CN105686979B - A kind of fulvic acid toothpaste and preparation method thereof - Google Patents

A kind of fulvic acid toothpaste and preparation method thereof Download PDF

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Publication number
CN105686979B
CN105686979B CN201610150070.4A CN201610150070A CN105686979B CN 105686979 B CN105686979 B CN 105686979B CN 201610150070 A CN201610150070 A CN 201610150070A CN 105686979 B CN105686979 B CN 105686979B
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fulvic acid
toothpaste
raw material
acid
pigment
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CN105686979A (en
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丁观军
程吉平
吴兴合
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HANGZHOU JIAOJIE ORAL HEALTH CARE PRODUCTS CO Ltd
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HANGZHOU JIAOJIE ORAL HEALTH CARE PRODUCTS CO Ltd
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    • 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
    • A61K8/965—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution of inanimate origin
    • 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
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/36—Carboxylic acids; Salts or anhydrides 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
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/37—Esters of carboxylic acids
    • 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

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

Abstract

The invention discloses a kind of fulvic acid toothpaste and preparation method thereof, the fulvic acid toothpaste includes the raw material of following mass fraction: 1.0~20.0 parts of fulvic acid, 0.03-3 parts of bacteriostatic agent.The preparation method of the fulvic acid toothpaste includes the following steps: S1, the raw material is placed in 200rpm~1000rpm stirring 20min~60min in blender；S2, vacuum outgas are at paste.The fulvic acid formulation of tooth-paste is reasonable, simple process, and lotion is uniform and stable, it is easy to industrialization, fulvic acid is added, lactobacillus bulgaricus, streptococcus thermophilus and lactobacillus acidophilus can be inhibited in intraoral production acid, make tooth from the erosion of acid, and the destruction to enamel.

Description

A kind of fulvic acid toothpaste and preparation method thereof
Technical field
The invention belongs to chemical product technical fields, and in particular to a kind of to inhibit lactobacillus bulgaricus, streptococcus thermophilus The fulvic acid toothpaste and preparation method thereof of acid is produced in oral cavity with lactobacillus acidophilus.
Background technique
Toothpaste is a kind of common daily necessities, for cleaning oral cavity tooth-whitening or preventing odontopathy (similar In saprodontia).The etiology of dental caries theory of existing mainstream is tetrad factor theory, specifically include bacterium, oral environment, host and when Between.In etiology, origin is that cariogenicity food ingredients (comprising sucrose and purification carbohydrate etc.) are tightly attached to tooth Tooth surface forms biomembrane with sialoprotein.This biomembrane can stick securely and be attached to dental surface.In suitable temperature Under, intraoral pathogenic bacteria can be adhered on biomembrane and form bacterial plaque, generate low ph environment by bacterial plaque, make enamel hydroxyl Base apatite is decomposed, and is invaded tooth, and then destroy tooth organic matter, is generated cavity.Bacterium is the pathogenetic necessary item of dental caries Part.Common cariogenic bacterium includes streptococcus, lactobacillus and actinomyces.Its main pathogenic bacteria of decayed tooth includes deformation chain Coccus, lactobacillus acidophilus etc..Streptococcus mutans can decompose glucide and generate acidic environment of the pH 4.5 or so；Acidophilus cream Bacillus and streptococcus thermophilus etc. are then common in Yoghourt, can produce in the case where there is enough carbohydrates (sucrose, lactose etc.) Acidic environment of the raw pH 3.0 or so.The mechanism of action of Chinese medicine preventing decayed tooth be inhibit pathogenic bacteria growth, inhibit pathogenic bacteria produce acid, Inhibit bacterium glycosyl transferase and transposon mutagenesis, influence the formation of plaque bio-film and promotes the biological mine of hard tooth tissue Change, wherein main research contents is the production acid for inhibiting the growth of pathogenic bacteria and inhibiting pathogenic bacteria.How to avoid in food beverage It is one extremely important that residue (lactobacillus acidophilus etc.), which leads to the problem of acidic materials in oral cavity and corrodes tooth,.
