CN113274320A

CN113274320A - Toothpaste and preparation method thereof

Info

Publication number: CN113274320A
Application number: CN202110383621.2A
Authority: CN
Inventors: 李琼; 林晓晨
Original assignee: Yunnan Nuote Jinshen Oral Care Products Co ltd
Current assignee: Yunnan Nuote Jinshen Oral Care Products Co ltd
Priority date: 2021-04-09
Filing date: 2021-04-09
Publication date: 2021-08-20

Abstract

The invention discloses toothpaste which comprises the following raw materials in percentage by weight: 0.03-0.5% of panax notoginseng saponins, 0.05-0.5% of panax notoginseng extract, 25-50% of friction agent, 20-55% of wetting agent, 1.5-2.5% of foaming agent, 1.2-1.5% of adhesive, 0.15-0.3% of stabilizing agent, 0.1-0.3% of preservative, 0.25-0.35% of sweetening agent, 1-1.2% of essence and the balance of water. The invention also provides a preparation method of the toothpaste. The toothpaste provided by the invention can realize the two-way regulation of hemostasis and blood circulation promotion, can permeate into extravasated blood generated by cleaning focus parts while stopping bleeding, has the obvious effects of anticoagulation and platelet aggregation inhibition, and has the effect of stopping bleeding without leaving extravasated blood. The preparation method is simple to operate, and the maximum exertion of the effects of the components can be realized.

Description

Toothpaste and preparation method thereof

Technical Field

The invention relates to the technical field of oral care, in particular to toothpaste and a preparation method thereof.

Background

Tooth cleaning is important for making teeth beautiful, protecting gum health and preventing halitosis, toothpaste is one of tooth cleaning products, generally in the form of gel, and is usually applied to a toothbrush, the surfaces of the teeth are cleaned by means of mechanical friction of the toothbrush, and the teeth and the periphery thereof are cleaned to make the oral cavity clean and fresh, and toothpaste is a necessity of human daily life at present.

Toothpastes are complex mixtures that are generally composed of abrasive agents, humectants, surfactants, binders, flavors, sweeteners, and other specific ingredients. In order to prevent and treat oral diseases, some special components are added into some toothpaste, so that the toothpaste has the treatment effect of medicines, and is also called as functional toothpaste. The existing functional toothpaste mainly comprises antibacterial and anti-inflammatory toothpaste, antiallergic toothpaste, detergent whitening toothpaste, deodorant toothpaste, anticarious and desensitization toothpaste, antibacterial and anti-inflammatory toothpaste, blood circulation promoting and stasis removing toothpaste and metabolism improving toothpaste.

At present, toothpaste for promoting blood circulation to remove blood stasis and improving metabolism has various types, but most toothpaste has the efficacy of unidirectional regulation, such as only used for promoting blood circulation to remove blood stasis or only used for stopping bleeding, and can not effectively prevent and protect health aiming at symptoms of gingival bleeding.

Disclosure of Invention

One of the objects of the present invention is to overcome the disadvantages of the prior art, thereby providing a toothpaste which has the effects of inhibiting gingival inflammation and gingival bleeding on the basis of the basic functions of oral cavity cleaning and breath freshening; can permeate into extravasated blood generated by cleaning focus parts while stopping bleeding, has obvious anticoagulation and platelet aggregation inhibition effects, can realize the bidirectional regulation effects of stopping bleeding and activating blood, and achieves the aim of stopping bleeding without leaving blood stasis.

The invention also aims to provide a preparation method which is simple to operate and can realize the maximum exertion of the effects of all the components.

In order to achieve the above purpose, the invention provides the following technical scheme:

the toothpaste comprises the following raw materials in percentage by weight:

0.03-0.5% of panax notoginseng saponins, 0.05-0.5% of panax notoginseng extract, 25-50% of friction agent, 20-55% of wetting agent, 1.5-2.5% of foaming agent, 1.2-1.5% of adhesive, 0.15-0.3% of stabilizing agent, 0.1-0.3% of preservative, 0.25-0.35% of sweetening agent, 1-1.2% of essence and the balance of water.

As an implementation mode, the panax notoginseng saponins are prepared by a macroporous resin method.

