的真空度达到-0.09~-0.095MPa时继续均质20~30min,使膏体达到紧致状态,然后关闭所述真空泵,将步骤S1所配备的香精通过所述真空泵吸入到所述牙膏制膏机中;
    S5、开启所述真空泵继续均质10~20min,得到具有一定粘性的、稀稠适当的膏体,经质量检验合格后进行灌装、包装,即可制得所需的牙膏成品。
PCT/CN2018/112368 2018-09-28 2018-10-29 一种新会柑果皮萃取液制作牙膏的配方及工艺 WO2020062389A1 (zh)

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