CN110731935A

CN110731935A - toothpaste for diminishing inflammation and relieving pain

Info

Publication number: CN110731935A
Application number: CN201911285697.0A
Authority: CN
Inventors: 赵志峰; 何强; 何宗昊; 邬昊曦; 靳岳
Original assignee: Haoye Zanthoxylum Industry Research Institute Hanyuan County
Current assignee: Haoye Zanthoxylum Industry Research Institute Hanyuan County
Priority date: 2019-12-13
Filing date: 2019-12-13
Publication date: 2020-01-31

Abstract

The invention discloses anti-inflammatory analgesic toothpaste and a preparation method thereof, wherein the toothpaste comprises 3-9 parts of anti-inflammatory analgesic active ingredients, 17-55 parts of an abrasive, 3-9 parts of a foaming agent, 12-36 parts of a wetting agent and a proper amount of water, and the raw materials of the anti-inflammatory analgesic mainly comprise a pepper extract and a pepper leaf extract.

Description

toothpaste for diminishing inflammation and relieving pain

Technical Field

The invention relates to the field of daily necessities, in particular to a preparation method of anti-inflammation and analgesic toothpaste and anti-inflammation and analgesic toothpaste prepared by the method.

Background

Gingivitis, which is the most common disease in humans, is the disease, and according to incomplete survey statistics, people in China with gingivitis account for over 80% of the total population, while young and adult people more commonly have mild gingivitis, which may become severe and may develop into periodontal disease if not discovered early.

Gingivitis is caused by the lack of attention to oral hygiene, long-term irritation of teeth due to soft tartar and hard tartar formed by food residue, bacteria and the like around the teeth, incorrect tooth brushing habits, vitamin deficiency and the like. The periodontal health rate of people in the age range of 35-44 years in China is 14.5%, the cities are higher than the countryside, the women are higher than the men, and the western regions are the highest; the detection rate of gingival bleeding is 77.3%, the number of teeth with gingival bleeding is 8.77 for all people, women are higher than men, no difference exists between city and countryside, and the highest is in the middle area; the detection rate of periodontal pockets is 40.9%, the city is lower than that in rural areas, the male is higher than that in female, and the middle area is highest; the detection rate of the attachment loss equal to or more than 4 mm is 38.9%, the number of males is higher than that of females, there is no difference between cities and countries, and the highest rate is in the eastern region.

From the perspective of traditional Chinese medicine, gingivitis belongs to the category of gingival bleeding and fever with swollen head in the traditional Chinese medicine, more than yangming meridian excess heat is related, foot yangming stomach meridian circulates to the side of nose and enters upper teeth, and hand yangming large intestine upper item passes through cheek and enters lower teeth. Gingivitis is caused by heat accumulation in the spleen and stomach or inflammation of the stomach with excess fire circulating through yangming channels and collaterals on gums, so that the gums are swollen and painful, the channel heat is not dissipated, the channels are burned, and the channels are damaged, so that the gums are easy to bleed. In order to avoid inflammation of the gingival tissue, care of the oral cavity is of particular importance.

The oral care products are indispensable cleaning and health care products in daily life of people, and products are various in types, comprise toothpaste, chewing gum, mouthwash, tooth powder, oral spray and the like, and are mainly used for keeping the oral cavity and the teeth clean, promoting breath freshening, nursing the gums, maintaining good microenvironment of the oral cavity and the like.

In recent years, due to changes of living habits and consumption concepts of people, more requirements are put forward on the toothpaste, various toothpastes with health care functions emerge in the market, particularly, the Chinese herbal medicine toothpaste has huge market share, has the health care functions of inhibiting harmful bacteria in the oral cavity, refreshing breath, protecting teeth, preventing and treating oral diseases and the like, and at present, the toothpaste containing Chinese herbal medicines is adopted for preventing and treating gingivitis, is widely accepted by , and has the characteristics of safety, simplicity in operation, convenience in carrying and the like.

In recent years, natural medicines, particularly traditional Chinese medicines in China, are applied to oral care products as active ingredients to solve related oral problems and become hot spots in the market and pursuits of consumers, analgesic oral care products are sold in the market and are mainly realized by western medicine ingredients or single traditional Chinese medicines, or new traditional Chinese medicine toothpaste with analgesic and anti-inflammatory effects is simply developed, and substantial problems to be solved are not proposed.

