CN107693392B - Toothpaste containing enzyme preparation and preparation method thereof - Google Patents

Toothpaste containing enzyme preparation and preparation method thereof Download PDF

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Publication number
CN107693392B
CN107693392B CN201710131247.0A CN201710131247A CN107693392B CN 107693392 B CN107693392 B CN 107693392B CN 201710131247 A CN201710131247 A CN 201710131247A CN 107693392 B CN107693392 B CN 107693392B
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toothpaste
enzyme
enzyme preparation
stirring
lactoferrin
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CN107693392A (en
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陈敏珊
郑晓霞
曾晓宇
李立芬
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Guangzhou Shuke Industrial Co.,Ltd.
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Guangzhou Weimeizi Industrial Co ltd
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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
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/64Proteins; Peptides; Derivatives or degradation products thereof
    • A61K8/66Enzymes
    • 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
    • A61K8/40Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing nitrogen
    • A61K8/44Aminocarboxylic acids or derivatives thereof, e.g. aminocarboxylic acids containing sulfur; Salts; Esters or N-acylated derivatives thereof
    • A61K8/442Aminocarboxylic acids or derivatives thereof, e.g. aminocarboxylic acids containing sulfur; Salts; Esters or N-acylated derivatives thereof substituted by amido group(s)
    • 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
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/64Proteins; Peptides; Derivatives or degradation products 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
    • A61K8/72Cosmetics 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
    • A61K8/81Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
    • A61K8/8164Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a carboxyl radical, and containing at least one other carboxyl radical in the molecule, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers, e.g. poly (methyl vinyl ether-co-maleic anhydride)
    • 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
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q17/00Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
    • A61Q17/005Antimicrobial preparations

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Birds (AREA)
  • Epidemiology (AREA)
  • Dermatology (AREA)
  • Oral & Maxillofacial Surgery (AREA)
  • Cosmetics (AREA)

Abstract

The invention discloses a toothpaste containing enzyme preparation and its preparing method, wherein the toothpaste contains enzyme preparation composition composed of detergent enzyme and inhibiting/sterilizing enzyme. The enzyme preparation composition of the toothpaste has stable activity in the shelf life, and can ensure the stability of the toothpaste. The toothpaste of the invention can effectively decompose water-soluble glucan in dental calculus, prevent the formation of dental calculus, effectively remove dental calculus, obviously kill harmful bacteria in oral cavity, and prevent oral diseases such as dental caries, gingivitis, periodontitis and the like, thereby keeping oral health.