As an implementable mode, the preparation method of the dencichine extract comprises the following steps:

s1, extracting Notoginseng radix with water for more than two times, and mixing the filtrates to obtain extractive solution;

s2, centrifuging the leaching solution, and concentrating the centrifuged supernatant to obtain a concentrated solution;

s3, adding ethanol into the concentrated solution, standing and performing suction filtration to obtain filtrate, and heating and concentrating the filtrate to obtain the dencichine extract.

As an implementable mode, the relative density of the dencichine extract is not less than 1.35g/cm at 50 DEG C³。

As a practical way, the abrasive is in dibasic calcium phosphate dihydrate and/or hydrated silica.

As a practical way, the humectant is glycerin and/or sorbitol.

As a practical way, the foaming agent is sodium lauryl sulfate.

As an implementation mode, the binder is one or more of sodium carboxymethylcellulose, hydroxyethyl cellulose, xanthan gum, guar gum and carrageenan.

As a practical way, the stabilizer is one or more of tetrasodium pyrophosphate, sodium dihydrogen phosphate and trisodium phosphate.

As a practical way, the preservative is sodium benzoate; the sweetener is saccharin sodium.

A preparation method of the toothpaste comprises the following steps:

(1) adding the panax notoginseng saponins, the dencichine extract, the sweetening agent and the stabilizing agent into deionized water, mixing and dissolving to obtain an aqueous solution;

(2) mixing and stirring the friction agent, the adhesive, the foaming agent and the preservative to obtain powder;

(3) sucking the aqueous solution and the wetting agent into a paste making machine by using negative pressure, and stirring in a vacuum state;

(4) and adjusting the pressure of the paste making machine, sequentially adding the powder and the essence, mixing and stirring, and then grinding and degassing to form paste.

As an implementable manner, the addition manner of the powder in the step (4) is: adding the mixture when the pressure of the paste making machine is adjusted to-0.04 MPa to-0.06 MPa, and continuously stirring for 25-30min under the vacuum degree of-0.094 to-0.097 MPa of the paste making machine, wherein the stirring speed is 950-1050 r/min.

As a practical way, after the essence is added in the step (4), stirring is carried out for 20-25min at the rotating speed of 950-1050 r/min.

Notoginseng, also known as "jin Bu Shi", is the dry root and rhizome of Panax notoginseng belonging to Araliaceae. It is recorded in compendium of materia Medica for the earliest time and has the efficacy of stopping bleeding, removing blood stasis, relieving swelling and pain. The pseudo-ginseng is a small compound, contains various active ingredients, and different ingredients play different roles in different pathological states, thereby having the triple effects of stopping bleeding, promoting blood circulation and enriching blood.

Panax notoginsenosides, named as total arasaponin, notoginsenoside N-FE, notoginsenoside FE, and total arasaponin, are effective medicinal components extracted from Panax notoginseng according to extraction and separation techniques, and comprise more than 20 saponin active substances, 17 trace elements, proteins, abundant vitamins, polysaccharides, etc.

The panax notoginseng saponins are obtained by a macroporous resin method from a panax notoginseng cut, the content of the obtained panax notoginseng saponins accounts for 9.75-14.90 wt% of the total amount of the panax notoginseng cut, and the panax notoginseng saponins mainly comprise ginsenoside Rb1, Rd, Re, Rg1, Rg2 and Rh 1; notoginsenoside R1, R2, R3, R4, R6, R7 and 77 volatile oils; 17 amino acids, notoginseng polysaccharide, notoginseng flavone and other physiologically active matters, wherein 4 kinds of monomer saponin including ginsenoside Rg1 (3-4 wt% in the cut of notoginseng), Rb1 (2-3 wt% in the cut of notoginseng), Rd (about 0.5 wt% in the cut of notoginseng) and notoginsenoside R1 (about 0.5 wt% in the cut of notoginseng) account for about 80% of the total arasaponin. The panax notoginseng saponins have the functions of promoting blood circulation, removing blood stasis, dredging collaterals, activating collaterals and inhibiting platelet aggregation.