Chinese patent CN103417402B discloses azulene bactericidal toothpaste, which consists of azulene, aluminum hydroxide, lauroampho PG-acetate sodium phosphate, guar gum, sorbitol and water, the azulene bactericidal toothpaste has the advantages of abundant foam, strong bactericidal power, comprehensive oral care and oral and tooth health protection, and is bactericidal toothpastes meeting the requirements of modern people.Chinese patent application 201510711524.6 discloses chitin tooth-protecting toothpaste, which mainly consists of chitin, sorbitol sugar solution, silicon dioxide, sodium dodecyl sulfate, sodium carboxymethylcellulose, deionized water, saccharin sodium, menthol, clove and nipagin fat, and the prepared chitin tooth-protecting toothpaste has the functions of cleaning oral cavity, preventing and treating oral ulcer, gingival swelling and pain, bleeding and the like besides the function of common toothpaste, wherein the chitin molecule contains-OH and NH²⁺The polar group can effectively inhibit the propagation of harmful bacteria in the oral cavity, proliferate beneficial bacteria, improve the environment in the oral cavity, and the unique nutrient factors and functional factors of the chitin have strong biocompatibility and film forming capability, so as to effectively protect gum and tooth surface from erosion and comprehensively protect the oral cavity.

The zanthoxylum is a rutaceae plant, is pungent in taste and strong in fragrance, is of unique edible spices in China, is about 250 varieties in the whole world, is distributed in tropical and subtropical regions of Asia, America, Africa and oceanic continents, is about 45 varieties and 13 varieties in China, and the main varieties are zanthoxylum and zanthoxylum seeds commonly called green zanthoxylum, zanthoxylum piperitum, zanthoxylum simulans and the likeZanthoxylum bungeanum is mainly concentrated in the producing area. The main cultivated species include zanthoxylum bungeanum, zanthoxylum micranthum, bean pepper, zanthoxylum bungeanum, capsicum annuum, white pepper, etc. The Ministry of health in 2002 confirms that the pepper is a medicinal and edible raw material, and the current planting area exceeds 12 kilohm²The annual production of pricklyash peel is about 12 million tons, and the output value is 15 hundred million yuan.

Zanthoxylum bungeanum refers to the pericarp of Zanthoxylum bungeanum. The chemical components of the pepper mainly comprise volatile oil, alkaloid, amide, coumarin, flavone and the like, and other components comprise three-shielding, remained alcohol, hydrocarbons, lignans, fatty acid and the like. However, if the zanthoxylum bungeanum maxim extract is directly applied to the production of toothpaste, bad experience feeling is necessarily brought by the numb substances in the zanthoxylum bungeanum maxim during the use process, and meanwhile, the toothpaste added with the zanthoxylum bungeanum maxim extract can be separated out during the long-time storage process, and although the homogenization treatment is repeatedly carried out in the experimental process, the 6-month observation shows that the separated out substances still exist in the toothpaste, so that the use of a user is influenced.

In view of the defects, has stable texture, the pepper extract can not be separated out after long-term storage, the toothpaste has no numb taste, and the traditional Chinese medicine toothpaste with the functions of easing pain and assisting inflammation is urgently needed by the industry, and has important significance for relieving uncomfortable symptoms of human oral cavity, keeping good micro-ecology of the oral cavity, relieving interpersonal interaction pressure and the like.

Disclosure of Invention

Based on the analysis, the invention provides toothpaste which has stable texture, no precipitation of the pepper extract after long-term storage, no numb taste of the toothpaste and analgesic and anti-inflammatory functions, and the toothpaste is realized by the following means:

kinds of anti-inflammatory and analgesic toothpaste is prepared from the following raw materials in parts by weight:

3-9 parts of an anti-inflammatory analgesic active ingredient, 17-55 parts of an abrasive, 3-9 parts of a foaming agent, 12-36 parts of a wetting agent and a proper amount of water.

, the toothpaste is prepared from the following raw materials in parts by weight:

6 parts of anti-inflammatory analgesic active ingredients, 36 parts of an abrasive, 6 parts of a foaming agent, 24 parts of a wetting agent and a proper amount of water.

A method for preparing anti-inflammatory analgesic toothpaste, comprising the following steps:

(1) preparing a liquid phase: putting a wetting agent into a stirring pot, wetting and stirring, adding a foaming agent and water, continuously stirring, and fully swelling to prepare a uniform semitransparent liquid phase for later use;

(2) and (2) preparing the paste, namely putting the abrasive and the anti-inflammatory analgesic active ingredients into a paste making machine, stirring uniformly, pumping the vacuum degree to-0.05 MPa, simultaneously starting a low-speed stirrer for stirring, adding the semitransparent liquid phase prepared in the step (1), keeping the vacuum degree at-0.06 to-0.085 MPa until the liquid phase is completely fed, homogenizing for 40-60min, degassing, opening a normal pressure valve after the degassing is finished, and degassing to obtain the anti-inflammatory analgesic toothpaste.