Description

Toothpaste containing enzyme preparation and preparation method thereof
Technical Field
The invention relates to the technical field of oral care, in particular to application of an enzyme preparation in an oral care product, and specifically relates to toothpaste containing the enzyme preparation and a preparation method thereof.
Background
As a biological agent, the enzyme is gradually applied to toothpaste products due to the advantages of good safety, high activity and the like. At present, enzyme preparation toothpaste products on the market are increasingly common and are used for tooth allergy, sterilization and inflammation diminishing, caries prevention, gingivitis and tooth whitening, but enzyme preparation toothpaste which can remove dental calculus and effectively inhibit bacteria and sterilize is rare.
Tartar is a soft yellow or off-white deposit that adheres to the tooth surface, restorations, calculus, and gums and has weaker adhesion than plaque. At present, enzyme is added into toothpaste, so that insoluble plaque gum base and food residues are converted into water-soluble substances by catalysis of the enzyme, and the water-soluble substances are dissolved by water and discharged out of oral cavities when teeth are brushed and mouth is rinsed, so that teeth can be whitened, and oral diseases such as dental caries, gingivitis and the like can be prevented.
Natural antiseptic and antibacterial components are always the hot and the effort direction for the research of oral care industry and even the whole daily chemical industry. Biological enzyme preparation such as lysozyme, as a natural antibacterial active ingredient, has been applied to some oral products, can obviously improve the gingivitis condition of oral cavity, and effectively inhibit periodontal pathogenic bacteria.
The stability of the biological enzyme activity is a technical key in the application research of the oral care products. Enzymes may lose activity due to physical factors (light, temperature, pressure), chemical factors (pH, electrolytes, ionic strength, oxidation and reduction), and production factors (enzymatic degradation). The oral care products are complex mixtures, so that the stability of the product is ensured while the enzyme activity in the shelf life is required to be maintained, and the problem of applying the biological enzyme preparation in the oral care products is solved.
The enzyme activity is the key of the success or failure of the enzyme preparation toothpaste. The enzyme activity is extremely sensitive and changes rapidly, so that the conditions are not suitable slightly, and the enzyme activity in the toothpaste is reduced or even completely inactivated.
The existing enzyme preparation toothpaste mainly has the following defects:
(1) in order to ensure the enzyme activity of the enzyme-containing toothpaste, an enzyme stabilizer or a strengthening agent is usually added, or the enzyme-containing toothpaste with color strips and double components is prepared, so that the problem that the biological enzyme is incompatible with other components of the toothpaste, such as a surfactant, is solved. But the complicated steps of preparing the paste separately, independently subpackaging and the like are required.
(2) The effects of the enzyme-containing toothpaste such as caries prevention and bacteriostasis are not supported by specific experimental data, an in-vitro method is not used for verification, and the effects of testing bacterial plaque, gingival index and caries prevention are mostly determined and tested clinically.
(3) Enzyme-containing toothpastes which can effectively remove tartar and have bactericidal effects are less common.
(4) The shelf life of the enzyme-containing toothpaste has no approximate period, and the product quality needs to be improved.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the toothpaste containing the enzyme preparation, which has simple preparation method and high enzyme activity, can effectively prevent the formation of tartar and remove tartar, can kill harmful germs in the oral cavity and maintain the oral health.
The invention also aims to provide a preparation method of the toothpaste containing the enzyme preparation.
The above object of the present invention is achieved by the following scheme:
a toothpaste containing enzyme preparation, which comprises enzyme preparation composition, wherein the enzyme preparation composition consists of detergent enzyme and bacteriostatic/bactericidal enzyme; the detergent enzyme is dextranase, preferably alpha-dextranase belonging to dextranase; the bacteriostatic/bactericidal enzyme is glucose oxidase, lactoperoxidase, lactoferrin and lysozyme.
The enzyme preparation composition accounts for 0.13-0.5% of the total weight of the toothpaste formula.
In the enzyme preparation composition, the weight ratio of the detergent enzyme to the inhibiting/sterilizing enzyme is 1: 8-5: 4.
In the enzyme preparation composition, the weight ratio of glucose oxidase, lactoperoxidase and lactoferrin is 1: 1: 1; the weight ratio of the total weight of the glucose oxidase, the lactoperoxidase and the lactoferrin to the lysozyme is 3: 10-6: 1.
The inventor finds that the activity of the enzyme preparation is greatly influenced by the ingredients of the toothpaste formula, and the reasonable collocation of the formula structure of the toothpaste directly relates to whether the enzyme preparation can be kept stable, and is the key for keeping higher enzyme activity of the toothpaste. Therefore, on the basis of establishing the enzyme preparation composition, the reasonable selection of the formulation components with optimal collocation is crucial.
