CN106691886B

CN106691886B - Toothpaste containing insoluble dietary fiber and sodium phytate and preparation method thereof

Info

Publication number: CN106691886B
Application number: CN201710073575.XA
Authority: CN
Inventors: 丁观军; 程吉平; 吴兴合
Original assignee: Hangzhou Jiaojie Oral Health Care Products Co ltd
Current assignee: Hangzhou Jiaojie Oral Health Care Products Co ltd
Priority date: 2017-02-10
Filing date: 2017-02-10
Publication date: 2020-04-21
Anticipated expiration: 2037-02-10
Also published as: CN106691886A

Abstract

Insoluble dietary fibers and sodium phytate have wide application in the oral care field. The toothpaste containing the insoluble dietary fibers and the sodium phytate has remarkable stain removing and cleaning capabilities, and has a better effect than the toothpaste added with the insoluble dietary fibers or the sodium phytate; under certain conditions, the toothpaste with the mass ratio of the insoluble dietary fiber to the sodium phytate being 8:2 has the best stain removal and cleaning capability, can avoid tooth abrasion caused by excessive use of high-friction raw materials, and is safer and more reliable. Therefore, the toothpaste containing the insoluble dietary fiber and the sodium phytate has good application prospect in the field of oral care products.

Description

Toothpaste containing insoluble dietary fiber and sodium phytate and preparation method thereof

Technical Field

The invention belongs to the technical field of daily chemicals, and particularly relates to toothpaste containing insoluble dietary fibers and sodium phytate and a preparation method thereof.

Background

In the oral environment, tooth stains are often mixed with extrinsic stains on the tooth surface, the formation of which is based on the acquired film. The saliva-acquired membrane is formed by selective adsorption of glycoproteins in saliva onto the tooth surface, and is a thin, cell-free, unstructured, homogeneous organic membrane, which is about a few microns thick. The acquired membrane contains amino acids, proteins, carbohydrates, lipids and other substances, and can be formed on the surfaces of fillings, dental calculus, restoration and appliance in the tooth surface and oral cavity through the action of ion charges. After the acquired membrane is formed, bacteria, dietary pigment such as tea, coffee, soy sauce and the like can be adhered to the acquired membrane to form tooth surface stains or tooth surface exogenous stains, and the acquired membrane has promotion on the occurrence and development of dental caries and periodontal diseases. Therefore, removing the stain on the tooth surface based on the acquired pellicle, reducing the pathogenic bacteria in the oral cavity, cleaning the oral cavity, and contributing to the prevention and treatment of caries and periodontal disease.

In general, consumers use whitening toothpaste to remove stains on the tooth surface with strong physical friction, and perform daily oral care. However, strong physical friction may cause damage to teeth in the mouth, such as small scratches, and may cause adverse effects such as tooth wear and caries over a long period of time. Therefore, research and development work has been continuously conducted to develop various toothpaste and toothbrush technologies such as high cleaning silica, spherical silica, and high density bristle brushing, which bring better cleaning effect and suitable physical friction performance, i.e. suitable rda (radio active dental ablation) value and read (radio active end ablation) value.

Among these different technologies, phytic acid, also known as phytic acid, is a clinically proven natural chemical stain removal and whitening active substance that can effectively reduce stains on tooth surfaces. Phytic acid is an organic phosphoric acid compound and has strong chelating capacity. It has 6 negative phosphate radicals, and can be effectively matched with protein molecules besides being combined with metal cations. Therefore, sodium phytate has high affinity with enamel surface, can affect adsorption and desorption of protein and pigment on enamel surface, can prevent stain or pigmentation, and helps to remove pigment and dental calculus. Meanwhile, the insoluble dietary fiber is found to be a food additive and an abrasive with certain cleaning capacity, so that the insoluble dietary fiber can be used for effectively removing stains on the tooth surface and ensuring the safety of the product. Therefore, the mutual matching use of the insoluble dietary fiber and the sodium phytate raw material in the toothpaste formula can have good application prospect in the aspects of toothpaste stain removal and cleaning.

Disclosure of Invention

The research focuses on the stain removing and Cleaning capability (PCR) of toothpaste with different ratios of insoluble dietary fibers and sodium phytate, so as to discover or invent the toothpaste with the optimal Ratio of the insoluble dietary fibers and the sodium phytate and the preparation method thereof. The insoluble fiber or insoluble dietary fiber refers to a fiber material which can not be dissolved in the toothpaste body and can keep the appearance.

In order to achieve the purpose, after a series of experiments, the technical scheme of the invention is as follows:

a toothpaste containing insoluble fiber and sodium phytate is characterized in that: the mass ratio range of the insoluble fiber to the sodium phytate is 20: 1-1: 4; the content of insoluble fiber in toothpaste is 1.0wt% or more; the content of the toothpaste abrasive except the insoluble fiber is 0-40%.