Chinese patent literature CN103536496A discloses a kind of toothpaste and preparation method thereof.Its constituent and weight percent Than are as follows: puerh tea leaves extract 3%-7%, notoginseng leaf extract 4%-8%, fulvic acid 5%-10%, surplus are auxiliary material.Pass through Oral helicobacter pylori can pointedly be inhibited using puerh tea leaves extract and notoginseng leaf extract, few side effects are suitable for length Phase uses, good using fulvic acid antiphlogistic effects in constituent, prevents and treats recurrent oral ulceration.
In above patent document, mainly inhibit oral cavity helicobacter pylorus using puerh tea leaves extract and notoginseng leaf extract Bacterium, and fulvic acid is being wherein to play anti-inflammatory, prevention and treatment recurrent oral ulceration, although fulvic acid can play certain resist Scorching, prevention and treatment recurrent oral ulceration effect, but effect is poor, and and has no that fulvic acid inhibits pathogenic bacteria to produce acid aspect Report.
Summary of the invention
For this purpose, technical problem to be solved by the present invention lies in food or beverage residue can lactobacillus bulgaricus, The technical issues of acid is produced under the action of streptococcus thermophilus and lactobacillus acidophilus in oral cavity, tooth can be corroded, destroy enamel, from And provide a kind of Huang that can pointedly inhibit lactobacillus bulgaricus, streptococcus thermophilus and lactobacillus acidophilus to produce acid in oral cavity Rotten acid toothpaste and preparation method thereof.
To achieve the above object, the technical solution of the present invention is as follows:
A kind of fulvic acid toothpaste of the present invention, the raw material including following mass fraction:
1.0~20.0 parts of fulvic acid
0.03-3 parts of bacteriostatic agent.
Further, the fulvic acid toothpaste includes the raw material of following mass fraction:
3.0~20.0 parts of fulvic acid
0.03-3 parts of bacteriostatic agent.
Further, the fulvic acid toothpaste includes the raw material of following mass fraction:
7.0~20.0 parts of fulvic acid
0.03-3 parts of bacteriostatic agent.
The bacteriostatic agent is at least one of zinc citrate, sodium benzoate, methylparaben.
The fulvic acid toothpaste further include rubbing agent, thickener, moisturizer, sweetener, foaming agent, toothpaste essence, pigment, At least one of fluorine compounds.
Further, the fulvic acid toothpaste includes the raw material of following mass fraction:
The rubbing agent is at least one of silica (such as hydrated silica), calcium phosphate dibasic dihydrate, calcium carbonate；
The thickener is at least one of xanthan gum, carragheen, sodium carboxymethylcellulose；
The moisturizer is at least one of glycerol, sorbierite, polyethylene glycol (such as polyethylene glycol 400)；
The sweetener is at least one of saccharin, Sucralose, xylitol；
The foaming agent be lauryl sodium sulfate, Cocoamidopropyl betaine, in sodium lauroyl sarcosine at least It is a kind of；The toothpaste essence is Mint Essence；
The pigment is at least one of light green pigment, allured red pigment, bright blue pigment, lemon yellow pigment, pearl powder； The fluorine compounds are sodium fluoride and/or sodium monofluorophosphate.
Preferably, the fulvic acid toothpaste includes the raw material of following mass fraction:
The pH < 8.0 of the fulvic acid toothpaste.
The present invention also provides the preparation methods of above-mentioned fulvic acid toothpaste, include the following steps:
S1, the raw material is placed in 200rpm~1000rpm stirring 20min~60min in blender；
S2, vacuum outgas are at paste.
Compared with prior art, the invention has the following beneficial effects:
1, fulvic acid toothpaste described in the embodiment of the present invention comprising the raw material of following mass fraction: fulvic acid 1.0~ 20.0 parts；0.03-3 parts of bacteriostatic agent.The fulvic acid toothpaste when in use, can act synergistically between fulvic acid and bacteriostatic agent, And inventor is had found by a large amount of creative works, by using fulvic acid, and limits the quality of fulvic acid and bacteriostatic agent Than for 1.0~20.0:0.03-3, obtained fulvic acid toothpaste can targetedly inhibit lactobacillus bulgaricus, thermophilus Bacterium and lactobacillus acidophilus produce acid in oral cavity, to make tooth from the erosion of acid, and the destruction to enamel.