The formula of the toothpaste body of the toothpaste containing the enzyme preparation comprises the following components:
Figure GDA0002602277850000021
Figure GDA0002602277850000031
the percentage is that each component accounts for the total weight of the formula.
In the formula, alpha-dextranase, glucose oxidase, lactoperoxidase, lactoferrin and lysozyme are the enzyme preparation of the invention. Wherein, the alpha-dextranase belongs to dextranase and can effectively remove water-soluble glucan in tartar and tartar, thereby being capable of removing tartar and preventing the formation of tartar; the glucose oxidase is an aerobic dehydrogenase prepared by fermenting aspergillus niger and the like, has no toxic or side effect on human bodies, and has the functions of removing glucose, deoxidizing, sterilizing and the like; the lactoperoxidase can effectively kill escherichia coli, staphylococcus aureus, pseudomonas aeruginosa, bacillus subtilis, salmonella and other harmful gram-negative bacteria; lactoferrin is a natural active glycoprotein with multiple physiological functions, belongs to a broad-spectrum bacteriostatic agent, and can inhibit gram-negative bacteria (such as escherichia coli and salmonella) and gram-positive bacteria (such as staphylococcus aureus, listeria monocytogenes and the like); the lysozyme can kill streptococcus, lactobacillus, filamentous bacteria and other harmful bacteria which promote decayed teeth in the oral cavity; the alpha-dextranase, the glucose oxidase, the lactoperoxidase, the lactoferrin and the lysozyme are all commercially available products, and the method can be realized.
The PVM/MA copolymer is an abbreviation of vinyl methyl ether/maleic anhydride copolymer.
In the above formulation, in order to maintain the activity of the enzyme preparation composition, the colloidal system of the present invention does not select sodium carboxymethylcellulose having poor enzyme resistance, but uses a combination of xanthan gum and carrageenan.
The inventor finds that sodium lauryl sulfate serving as an anionic surfactant can reduce the enzyme activity of the enzyme preparation composition, but the influence of the sodium lauryl sulfate on the enzyme activity can be greatly reduced and the foaming performance of enzyme-containing toothpaste can be ensured after the amphoteric surfactant such as cocamidopropyl betaine and sodium lauryl sulfate are compounded, so that the stability of the enzyme activity and the mouthfeel during tooth brushing can be ensured.
The invention also provides a preparation method of the toothpaste containing the enzyme preparation, which comprises the following steps:
step 1
Adding saccharin sodium and sodium pyrophosphate into deionized water, stirring to dissolve completely, adding glycerol, sorbitol, polyethylene glycol-8 and titanium dioxide, and stirring for 5min to obtain liquid phase;
adding silicon dioxide, xanthan gum, carrageen and PVM/MA copolymer into a container and uniformly stirring to obtain mixed powder;
step 2
And (2) adding the mixed powder in the step (1) into the liquid phase in the step (1), stirring for 20min, then adding essence, sodium lauryl sulfate, cocamidopropyl betaine, alpha-dextranase, glucose oxidase, lactoperoxidase, lactoferrin, potassium thiocyanate and lysozyme, stirring for 15min, and degassing to prepare the toothpaste containing the enzyme preparation.
The toothpaste containing the enzyme preparation has obvious dental tartar removal effect, and in the test of removing artificial dental tartar in vitro, the removal rate of 30% of dental tartar can be achieved only by adding 0.1% of alpha-dextranase. The toothpaste can keep higher enzyme activity, and the enzyme activity retention rate is up to 100% after the toothpaste is placed at room temperature for 6 months.
Compared with the prior art, the invention has the following beneficial effects:
1. the toothpaste containing the enzyme preparation can effectively decompose water-soluble glucan in dental calculus so as to prevent the formation of the dental calculus and help to remove the dental calculus, and can obviously kill harmful bacteria in oral cavity and prevent oral diseases such as dental caries, gingivitis, periodontitis and the like so as to keep the oral cavity healthy.
2. In the toothpaste formula, the optimal tartar removal effect can be ensured by controlling the dosage of the alpha-dextranase to be 0.01-0.1%, if the dosage is less than the dosage, the tartar removal effect of the toothpaste is poor, and if the dosage is higher than the dosage, the tartar removal effect of the toothpaste cannot be improved, and the cost is increased.
3. In the enzyme preparation composition, the lysozyme, the lactoperoxidase system and the lactoferrin are compounded and combined in a proper proportion, and a better synergistic effect is achieved by optimizing the compounding proportion of the lysozyme, the lactoperoxidase system and the lactoferrin.
4. The bioactive substances are easy to destroy and difficult to store in the toothpaste, and the formula needs to be careful to keep the good compatibility of the bioactive substances and the basic components of the toothpaste. Therefore, the toothpaste formula of the invention adopts the toothpaste components and the dosage which have better compatibility with the enzyme preparation, thereby ensuring that the toothpaste has higher enzyme activity and simultaneously ensuring the stability of the toothpaste.