Dencichine, also known as pseudo-heptanine, is chemically named as beta-oxalyl-L-alpha, beta-diaminopropionic acid. Is a non-protein amino acid extracted from leguminous or araliaceae plants. The dencichine is extracted from dry roots or cut mouths of panax notoginseng of Araliaceae, has obvious hemostatic effect and accounts for about 0.90 wt% of the total amount of panax notoginseng, is an extract prepared by crude extraction of cut mouths of panax notoginseng, and has the relative density of not less than 1.35g/cm when the temperature is 50 DEG C³. Pharmacological experiments show that the dencichine has obvious preventive and therapeutic hemostasis effects in various bleeding models, and shows good hemostasis effect at low dosage.

Flavors are the most expensive component of a toothpaste, and the style of toothpaste depends essentially on the flavor used. The toothpaste essence is an important factor for distinguishing toothpaste products according to actual use feelings of consumers. The essence for toothpaste is prepared by blending natural perfume and synthetic perfume according to the fragrance of natural plants, and has raw material components with natural flavor and various fragrance types. When the toothpaste essence is selected, the principle that the toothpaste has good compatibility with other components and the paste does not change color or taste when in use is required to be followed.

Compared with the prior art, the invention has the following beneficial effects:

the toothpaste provided by the invention mainly comprises panax notoginseng saponins, panax notoginseng saponins extract, an abrasive, a wetting agent, a foaming agent, an adhesive and a stabilizing agent, wherein the panax notoginseng saponins and the panax notoginseng saponins extract are simultaneously added, the panax notoginseng saponins can inhibit gingival inflammation, the panax notoginseng saponins can inhibit gingival bleeding, and the panax notoginseng saponins are proportioned according to the mass percentage, so that the panax notoginseng saponins can play a role in stopping bleeding when tissue trauma bleeding occurs in a machine body; during hemostasis, the dencichine can also permeate into focus parts to clean generated blood stasis; the panax notoginseng saponins can promote blood circulation and have obvious effects of resisting blood coagulation and inhibiting platelet aggregation. Therefore, the toothpaste of the present application has the effect of inhibiting gingival inflammation and gingival bleeding.

The preparation method provided by the invention mainly comprises the steps of preparing the components into a water phase, an oil phase and powder according to the characteristics of the components, then mixing and stirring the oil phase and the water phase uniformly under a negative pressure state in sequence, and finally adding the powder under a specified negative pressure and rotating speed.

Detailed Description

The technical solutions of the present invention will be described clearly and completely below, and it should be apparent that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Example 1

The invention provides toothpaste, which comprises the following components in parts by weight:

the embodiment also provides a preparation method of the toothpaste, which comprises the following steps:

A. preparing materials according to the component proportion, putting the panax notoginseng saponins, the dencichine, the saccharin sodium, the tetrasodium pyrophosphate, the sodium dihydrogen phosphate and the deionized water in the prepared materials into a water phase device, and fully mixing and dissolving for later use;

B. putting the glycerol and the sorbitol in the prepared materials into an oil phase device, and fully and uniformly mixing the glycerol and the sorbitol as the humectants for later use;

C. uniformly stirring calcium hydrogen phosphate dihydrate, hydrated silica, sodium lauryl sulfate, sodium benzoate, sodium carboxymethylcellulose and hydroxyethyl cellulose in a powder mixer for later use;

D. sucking the liquid material prepared in step A, B into a three-in-one paste making machine through a pipeline under negative pressure, and stirring for 2min under vacuum;

E. and D, absorbing the uniformly mixed powder in the step C into a three-in-one paste making pot when the vacuum degree is-0.05 MPa, continuously stirring for 28min under the condition that the stirring speed of a high-speed stirrer is 1000r/min and the vacuum degree is-0.095 MPa, finally adding the mint essence, stirring for 23min again, stirring at high speed until the mixture is fully mixed, grinding, degassing to prepare paste, and finally filling and packaging.