, degassing in the step (2) to-0.092-0.098 MPa, and maintaining for 15 min.

, mixing the anti-inflammatory and analgesic active ingredients in the step (2) with the pepper extract and the pepper tender leaf extract according to a ratio of 4:7 (m/v).

, the pricklyash peel extract is prepared by the following method:

(1) grinding fresh pepper by using liquid nitrogen, and freezing and storing for later use to obtain pepper sample tissue powder;

(2) adding analytically pure methanol into the tissue powder of the pepper sample, carrying out ultrasonic extraction treatment, centrifuging at low temperature, collecting supernatant, continuously extracting residues for 3 times under the same condition, combining three extracting solutions, and re-dissolving with methanol-water solution with volume concentration of 15% (v/v) after rotary evaporation and drying;

(3) gradually extracting the re-dissolved extracting solution: firstly, extracting with analytically pure petroleum ether and the re-dissolved extracting solution according to the volume ratio of 1:1, retaining a methanol water phase, then extracting with analytically pure dichloromethane and the methanol water phase according to the volume ratio of 1:1, retaining the dichloromethane phase, evaporating an organic solvent to dryness after extraction, and then dissolving with analytically pure methanol to obtain a methanol solution-extracting solution;

(4) performing column chromatography on the methanol solution-extracting solution, passing through a C-18 column, eluting with methanol-water solution, sequentially eluting with gradient eluents with volume concentrations of 25%, 50%, 75% and 90%, collecting the eluate with volume concentration of 50% (v/v), rotary evaporating the obtained eluate, and freeze drying to obtain the fructus Zanthoxyli extract.

, ultrasonic leaching with ultrasonic leaching parameter of 240V40kHz for 20min in step (2), and centrifuging at 4-10 deg.C.

, preparing the pepper tender leaf extracting solution by the following method:

(1) adding 2 times of water into the tender leaves of the zanthoxylum bungeanum maxim, mixing, and stirring at the temperature of 35-38 ℃ and the rotating speed of 100-;

(2) transferring the mixture into a fermentation tank, sealing and fermenting at constant temperature, drying the fermented mixture for 3-6h at 43-48 ℃, then adding the dried mixture into 0.6-1kg of 35-45% ethanol aqueous solution by volume fraction, then adding 4-6g of 0.3-0.6% citric acid aqueous solution by mass fraction, stirring for 3-5h at 45-55 ℃ and the rotating speed of 200-400r/min, and sieving by a 200-mesh sieve with 100-mesh sieve to obtain times of filtrate and times of filter cakes;

(3) and (3) filtering the -time filtrate by using four layers of medical absorbent gauze to obtain a secondary filtrate, and performing reduced pressure evaporation and concentration on the secondary filtrate to obtain 1/15-1/10 of the original mass, namely obtaining the pepper tender leaf extracting solution.

, concentrating by rotary evaporation under reduced pressure in step (3) at 45-55 deg.C and 30-60r/min under absolute pressure of 0.04-0.06 MPa.

The invention also discloses anti-inflammatory analgesic toothpaste prepared by the preparation method of any .

The invention has the beneficial effects that:

1. the invention adopts the pepper extract and the pepper tender leaf extract to prepare the anti-inflammatory analgesic toothpaste together, can fully perform complexation when contacting with auxiliary materials, provides adhesiveness and film-forming property for the toothpaste, and can adhere to the oral mucosa and form a film in the using process, thereby achieving the effect of lasting bacteriostasis.

2. The anti-inflammation and analgesic toothpaste prepared by the invention can effectively reduce the pain of patients suffering from canker sore, shorten the healing time of the canker sore, has obvious protection effect on the mouth, has high stability and high safety of the effective components in the toothpaste, and is more ideal healthy toothpastes.

Detailed Description

In order to make the objects, technical solutions and advantages of the present invention more apparent, the following will describe in further detailed embodiments of the present invention, but the embodiments of the present invention are not limited thereto, and the process parameters or conditions not particularly mentioned can be performed with reference to the conventional techniques.