2, fulvic acid toothpaste described in the embodiment of the present invention comprising the raw material of following mass fraction: fulvic acid 7.0~ 20.0 parts；0.03-3 parts of bacteriostatic agent.Inventor has found that under aforementioned proportion, fulvic acid toothpaste not only can by creative work Effectively lactobacillus bulgaricus, streptococcus thermophilus and lactobacillus acidophilus is inhibited to produce acid in oral cavity, to make tooth from acid It corrodes, and the destruction to enamel；And can also effectively stable tooth micro-vickers hardness, take care of one's teeth.
3, fulvic acid toothpaste described in the embodiment of the present invention, bacteriostatic agent are zinc citrate, in sodium benzoate, methylparaben At least one.Inventor has found that above-mentioned bacteriostatic agent can make to act synergistically between fulvic acid and bacteriostatic agent by creative work More preferably.
4, the preparation method of fulvic acid toothpaste described in the embodiment of the present invention, simple process, lotion is uniform and stable, is easy to produce Industry.
Detailed description of the invention
Fig. 1 is variation diagram before and after the antibacterial enamel microhardness produced in acid experiment of different proportion fulvic acid toothpaste.
Specific embodiment
Purposes, technical schemes and advantages in order to better illustrate the present invention, below in conjunction with the drawings and specific embodiments The present invention is described further.The present invention can be embodied in many different forms, and should not be construed as limited to herein The embodiment of elaboration.On the contrary, these embodiments are provided, so that the disclosure will be thorough and complete, and will be of the invention Design is fully conveyed to those skilled in the art, and the present invention will only be defined by the appended claims.
Embodiment 1
Fulvic acid toothpaste provided by the present embodiment is made of following raw materials according by percentage to the quality:
Sorbierite 55%, hydrated silica 16%, polyethylene glycol 400 5%, lauryl sodium sulfate 1.8%, carragheen 1%, saccharin 0.18%, zinc citrate 0.05%, Mint Essence 0.08%, light green pigment 0.005%, pearl powder 0.02%, Huang Rotten acid 1.00%, deionized water surplus.
The preparation method of corresponding fulvic acid toothpaste, includes the following steps:
S1, the raw material is placed in 200rpm stirring 60min in blender；
S2, vacuum outgas are at paste.
Above-mentioned fulvic acid toothpaste is denoted as toothpaste a, tests through pH, and the pH of toothpaste a is 7.0.
Embodiment 2
Fulvic acid toothpaste provided by the present embodiment is made of following raw materials according by percentage to the quality:
Sorbierite 55%, hydrated silica 16%, polyethylene glycol 400 5%, lauryl sodium sulfate 1.8%, carragheen 1%, saccharin 0.18%, zinc citrate 0.05%, Mint Essence 0.08%, allured red pigment 0.005%, pearl powder 0.02%, Fulvic acid 3.00%, deionized water surplus.
The preparation method of corresponding fulvic acid toothpaste, includes the following steps:
S1, the raw material is placed in 700rpm stirring 30min in blender；
S2, vacuum outgas are at paste.
Above-mentioned fulvic acid toothpaste is denoted as toothpaste b, tests through pH, and the pH of toothpaste b is 7.2.
Embodiment 3
Fulvic acid toothpaste provided by the present embodiment is made of following raw materials according by percentage to the quality:
Sorbierite 55%, hydrated silica 16%, polyethylene glycol 400 5%, lauryl sodium sulfate 1.8%, carragheen 1%, saccharin 0.18%, zinc citrate 0.05%, Mint Essence 0.08%, bright blue pigment 0.005%, pearl powder 0.02%, Huang Rotten acid 7.00%, deionized water surplus.
The preparation method of corresponding fulvic acid toothpaste, includes the following steps:
S1, the raw material is placed in 1000rpm stirring 20min in blender；
S2, vacuum outgas are at paste.
Above-mentioned fulvic acid toothpaste is denoted as toothpaste c, tests through pH, and the pH of toothpaste c is 7.1.