Example 2

A. preparing materials according to the component proportion, putting the panax notoginseng saponins, the dencichine, the saccharin sodium, the trisodium phosphate and the deionized water in the prepared materials into a water phase device, and fully mixing and dissolving for later use;

B. taking glycerol with required amount as oil phase for later use;

C. uniformly stirring hydrated silica, sodium lauryl sulfate, sodium benzoate, sodium carboxymethylcellulose and xanthan gum in a powder mixer for later use;

D. sucking the liquid material prepared in step A, B into a three-in-one paste making machine through a pipeline under negative pressure, and stirring for 1min under vacuum;

E. and D, absorbing the uniformly mixed powder in the step C into a three-in-one paste making pot when the vacuum degree is-0.04 MPa, continuously stirring for 25min under the condition that the stirring speed of a high-speed stirrer is 950r/min and the vacuum degree is-0.094 MPa, finally adding the spearmint essence, stirring for 20min again, stirring at high speed until the mixture is fully mixed, grinding, degassing to prepare paste, and finally filling and packaging.

Example 3

A. preparing materials according to the component proportion, putting the panax notoginseng saponins, the dencichine, the saccharin sodium, the tetrasodium pyrophosphate and the deionized water in the prepared materials into a water phase device, and fully mixing and dissolving for later use;

B. taking sorbitol with required amount as an oil phase for later use;

C. uniformly stirring calcium hydrogen phosphate dihydrate, sodium lauryl sulfate, sodium benzoate and sodium carboxymethylcellulose in the prepared materials in a powder mixer for later use;

D. sucking the liquid material prepared in step A, B into a three-in-one paste making machine through a pipeline under negative pressure, and stirring for 3min under vacuum;

E. and D, absorbing the uniformly mixed powder in the step C into a three-in-one paste making pot when the vacuum degree is-0.06 MPa, continuously stirring for 30min under the condition that the stirring speed of a high-speed stirrer is 1050r/min and the vacuum degree is-0.097 MPa, finally adding the tea refreshing essence, stirring for 25min again, stirring at high speed until the mixture is fully mixed, grinding, degassing to prepare paste, and finally filling and packaging.

The experimental effect is verified:

the hemostatic effect of the toothpaste provided by the invention is verified by taking the sanchinin extract adopted by the application as a research object:

1. experimental materials:

1. animals: male ICR mice, weighing 18-22g, were provided by Beijing Huafukang Biotechnology GmbH (Certification: SCXK (Jing) 2019-.

2. Drugs and reagents:

preserving the sanchinin extract at normal temperature; tranexamic acid samples, manufactured by Changzhou Yin Sheng pharmaceutical Co., Ltd, with a batch number of 20191221, had a validity period of 3 years and were stored at normal temperature. The 2 products are all provided by Yunnan Note gold ginseng oral care products, Inc.

3. The experimental method comprises the following steps:

effect on clotting time in mice (slide method)

60 ICR mice were randomly divided into 6 groups of 10 mice each, namely, a saline physiological group, an intraperitoneal (ip) injection (ip) group of dencichine extract (12.5, 25, 50mg/kg), an oral administration (ig) group of dencichine extract (50mg/kg) and a tranexamic acid positive group (50 mg/kg). Performing intraperitoneal injection on the sanchinin extract (12.5, 25 and 50mg/kg) groups at a dose of 20mL/kg, performing intraperitoneal injection for 1 time/day, performing intragastric gavage on the other groups of animals at a dose of 20mL/kg for 1 time/day, continuously administering for 6 days, 30min after the last administration, rapidly removing one side eyeball by using bent forceps, dropping one drop of blood at each side of a glass slide, wherein the diameter of the blood drop is about 5mm, and immediately timing. And slightly raising the blood drop edge inwards once every 30 seconds by using a cleaning pin, and observing whether blood filaments are raised. The required time from the beginning of blood collection to the time of picking up the blood filaments is the blood coagulation time. Another drop of blood was given for final review and the results are shown in table 1:

TABLE 1 Effect of sanchinin extract on clotting time (x + -s) in mice

Note:^#P<0.05，^##P<0.01, compared to the saline group (t-test).