The toothpaste containing the insoluble fiber and the sodium phytate is characterized in that the insoluble fiber is dietary fiber.

The toothpaste containing the insoluble dietary fibers and the sodium phytate is characterized in that the insoluble dietary fibers are long-strip-shaped, the length-width ratio range is 3-40, and the length is more than 20 micrometers.

The toothpaste containing the insoluble dietary fibers and the sodium phytate is characterized in that the mass ratio of the insoluble dietary fibers to the sodium phytate ranges from 10:1 to 1: 2.

The toothpaste containing the insoluble dietary fibers and the sodium phytate is characterized in that the mass ratio of the insoluble dietary fibers to the sodium phytate is 8: 2-1: 1.

The toothpaste containing the insoluble dietary fibers and the sodium phytate is characterized by comprising the following components in percentage by mass:

2-20 wt% of insoluble dietary fiber,

0.5-10 wt% of sodium phytate,

0-40 wt% of other toothpaste abrasive,

0.02-8 wt% of thickening agent,

1-50 wt% of the humectant,

0.001-0.1 wt% of sweetening agent,

0.004-0.1 wt% of the bacteriostatic agent,

0-5 wt% of foaming agent,

0-2 wt% of fluoride,

0.3-3 wt% of essence,

0wt% -0.01 wt% of pigment.

The toothpaste containing insoluble dietary fibers and sodium phytate is characterized in that the other toothpaste abrasive is at least one of silicon dioxide, calcium hydrophosphate dihydrate or calcium carbonate; the thickening agent is at least one of carbomer, xanthan gum, carrageenan or sodium carboxymethylcellulose; the humectant is at least one of glycerol, sorbitol or polyethylene glycol 400; the sweetener is at least one of saccharin, sucralose or xylitol; the bacteriostatic agent is at least one of zinc citrate, sodium benzoate or methylparaben; the foaming agent is at least one of sodium dodecyl sulfate, cocamidopropyl betaine or sodium lauroyl sarcosinate; the essence is mint essence; the pigment is at least one of fruit green pigment, allure red pigment, brilliant blue pigment or lemon yellow pigment.

The toothpaste containing insoluble dietary fibers and sodium phytate is characterized in that a toothpaste formula comprises 40.0wt% of glycerin, 0.70wt% of carrageenan, 0.70wt% of xanthan gum, 4.00wt% of xylitol, 0.30wt% of sodium pyrophosphate, 0.05wt% of zinc citrate, 20wt% of calcium hydrogen phosphate dihydrate, 0.40wt% of essence, 8.0wt% of insoluble dietary fibers, 2.0 wt% of sodium phytate and the balance of deionized water.

The preparation method of the toothpaste containing the insoluble dietary fiber and the sodium phytate is characterized by comprising the following steps of: placing the components of the formula of the toothpaste in a stirrer to stir at 200-1000 rpm for 20-60 min; vacuum degassing to obtain paste.

Compared with the prior art, the technical scheme of the invention has the following advantages:

1. the toothpaste containing the insoluble dietary fibers and the sodium phytate provided by the embodiment of the invention has good stain removing and cleaning capabilities. When the toothpaste with the optimal ratio of the insoluble dietary fiber to the sodium phytate is used, the insoluble dietary fiber and the sodium phytate can act synergistically, so that tooth abrasion caused by excessive use of high-friction raw materials is avoided, and people can feel safer and more relieved.

2. The preparation method of the toothpaste disclosed by the invention is simple in process, uniform and stable in paste and easy to industrialize.

Drawings

Fig. 1 is a Scanning Electron Micrograph (SEM) of insoluble dietary fibers;

FIG. 2 is a bar graph of the coefficients of stain removing and cleaning ability (PCR,%) of each dentifrice (TP 1, TP2, TP3 and TP 4) in an in vitro stain removing and cleaning experiment (8 enamel samples per group). The english letters indicate the statistical difference between the groups of stain removing and cleaning ability coefficients for different toothpastes (p value <0.05 indicating that there is a significant difference between the two in the statistical t-test if the letters are indicated to be different).

Detailed Description

To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to the accompanying drawings and specific embodiments. This invention may be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete and will fully convey the concept of the invention to those skilled in the art, and the present invention will only be defined by the appended claims.

In the following examples, insoluble dietary fibers of micron size, length of about 100 microns and width of about 30 microns were used, which were off-spec, stringy, flexible, and had a morphology different from other hard abrasives calcium carbonate, disodium hydrogen phosphate, or silica (instrument characterization: scanning electron microscopy Hitachi S-3400N).