Embodiment 4
Fulvic acid toothpaste provided by the present embodiment is made of following raw materials according by percentage to the quality:
Sorbierite 55%, hydrated silica 16%, polyethylene glycol 400 5%, lauryl sodium sulfate 1.8%, carragheen 1%, saccharin 0.18%, zinc citrate 0.05%, Mint Essence 0.08%, lemon yellow pigment 0.005%, pearl powder 0.02%, Fulvic acid 15.00%, deionized water surplus.
The preparation method of corresponding fulvic acid toothpaste, includes the following steps:
S1, the raw material is placed in 500rpm stirring 40min in blender；
S2, vacuum outgas are at paste.
Above-mentioned fulvic acid toothpaste is denoted as toothpaste d, tests through pH, and the pH of toothpaste d is 7.0.
Embodiment 5
Fulvic acid toothpaste provided by the present embodiment is made of following raw materials according by percentage to the quality:
Sorbierite 55%, hydrated silica 16%, polyethylene glycol 400 5%, lauryl sodium sulfate 1.8%, carragheen 1%, saccharin 0.18%, zinc citrate 0.05%, Mint Essence 0.08%, light green pigment 0.005%, pearl powder 0.02%, Huang Rotten acid 20.00%, deionized water surplus.
The preparation method of corresponding fulvic acid toothpaste, includes the following steps:
S1, the raw material is placed in 400rpm stirring 50min in blender；
S2, vacuum outgas are at paste.
Above-mentioned fulvic acid toothpaste is denoted as toothpaste e, tests through pH, and the pH of toothpaste e is 7.1.
Embodiment 6
Fulvic acid toothpaste provided by the present embodiment is made of following raw materials according by percentage to the quality:
Sorbierite 55%, hydrated silica 16%, polyethylene glycol 400 5%, lauryl sodium sulfate 1.8%, carragheen 1%, saccharin 0.18%, zinc citrate 2.0%, Mint Essence 0.08%, allured red pigment 0.005%, pearl powder 0.02%, Huang Rotten acid 7.00%, deionized water surplus.
The preparation method of corresponding fulvic acid toothpaste, includes the following steps:
S1, the raw material is placed in 200rpm stirring 60min in blender；
S2, vacuum outgas are at paste.
It is tested through pH, fulvic acid toothpaste pH made from the present embodiment is 7.3.
Embodiment 7
Fulvic acid toothpaste provided by the present embodiment is made of following raw materials according by percentage to the quality:
Sorbierite 55%, hydrated silica 16%, polyethylene glycol 400 5%, lauryl sodium sulfate 1.8%, carragheen 1%, saccharin 0.18%, zinc citrate 3.0%, Mint Essence 0.08%, bright blue pigment 0.005%, pearl powder 0.02%, yellow corruption Sour 3.00%, deionized water surplus.
The preparation method of corresponding fulvic acid toothpaste, includes the following steps:
S1, the raw material is placed in 500rpm stirring 30min in blender；
S2, vacuum outgas are at paste.
It is tested through pH, fulvic acid toothpaste pH made from the present embodiment is 7.1.
Embodiment 8
Fulvic acid toothpaste provided by the present embodiment is made of following raw materials according by percentage to the quality:
Sorbierite 55%, hydrated silica 16%, polyethylene glycol 400 5%, lauryl sodium sulfate 1.8%, carragheen 1%, saccharin 0.18%, sodium benzoate 0.03%, Mint Essence 0.08%, lemon yellow pigment 0.005%, pearl powder 0.02%, Fulvic acid 15.00%, deionized water surplus.
The preparation method of corresponding fulvic acid toothpaste, includes the following steps:
S1, the raw material is placed in 800rpm stirring 25min in blender；
S2, vacuum outgas are at paste.
It is tested through pH, fulvic acid toothpaste pH is about 7.0 made from the present embodiment.