As can be seen from Table 1, the blood coagulation time can be shortened by the dencichine extract (50mg/kg) oral administration group (ig), the dencichine extract (25 mg/kg), the intraperitoneal injection group (ip) and the positive drug, and the difference is statistically significant (P is less than 0.05) compared with the normal saline, wherein the blood coagulation time of the dencichine extract (50mg/kg) oral administration group (ig), the dencichine extract (50mg/kg), the intraperitoneal injection group (ip) and the tranexamic acid group is respectively shortened by 79.6%, 64.4% and 66.9%, which indicates that the oral administration and the intraperitoneal injection of the dencichine extract have certain procoagulant effects.

Influence on bleeding time of mouse tail tip

60 ICR mice were randomly divided into 6 groups of 10 mice each, namely, a physiological saline group, a dencichine extract (12.5, 25, 50mg/kg) intraperitoneal injection group, a dencichine extract (50mg/kg) oral administration group (ig) and a positive drug tranexamic acid group (50 mg/kg). The preparation method comprises the steps of carrying out intraperitoneal injection on sanchinin extract (12.5, 25 and 50mg/kg) groups in an intraperitoneal injection (ip) mode at 20mL/kg for 1 time/day, carrying out intragastric gavage on the other groups of animals at 20mL/kg for 1 time/day, continuously administering for 5 days, transecting the tail tip at a position 0.5cm away from the tail tip 30min after the last administration, slightly wiping the tail tip with filter paper every 30s, and setting the bleeding time of the tail tip from the transection of the tail tip to the condition that no blood stain is found in the filter paper.

TABLE 2 Effect of sanchinin extract on the hemostatic time of mice (+ -s).

Note:^#P<0.05，^##P<0.01, compared to the saline group (t-test).

Test results show that the bleeding time of mouse tail tips in the positive drug tranexamic acid group is obviously shortened, and compared with a normal saline group, the difference has statistical significance (P <0.05) (see table 2). The bleeding time of the tail tip of the mouse in the (ip) intraperitoneal injection (ip) group of the dencichine extract (50mg/kg) is shortened by 65.1 percent compared with that in the normal saline group, and the difference has statistical significance (P is less than 0.01).

Clinical trial verification

The toothpaste prepared in example 1 of the present application was used as a test group, and a commercially available toothpaste containing no dencichine and total notoginsenoside was used as a control group, and this clinical test was conducted in an oral hospital affiliated to Nanchang university, and the test completed 62 samples, 30 samples, and 32 samples of the control group. The conclusion of the experiment is that: the toothpaste of the test group is superior to the control group in terms of gingival inflammation control over time; adverse reactions do not occur in the two groups in the clinical test process, and the application is safe.

The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.

Claims

1. The toothpaste is characterized by comprising the following raw materials in percentage by weight:

2. The toothpaste according to claim 1, wherein the panax notoginseng saponins are prepared by a macroporous resin method.

3. The toothpaste according to claim 1, wherein the preparation method of the dencichine extract comprises the following steps:

4. The toothpaste according to any one of claims 1 to 3, wherein the dencichine extract has a relative density of not less than 1.35g/cm at 50 ℃³。

5. The toothpaste of claim 1, wherein the abrasive is in dibasic calcium phosphate dihydrate and/or hydrated silica; the humectant is glycerin and/or sorbitol.

6. The toothpaste according to claim 1, wherein the binder is one or more of sodium carboxymethylcellulose, hydroxyethylcellulose, xanthan gum, guar gum, and carrageenan.

7. The toothpaste according to claim 1, wherein the stabilizer is one or more of tetrasodium pyrophosphate, sodium dihydrogen phosphate, trisodium phosphate.

8. The toothpaste of claim 1, wherein the foaming agent is sodium lauryl sulfate; the preservative is sodium benzoate; the sweetener is saccharin sodium.

9. A method of preparing a toothpaste as claimed in any one of claims 1 to 8 comprising the steps of:

10. The method according to claim 9, wherein the powder in step (4) is added in a manner of: adding the mixture when the pressure of the paste making machine is adjusted to-0.04 MPa to-0.06 MPa, and continuously stirring for 25-30min under the vacuum degree of-0.094 to-0.097 MPa of the paste making machine, wherein the stirring speed is 950-1050 r/min; preferably, after the essence is added in the step (4), stirring is carried out for 20-25min at the rotation speed of 950-1050 r/min.