Toothpaste 1 is TP1

The embodiment provides toothpaste TP1, which comprises the following raw materials in percentage by mass: 40.0wt% of glycerol, 0.70wt% of carrageenan, 0.70wt% of xanthan gum, 4.00wt% of xylitol, 0.30wt% of sodium pyrophosphate, 0.05wt% of zinc citrate, 20wt% of calcium hydrophosphate dihydrate, 0.40wt% of essence, 10.0wt% of insoluble dietary fiber, 0.0wt% of sodium phytate and the balance of deionized water. The preparation method of the anhydrous toothpaste comprises the following steps:

s1, placing the components in a stirrer and stirring for 40min at 800 rpm;

and S2, degassing in vacuum to form paste.

Toothpaste 2 instant TP2

The embodiment provides toothpaste TP2, which comprises the following raw materials in percentage by mass: 40.0wt% of glycerol, 0.70wt% of carrageenan, 0.70wt% of xanthan gum, 4.00wt% of xylitol, 0.30wt% of sodium pyrophosphate, 0.05wt% of zinc citrate, 20wt% of calcium hydrophosphate dihydrate, 0.40wt% of essence, 8.0wt% of insoluble dietary fiber, 2.0 wt% of sodium phytate and the balance of deionized water. The preparation method of the anhydrous toothpaste comprises the following steps:

s1, placing the components in a stirrer and stirring for 40min at 800 rpm;

and S2, degassing in vacuum to form paste.

Toothpaste 3 instant TP3

The embodiment provides toothpaste TP3, which comprises the following raw materials in percentage by mass: 40.0wt% of glycerol, 0.70wt% of carrageenan, 0.70wt% of xanthan gum, 4.00wt% of xylitol, 0.30wt% of sodium pyrophosphate, 0.05wt% of zinc citrate, 20wt% of calcium hydrophosphate dihydrate, 0.40wt% of essence, 5.0wt% of insoluble dietary fiber, 5.0wt% of sodium phytate and the balance of deionized water. The preparation method of the anhydrous toothpaste comprises the following steps:

s1, placing the components in a stirrer and stirring for 40min at 800 rpm;

and S2, degassing in vacuum to form paste.

Toothpaste 4 i.e. TP4

The embodiment provides toothpaste TP4, which comprises the following raw materials in percentage by mass: 40.0wt% of glycerol, 0.70wt% of carrageenan, 0.70wt% of xanthan gum, 4.00wt% of xylitol, 0.30wt% of sodium pyrophosphate, 0.05wt% of zinc citrate, 20wt% of calcium hydrophosphate dihydrate, 0.40wt% of essence, 0.0wt% of insoluble dietary fiber, 10.0wt% of sodium phytate and the balance of deionized water. The preparation method of the anhydrous toothpaste comprises the following steps:

s1, placing the components in a stirrer and stirring for 40min at 800 rpm;

and S2, degassing in vacuum to form paste.

In vitro stain removal and cleaning experiment

Cutting healthy bovine teeth by using a low-speed diamond cutting machine (SYJ-160 low-speed diamond cutting machine), preparing enamel sheets (length is multiplied by width, 10 cm is multiplied by 10 cm) with the thickness of 3mm, and polishing and grinding the enamel sheets to be smooth on the surfaces by using silicon carbide water sand paper of 200 meshes, 400 meshes, 1000 meshes, 2000 meshes and 4000 meshes respectively; and finally polishing with 3M polishing paper (3 microns) for brightness, and ultrasonically cleaning in deionized water for 3 min. Appropriate enamel samples were selected for surface microhardness. The staining process of the teeth is specifically as follows: each enamel piece is fixed in transparent resin, the smooth enamel surface faces upwards, 1.0wt% hydrochloric acid aqueous solution is placed in the enamel piece to be soaked for 60s, then 0.25wt% phytic acid aqueous solution is placed in the enamel piece to be soaked for 60s, and finally deionized water is used for cleaning. Before tooth staining, 100mL of staining solution is prepared, and the components of the staining solution are as follows: 0.54g instant coffee, 0.54g ground black tea powder, 0.40g mucin, and the balance deionized water. The dyeing method comprises the following specific steps: the enamel resin pieces were all placed in a vessel containing staining solution and placed at 37^oC constant rate 150 rpm constant temperature Oscillator (THZ-98A)) For 4 days. During this period, the staining solution was replaced. And after dyeing treatment, taking out the dyed sample, washing the dyed sample with enough clear water, drying the dyed sample in air for 10min, and putting the dried dyed sample into a refrigerator for later use.