Embodiment 9
Fulvic acid toothpaste provided by the present embodiment is made of following raw materials according by percentage to the quality:
Sorbierite 55%, hydrated silica 16%, polyethylene glycol 400 5%, lauryl sodium sulfate 1.8%, carragheen 1%, saccharin 0.18%, methylparaben 1.5%, Mint Essence 0.08%, lemon yellow pigment 0.005%, pearl powder 0.02%, Fulvic acid 15.00%, deionized water surplus.
The preparation method of corresponding fulvic acid toothpaste, includes the following steps:
S1, the raw material is placed in 300rpm stirring 55min in blender；
S2, vacuum outgas are at paste.
It is tested through pH, fulvic acid toothpaste pH is about 7.0 made from the present embodiment.
Embodiment 10
Fulvic acid toothpaste provided by the present embodiment is made of following raw materials according by percentage to the quality:
Sorbierite 55%, hydrated silica 16%, polyethylene glycol 400 5%, lauryl sodium sulfate 1.8%, carragheen 1%, saccharin 0.18%, methylparaben 1.5%, Mint Essence 0.08%, allured red pigment 0.005%, pearl powder 0.02%, Fulvic acid 15.00%, sodium fluoride 0.15%, deionized water surplus.
The preparation method of corresponding fulvic acid toothpaste, includes the following steps:
S1, the raw material is placed in 300rpm stirring 55min in blender；
S2, vacuum outgas are at paste.
It is tested through pH, fulvic acid toothpaste pH is about 7.0 made from the present embodiment.
Comparative example 1
Toothpaste provided by this comparative example is made of following raw materials according by percentage to the quality:
Sorbierite 55%, hydrated silica 16%, polyethylene glycol 400 5%, lauryl sodium sulfate 1.8%, carragheen 1%, saccharin 0.18%, zinc citrate 0.05%, Mint Essence 0.08%, light green pigment 0.005%, pearl powder 0.02%, Huang Rotten acid 0.00%, deionized water surplus.
The preparation method of corresponding fulvic acid toothpaste, includes the following steps:
S1, the raw material is placed in 200rpm stirring 60min in blender；
S2, vacuum outgas are at paste.
Above-mentioned fulvic acid toothpaste is denoted as toothpaste f, tests through pH, and the pH of toothpaste f is 7.2.
Comparative example 2
Fulvic acid toothpaste provided by this comparative example is made of following raw materials according by percentage to the quality:
Sorbierite 55%, hydrated silica 16%, polyethylene glycol 400 5%, lauryl sodium sulfate 1.8%, carragheen 1%, saccharin 0.18%, Mint Essence 0.08%, lemon yellow pigment 0.005%, pearl powder 0.02%, fulvic acid 3.05%, go Ion water surplus.
The preparation method of corresponding fulvic acid toothpaste, includes the following steps:
S1, the raw material is placed in 1000rpm stirring 20min in blender；
S2, vacuum outgas are at paste.
It is tested through pH, the pH of fulvic acid toothpaste made from this comparative example is 7.0.
Comparative example 3
Fulvic acid toothpaste provided by this comparative example is made of following raw materials according by percentage to the quality:
Sorbierite 55%, hydrated silica 16%, polyethylene glycol 400 5%, lauryl sodium sulfate 1.8%, carragheen 1%, saccharin 0.18%, zinc citrate 0.02%, Mint Essence 0.08%, lemon yellow pigment 0.005%, pearl powder 0.02%, Fulvic acid 3.03%, deionized water surplus.
The preparation method of corresponding fulvic acid toothpaste, includes the following steps:
S1, the raw material is placed in 1000rpm stirring 20min in blender；
S2, vacuum outgas are at paste.
It is tested through pH, the pH of fulvic acid toothpaste made from this comparative example is 7.0.
Comparative example 4
Fulvic acid toothpaste provided by this comparative example is made of following raw materials according by percentage to the quality:
Sorbierite 55%, hydrated silica 16%, polyethylene glycol 400 5%, lauryl sodium sulfate 1.8%, carragheen 1%, saccharin 0.18%, Mint Essence 0.08%, lemon yellow pigment 0.005%, pearl powder 0.02%, fulvic acid 7.00%, go Ion water surplus.
The preparation method of corresponding fulvic acid toothpaste, includes the following steps:
S1, the raw material is placed in 1000rpm stirring 20min in blender；
S2, vacuum outgas are at paste.