Example 1

toothpaste for diminishing inflammation and relieving pain

(1) Preparing a pepper extract:

① grinding fresh fructus Zanthoxyli with liquid nitrogen, and freezing for use to obtain tissue powder of fructus Zanthoxyli sample;

② adding analytically pure methanol into tissue powder of fructus Zanthoxyli sample, ultrasonic extracting at 240V and 40kHz for 20min, centrifuging at 7 deg.C, collecting supernatant, extracting residue for 3 times under the same conditions, mixing three extractive solutions, rotary steaming, drying, and re-dissolving with 15% (V/V) methanol-water solution;

③ extracting the re-dissolved extractive solution step by using analytically pure petroleum ether and the re-dissolved extractive solution at a volume ratio of 1:1, keeping a methanol water phase, extracting with analytically pure dichloromethane and the methanol water phase at a volume ratio of 1:1, keeping a dichloromethane phase, evaporating the organic solvent to dryness after extraction, and dissolving with analytically pure methanol to obtain a methanol solution-extractive solution;

④ subjecting the methanol solution-extractive solution to column chromatography, passing through C-18 column, eluting with methanol-water solution, sequentially eluting with gradient eluents with volume concentrations of 25%, 50%, 75% and 90%, collecting eluate with volume concentration of 50% (v/v), rotary evaporating the eluate, and freeze drying to obtain fructus Zanthoxyli extract.

(2) Preparing a pepper tender leaf extracting solution:

① adding 2 times of water into tender leaf of fructus Zanthoxyli, mixing, and stirring at 36 deg.C and 200r/min for 35min to obtain mixture;

② transferring the mixture into a fermentation tank, sealing and fermenting at constant temperature, drying the fermented mixture at 45 deg.C for 4.5h, adding into 0.6-1kg of 40% ethanol water solution, adding 5g of 0.45% citric acid water solution, stirring at 50 deg.C and 300r/min for 4h, and sieving with 150 mesh sieve to obtain times of filtrate and times of filter cake;

③ filtering the filtrate with four layers of medical absorbent gauze to obtain secondary filtrate, and concentrating the secondary filtrate by evaporation under reduced pressure to 1/12 of the original quality to obtain extract of tender leaves of Zanthoxylum bungeanum, wherein the concentration by evaporation under reduced pressure is rotary evaporation concentration under the conditions of absolute pressure of 0.05MPa, temperature of 50 deg.C and rotation speed of 45 r/min.

(3) Preparing a liquid phase: putting 24kg of wetting agent into a stirring pot, wetting and stirring, adding 6kg of foaming agent and a proper amount of water, continuously stirring, and fully swelling to prepare a uniform semitransparent liquid phase for later use;

(4) preparing paste, namely putting 36kg of an abrasive and 6kg of an anti-inflammatory and analgesic active ingredient (prepared by mixing a pepper extract and a pepper tender leaf extracting solution according to a ratio of 4:7 (m/v)) into a paste making machine, uniformly stirring, pumping the vacuum degree to-0.05 MPa, simultaneously starting a low-speed stirrer for stirring, adding a semitransparent liquid phase, keeping the vacuum degree at-0.07 MPa until the liquid phase is completely fed, homogenizing for 50min, degassing to-0.095 MPa, keeping for 15min, opening a normal pressure valve after the completion, and discharging gas to obtain anti-inflammatory and analgesic toothpaste.

Example 2

toothpaste for diminishing inflammation and relieving pain

(1) Preparing a pepper extract:

② adding analytically pure methanol into tissue powder of fructus Zanthoxyli sample, ultrasonic extracting at 240V40kHz for 20min, centrifuging at 4 deg.C, collecting supernatant, extracting residue for 3 times under the same conditions, mixing three extractive solutions, rotary steaming, drying, and re-dissolving with 15% (V/V) methanol-water solution;

(2) Preparing a pepper tender leaf extracting solution:

① adding 2 times of water into tender leaf of fructus Zanthoxyli, mixing, and stirring at 35 deg.C and 100r/min for 20min to obtain mixture;

② transferring the mixture into a fermentation tank, sealing and fermenting at constant temperature, drying the fermented mixture at 43 deg.C for 3h, adding into 0.6kg of 35% ethanol water solution, adding 4g of 0.3% citric acid water solution, stirring at 45 deg.C and 200r/min for 3h, and sieving with 100 mesh sieve to obtain times of filtrate and times of filter cake;

③ filtering the filtrate with four layers of medical absorbent gauze to obtain secondary filtrate, and concentrating the secondary filtrate by evaporation under reduced pressure to 1/15 of the original quality to obtain extract of tender leaves of Zanthoxylum bungeanum, wherein the concentration by evaporation under reduced pressure is rotary evaporation concentration under the conditions of absolute pressure of 0.04MPa, temperature of 45 deg.C and rotation speed of 30 r/min.

(3) Preparing a liquid phase: putting 12kg of wetting agent into a stirring pot, wetting and stirring, adding 3kg of foaming agent and a proper amount of water, continuously stirring, and fully swelling to obtain a uniform semitransparent liquid phase for later use.