Before the treatment of brushing teeth, the L of enamel was measured using a NR10QC universal colorimeter₀Values (CIE standard color system, illuminant D65; five measurements each, averaged) were brushed on appropriate samples according to the results and divided into four groups of 8 samples each, corresponding to 4 toothpaste products. Subsequently, toothpaste slurries TP1, TP2, TP3 and TP4 containing 40g of toothpaste and 64g of deionized water, respectively, were prepared. The specific brushing tooth stain removing and cleaning process is as follows: placing the dyed sample into a tooth brushing machine for brushing teeth for 400 times, wherein the amount of the used toothpaste slurry is 10mL, the tooth brushing frequency is 60 times per minute, a high-density soft-bristle toothbrush (the diameter of the tip of a bristle is less than 0.01 mm) is adopted during tooth brushing, and the toothbrush bears 170 g; after brushing teeth, the tooth paste was rinsed thoroughly with deionized water to remove the toothpaste liquid from the surface, and L on the enamel surface was measured₁A value; finally, fully polishing with 3M polishing paper, removing residual stains on the surface, washing with deionized water, and measuring L of enamel again₂The value is obtained. At the end of the experiment, the stain removal and cleaning ability coefficients (PCR) of the toothpaste are respectively calculated according to the following formula:

PCR(%)=(L*₁-L*₀)/(L*₂-L*₀)×100

figure 2 is a bar graph of the stain removing cleaning power coefficient (PCR,%) of each toothpaste in vitro stain removing cleaning experiments (8 enamel samples per group). The english letters indicate the statistical difference between the groups of stain removing and cleaning ability coefficients for different toothpastes (p value <0.05 indicating that there is a significant difference between the two in the statistical t-test if the letters are indicated to be different).

In the in vitro tooth brushing and stain removing experiments, the stain removing and cleaning capacity coefficients of toothpaste TP1, TP2, TP3 and TP4 on enamel samples are 23.3 +/-7.8 (%), 45.9 +/-6.5 (%), 39.3 +/-6.0 (%) and 34.7 +/-5.4 (%), respectively, as shown in the figure 2. The cleaning power is arranged from strong to weak according to the stain removal, and the cleaning power is respectively toothpaste TP2, toothpaste TP3, toothpaste TP4 and toothpaste TP 1. In t-test statistical analysis of PCR values of different toothpastes, the stain-removing and cleaning abilities of the toothpaste TP1 are respectively and obviously different from the toothpaste TP2, TP3 and TP 4; there were no statistical differences between toothpaste TP2 and toothpaste TP3, nor between toothpaste TP3 and toothpaste TP 4; there was a significant difference between toothpaste TP2 and toothpaste TP 4. Therefore, the cleaning effect of the pure addition of the soft abrasive insoluble dietary fiber or the sodium phytate in the toothpaste formula is not as good as that of the two in a matching way; in the use of dietary fiber and sodium phytate, toothpaste TP2 containing 8.0% dietary fiber and 2.0% sodium phytate performed best. This suggests that the use of insoluble dietary fiber in combination with sodium phytate in a toothpaste containing a certain amount of dicalcium phosphate dihydrate may provide some positive and considerable stain removal cleansing benefits.

Stain removal cleaning of the experimental toothpaste was to remove the acquired enamel pellicle with associated stains or stains. These extrinsic stains on the tooth surface combined with the acquired membrane are often formed by drinking pigment-containing beverages and foods and smoking during daily life. The mechanism by which the experimental toothpaste removes extrinsic stains or stains from the tooth surface may include this: the sodium phytate has higher affinity with the surface of enamel, can weaken exogenous stains, the binding force between an acquired membrane and the surface of teeth, even can help to disintegrate the stains or stains on the surface of teeth, can prevent stains or pigments from being continuously deposited, and realizes the chemical stain removal and cleaning effect; meanwhile, the insoluble dietary fiber and the dicalcium phosphate dihydrate which are used as the abrasive can remove the tooth surface stains and acquired films with weak binding force with the tooth surface by the general physical cleaning capability, thereby realizing good physical stain removal cleaning effect. In the cleaning process of the abrasive, the abrasive calcium hydrophosphate dihydrate generally rubs with teeth in points or certain areas to form a strong friction cleaning effect; in contrast, insoluble dietary fibers may produce a cleansing effect in a direction perpendicular to their fiber longitudinal direction.

It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.

Claims

1. A toothpaste containing insoluble fiber and sodium phytate is characterized in that:

the toothpaste formula comprises 40.0wt% of glycerol, 0.70wt% of carrageenan, 0.70wt% of xanthan gum, 4.00wt% of xylitol, 0.30wt% of sodium pyrophosphate, 0.05wt% of zinc citrate, 20wt% of calcium hydrophosphate dihydrate, 0.40wt% of essence, 8.0wt% of insoluble dietary fiber, 2.0 wt% of sodium phytate and the balance of deionized water;

the insoluble fiber is a food-grade raw material and is dietary fiber;

the insoluble dietary fiber is in a strip shape, the length-width ratio range is 3-40, and the length is larger than 20 micrometers.

2. A method of preparing the toothpaste of claim 1, comprising the steps of:

placing the components of the formula of the toothpaste in a stirrer to stir at 200-1000 rpm for 20-60 min;

vacuum degassing to obtain paste.