It is tested through pH, the pH of fulvic acid toothpaste made from this comparative example is 7.0.
Carrying out toothpaste sample to above-mentioned each embodiment and comparative example inhibits bacterium to produce acid experiment:
Experimental material: easy extremely excellent yogurt powder (including lactobacillus bulgaricus, streptococcus thermophilus and lactobacillus acidophilus) is purchased from Know this Biotechnology Co., Ltd in Hangzhou；Mouthsimulator saliva: the allotment of Mouthsimulator saliva laboratory, specific ingredient are as follows: 137.35 mMNaCl、4.17mM NaHCO3、3.01mMKCl、7.17mM K2HPO4·3H2O、1.53mM MgCl2·6H2O、 20.00mMHCl、0.90mM CaCl2、0.51mM Na2SO4With Tris tune pH value to 7.0；Baurodont: the baurodont collected from market, It sufficiently cleans up to be put into 0.5% thymol aqueous solution and save；Long 3mm, width are prepared using low-speed diamond cutting machine The enamel thin slice of 3mm, thickness 1.5mm, then the silicon carbide water sand paper polishing through 200,400,1000,2000 and 4000 mesh is beaten respectively It is smooth to be milled to surface-brightening；It is finally polished smooth with 3M polishing paper (3 microns), and is cleaned by ultrasonic 3min in deionized water, it is spare.
Laboratory apparatus: microhardness tester (vickers hardness test method, load 500gf, load-time 15s) tests enamel tooth Piece screens high-quality tooth piece, is randomized into 7 groups, every group 5.
In toxicology, the amount of paste that the National People's Congress about consumes daily is 2.75g, remains 5% after rinsing.Daily human mouth Interior, the capacity of primary existing saliva is 9 milliliters or so.Therefore assume that toothpaste can uniformly remain in dental surface, not consider other If special circumstances, toothpaste is 0.1375g toothpaste/9mL saliva, i.e. 0.6875g toothpaste/45mL saliva in intraoral concentration. Experimental program is established according to this.Before experiment starts, experimental ware, enamel and Mouthsimulator saliva used sterilize in the UV lamp to be gone out Bacterium 2h.Experiment process is carried out in 100 grades of clean work stations, specific as follows: by 0.6875g Mouthsimulator saliva (blank sample), Toothpaste obtained is respectively put into the plastic bottle that capacity is 48mL in embodiment 1-5, comparative example 1-4, is then all put into 1.0g Yoghourt Powder and 45mL Mouthsimulator saliva are uniformly mixed with glass bar, and pH value determination (for 6.8 ± 0.2), finally sealed is saved in 37 DEG C Insulating box is placed for 24 hours.Experiment terminates, and with the pH value of pH meter measurement all samples, enamel piece is also taken out, and it is micro- hard to measure its Degree obtains its micro-vickers hardness changing value (after ▽ HV=processing-processing before).
It can be observed from Fig. 1: by Mouthsimulator saliva (blank sample), toothpaste f (comparative example 1), toothpaste a (embodiment 1), 2 toothpaste of comparative example, 3 toothpaste of comparative example, toothpaste b (embodiment 2), 4 toothpaste of comparative example, toothpaste c (embodiment 3), toothpaste d are (real Apply example 4) and toothpaste e (embodiment 5) processing for 24 hours after, the pH value of solution/suspension becomes 3.62,4.30,4.60,4.64 respectively, 4.65,4.68,4.72,4.79,4.90 and 4.92, the microhardness of enamel be -168.5 ± 83.8HV, -87.1 ± 15.7HV、-28.9±18.2HV、-22.0±6.3HV、-17.9±7.6HV、-8.4±24.8HV、0.3±3.9HV、5.0± 9.2HV, 3.3 ± 18.6HV and 3.2 ± 7.3HV.So when the not protection of toothpaste sample, blank sample pH value of solution is 3.62, enamel microhardness also declines nearly 60%, illustrates that enamel is acted on by significant acid attack；When control toothpaste f sample When the protection of product or low concentration fulvic acid toothpaste sample, sample solution pH is higher than blank sample, illustrates the addition of fulvic acid not But without increasing sample solution pH, its pH is reduced instead, to illustrate fulvic acid and bacteriostatic agent interaction, reduces sample The pH of solution, but enamel microhardness still declines, and illustrates that there are still acid attack effects in enamel face；When fulvic acid concentration is When 3.0%, sample solution pH is 4.68, and enamel microhardness that treated is suitable with normal enamel piece, illustrates fulvic acid Obviously inhibit lactobacillus bulgaricus in yogurt powder, acid caused by streptococcus thermophilus and lactobacillus acidophilus to enamel piece Corrosion, protects tooth；Especially when fulvic acid concentration be 7.0wt%-20wt% when, sample solution pH value be maintained at 4.79 and More than it, treated, and enamel piece micro-vickers hardness is also preceding on the same level or higher than being in handling, and illustrates tooth Enamel is not only by acid attack, and there are also a degree of enhancings for hardness.