5. The factors influencing the enzyme activity are many, such as pH, temperature, electrolyte and the like, therefore, when the inventor develops the toothpaste formula of the invention, in addition to considering the compatibility of the biological enzyme and other components of the toothpaste, the inventor also pays attention to control other indexes of the toothpaste, ensures that the conditions required by high enzyme activity are in a proper range, such as the water content and the salt content in the toothpaste formula are not too high, and the inventor adds the PVM/MA copolymer, on one hand, the acid-base property of the toothpaste can be controlled in a neutral to slightly acidic range, and also can delay the release of the biological active component, thereby effectively playing the role of the enzyme preparation composition.
Detailed Description
The present invention will be further described with reference to specific examples, which are not intended to limit the present invention in any way.
Example 1
The formula of the toothpaste body of the toothpaste containing the enzyme preparation in the embodiment is composed of the following components:
Figure GDA0002602277850000041
Figure GDA0002602277850000051
the percentage is that each component accounts for the total weight of the formula.
The preparation method of the toothpaste containing the enzyme preparation comprises the following steps:
step 1
Adding saccharin sodium and sodium pyrophosphate into deionized water, stirring to dissolve completely, adding glycerol, sorbitol, polyethylene glycol-8 and titanium dioxide, and stirring for 5min to obtain liquid phase;
adding silicon dioxide, xanthan gum, carrageen and PVM/MA copolymer into a container and uniformly stirring to obtain mixed powder;
step 2
Adding the mixed powder in the step 1 into the liquid phase in the step 1, stirring for 20min, then adding essence, sodium lauryl sulfate, cocamidopropyl betaine, alpha-dextranase and lysozyme, stirring for 15min, and degassing to prepare the toothpaste of the embodiment.
Example 2
The formula of the toothpaste body of the toothpaste containing the enzyme preparation in the embodiment is composed of the following components:
Figure GDA0002602277850000052
the percentage is that each component accounts for the total weight of the formula.
The preparation method of the toothpaste containing the enzyme preparation comprises the following steps:
step 1
Adding saccharin sodium and sodium pyrophosphate into deionized water, stirring to dissolve completely, adding glycerol, sorbitol, polyethylene glycol-8 and titanium dioxide, and stirring for 5min to obtain liquid phase;
adding silicon dioxide, xanthan gum, carrageen and PVM/MA copolymer into a container and uniformly stirring to obtain mixed powder;
step 2
Adding the mixed powder in the step 1 into the liquid phase in the step 1, stirring for 20min, then adding essence, sodium lauryl sulfate, cocamidopropyl betaine, alpha-dextranase, glucose oxidase, lactoperoxidase, lactoferrin, lysozyme and potassium thiocyanate, stirring for 15min, and degassing to prepare the toothpaste of the embodiment.
Example 3
The formula of the toothpaste body of the toothpaste containing the enzyme preparation in the embodiment is composed of the following components:
Figure GDA0002602277850000061
the percentage is that each component accounts for the total weight of the formula.
The preparation method of the toothpaste containing the enzyme preparation comprises the following steps:
step 1
Adding saccharin sodium and sodium pyrophosphate into deionized water, stirring to dissolve completely, adding glycerol, sorbitol, polyethylene glycol-8 and titanium dioxide, and stirring for 5min to obtain liquid phase;
adding silicon dioxide, xanthan gum, carrageen and PVM/MA copolymer into a container and uniformly stirring to obtain mixed powder;
step 2
Adding the mixed powder in the step 1 into the liquid phase in the step 1, stirring for 20min, then adding essence, sodium lauryl sulfate, cocamidopropyl betaine, alpha-dextranase, glucose oxidase, lactoperoxidase, lactoferrin, lysozyme and potassium thiocyanate, stirring for 15min, and degassing to prepare the toothpaste of the embodiment.
Example 4 stability testing of examples 1-3
After accelerated aging of the toothpastes of examples 1 to 3 at 45 ℃ for 3 months, the respective indexes related to the products were examined. The results are shown in Table 1.
Evaluation criteria:
1. sensory index paste: uniform and has no foreign matter.
2. The physical and chemical index pH is 5.5-10.0; stability: the paste does not overflow out of the tube mouth and does not separate out liquid, and the fragrance, the color and the luster are normal.
Table 1 examples 1-3 results of toothpaste stability experiments
Figure GDA0002602277850000071
As can be seen from the results in Table 1, the toothpaste product containing the enzyme preparation composition of the present invention has good overall stability and excellent quality.
Variations and modifications to the above-described embodiments may occur to those skilled in the art, which fall within the scope and spirit of the above description. Therefore, the present invention is not limited to the specific embodiments disclosed and described above, and some modifications and variations of the present invention should fall within the scope of the claims of the present invention. Furthermore, although specific terms are employed herein, they are used in a generic and descriptive sense only and not for purposes of limitation.

Claims (2)

1. The toothpaste containing the enzyme preparation is characterized by comprising an enzyme preparation composition, wherein the enzyme preparation composition accounts for 0.13-0.5% of the total weight of the toothpaste formula, and the enzyme preparation composition consists of detergent enzyme and bacteriostatic/bactericidal enzyme; the enzyme for inhibiting/killing bacteria is glucose oxidase, lactoperoxidase, lactoferrin and lysozyme, and the weight ratio of the detergent enzyme to the enzyme for inhibiting/killing bacteria is 1: 8-5: 4; the detergent enzyme is alpha-dextranase; the weight ratio of the glucose oxidase to the lactoperoxidase to the lactoferrin is 1: 1: 1, the weight ratio of the total weight of the glucose oxidase, the lactoperoxidase and the lactoferrin to the lysozyme is 3: 10-6: 1; the toothpaste comprises the following components in percentage by weight:
Figure FDA0002602277840000011
2. a method of preparing the toothpaste of claim 1, comprising the steps of:
step 1
Adding saccharin sodium and sodium pyrophosphate into deionized water, stirring to dissolve completely, adding glycerol, sorbitol, polyethylene glycol-8 and titanium dioxide, and stirring for 5min to obtain liquid phase;
adding silicon dioxide, xanthan gum, carrageen and PVM/MA copolymer into a container and uniformly stirring to obtain mixed powder;
step 2
And (2) adding the mixed powder in the step (1) into the liquid phase in the step (1), stirring for 20min, then adding essence, sodium lauryl sulfate, cocamidopropyl betaine, alpha-dextranase, glucose oxidase, lactoperoxidase, lactoferrin, potassium thiocyanate and lysozyme, stirring for 15min, and degassing to prepare the toothpaste containing the enzyme preparation.
CN201710131247.0A 2017-03-07 2017-03-07 Toothpaste containing enzyme preparation and preparation method thereof Active CN107693392B (en)

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Publication number Priority date Publication date Assignee Title
CN108578268B (en) * 2018-06-21 2019-07-23 广州康云生物科技有限公司 A kind of toothpaste containing lysozyme
CN112336658A (en) * 2019-08-09 2021-02-09 滕敏子 Dental caries preventing ice cream toothpaste without fluorine and preparation process thereof
CN111558033A (en) * 2020-05-14 2020-08-21 广州中昱医学生物科技有限公司 Oral cavity cleaning composition and application thereof
CN112190499B (en) * 2020-11-12 2022-03-01 好易康生物科技(广州)有限公司 Lysozyme oral care product for whitening teeth

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FR2651433A1 (en) * 1989-09-07 1991-03-08 Dana Dominique Enzyme complex having activity with respect to tartar and dental caries
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FR2651433A1 (en) * 1989-09-07 1991-03-08 Dana Dominique Enzyme complex having activity with respect to tartar and dental caries
EP1449513A1 (en) * 2003-02-19 2004-08-25 Sara Lee/DE N.V. Dental care product
CN105163705A (en) * 2013-02-14 2015-12-16 荷兰联合利华有限公司 Non-aqueous oral care compositions
CN105456041A (en) * 2015-12-11 2016-04-06 广州薇美姿实业有限公司 Toothpaste containing particles and transparent viscous substance

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"隆力奇DL复合酶牙膏对部分口腔微生物体外抑菌作用的实验研究";刘怡然等;《口腔生物医学》;20121231;第3卷(第4期);第205-207页 *

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