Comparative analysis comparative example 1,2,3,4 and when the effect of toothpaste a, b, toothpaste b prepared by discovery embodiment 2 (contains 0.05% zinc citrate and 3.00% fulvic acid) than toothpaste made from comparative example 3 (containing 0.02% and 3.030% fulvic acid) or right Toothpaste made from ratio 2 (containing 3.05% fulvic acid) is more preferable；Embodiment 1 is more preferable than comparative example 1；Embodiment 3 is more than comparative example 4 It is good；By the comparison of 2 three of comparative example 1, comparative example 2 and embodiment, also turn out that experiment effect is not that bacteriostatic agent and fulvic acid are independent The effect of superposition, so zinc citrate and fulvic acid can (mass ratio of fulvic acid and bacteriostatic agent be in the framework of the present definition 1.0~20.0:0.03-3, especially 3.0~20.0:0.05-3) in have mutual synergistic effect, inhibit bacterium production acid, protect tooth Tooth.
Similarly, the obtained fulvic acid toothpaste in embodiment 6- embodiment 10 is tested respectively using above-mentioned test method, Treated, and enamel piece micro-vickers hardness is also preceding on the same level or higher than being in handling, and illustrates enamel not only Not by acid attack, and there are also a degree of enhancings for hardness.
Obviously, the above embodiments are merely examples for clarifying the description, and does not limit the embodiments.It is right For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or It changes.There is no necessity and possibility to exhaust all the enbodiments.And it is extended from this it is obvious variation or It changes still within the protection scope of the invention.

Claims (5)

1. a kind of fulvic acid toothpaste, is made of the raw material of following mass fraction:
The bacteriostatic agent is zinc citrate or sodium benzoate.
2. fulvic acid toothpaste according to claim 1, it is characterised in that: the rubbing agent is silica, two hydration phosphorus At least one of sour hydrogen calcium, calcium carbonate；
The thickener is at least one of xanthan gum, carragheen, sodium carboxymethylcellulose；
The moisturizer is at least one of glycerol, sorbierite, polyethylene glycol；
The sweetener is at least one of saccharin, Sucralose, xylitol；
The foaming agent is at least one of lauryl sodium sulfate, Cocoamidopropyl betaine, sodium lauroyl sarcosine；
The toothpaste essence is Mint Essence；
The pigment is at least one of light green pigment, allured red pigment, bright blue pigment, lemon yellow pigment, pearl powder；
The fluorine compounds are sodium fluoride and/or sodium monofluorophosphate.
3. fulvic acid toothpaste according to claim 2, it is characterised in that: the raw material including following mass fraction:
4. fulvic acid toothpaste according to claim 3, it is characterised in that: the pH < 8.0 of the fulvic acid toothpaste.
5. a kind of preparation method of fulvic acid toothpaste of any of claims 1-4, includes the following steps:
S1, the raw material is placed in 200rpm~1000rpm stirring 20min~60min in blender；
S2, vacuum outgas are at paste.
CN201610150070.4A 2016-03-16 2016-03-16 A kind of fulvic acid toothpaste and preparation method thereof Expired - Fee Related CN105686979B (en)

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