(4) Preparing paste, namely putting 17kg of an abrasive and 3kg of an anti-inflammatory and analgesic active ingredient (prepared by mixing a pepper extract and a pepper tender leaf extracting solution according to a ratio of 4:7 (m/v)) into a paste making machine, uniformly stirring, pumping the vacuum degree to-0.05 MPa, simultaneously starting a low-speed stirrer for stirring, adding a semitransparent liquid phase, keeping the vacuum degree at-0.06 MPa until the liquid phase is completely fed, homogenizing for 40min, degassing to-0.092 MPa, keeping for 15min, opening a normal pressure valve after the completion, and discharging gas to obtain anti-inflammatory and analgesic toothpaste.

Example 3

toothpaste for diminishing inflammation and relieving pain

(1) Preparing a pepper extract:

② adding analytically pure methanol into tissue powder of fructus Zanthoxyli sample, ultrasonic extracting at 240V40kHz for 20min, centrifuging at 10 deg.C, collecting supernatant, extracting residue for 3 times under the same conditions, mixing three extractive solutions, rotary steaming, drying, and re-dissolving with 15% (V/V) methanol-water solution;

(2) Preparing a pepper tender leaf extracting solution:

① adding 2 times of water into tender leaf of fructus Zanthoxyli, mixing, and stirring at 38 deg.C and 300r/min for 50min to obtain mixture;

② transferring the mixture into a fermentation tank, sealing and fermenting at constant temperature, drying the fermented mixture at 48 deg.C for 6h, adding into 1kg of 45 vol% ethanol water solution, adding 6g of 0.6 wt% citric acid water solution, stirring at 55 deg.C and 400r/min for 5h, and sieving with 200 mesh sieve to obtain times of filtrate and times of filter cake;

③ filtering the filtrate with four layers of medical absorbent gauze to obtain secondary filtrate, and concentrating the secondary filtrate by evaporation under reduced pressure to 1/10 of the original quality to obtain extract of tender leaves of Zanthoxylum bungeanum, wherein the concentration by evaporation under reduced pressure is rotary evaporation concentration under the conditions of absolute pressure of 0.06MPa, temperature of 55 deg.C and rotation speed of 60 r/min.

(3) Preparing a liquid phase: putting 36kg of wetting agent into a stirring pot, wetting and stirring, adding 9kg of foaming agent and a proper amount of water, continuously stirring, and fully swelling to prepare a uniform semitransparent liquid phase for later use;

(4) the preparation method comprises the steps of putting 55kg of an abrasive and 9kg of an anti-inflammatory analgesic active ingredient (prepared by mixing a pepper extract and a pepper tender leaf extracting solution according to a ratio of 4:7 (m/v)) into an ointment making machine, stirring uniformly, pumping the vacuum degree to-0.05 MPa, starting a low-speed stirrer for stirring, adding the semitransparent liquid phase prepared in the step (1), keeping the vacuum degree at-0.085 MPa until the liquid phase is completely fed, homogenizing for 60min, degassing to 0.098MPa, keeping the vacuum degree for 15min, opening a normal pressure valve after the completion, and degassing to obtain the anti-inflammatory analgesic toothpaste.

Comparative example 1

toothpaste for diminishing inflammation and relieving pain

(the preparation process and formulation were the same as in example 1 except that the conventional method was used for the preparation of the Zanthoxylum piperitum extract)

(1) Preparing a pepper extract: pulverizing fructus Zanthoxyli, extracting with ethanol, purifying, and concentrating to obtain fructus Zanthoxyli extract;

(2) preparing a pepper tender leaf extracting solution:

Comparative example 2

toothpaste for diminishing inflammation and relieving pain

(the preparation process and the formula are the same as those of example 1, but the conventional method is adopted when preparing the extracting solution of the tender leaves of the peppers)

(1) Preparing a pepper extract:

(2) Preparing a pepper tender leaf extracting solution: adding 6 times of water into the tender leaves of the zanthoxylum bungeanum maxim, soaking for 2 hours, heating to boil, decocting for 15 minutes by mild fire, filtering an extracting solution, adding 6 times of water of the tender leaves of the zanthoxylum bungeanum maxim, repeatedly decocting and filtering for 2 times, and combining the extracting solutions to obtain a zanthoxylum bungeanum maxim plant extracting solution;

Comparative example 3

toothpaste for diminishing inflammation and relieving pain

(the preparation process and the formula are the same as those of example 1, but the conventional method is adopted when the pepper extract and the pepper tender leaf extracting solution are prepared)

Test example

Sterilization test

1. Test materials: example 1, comparative examples 1-3 were selected to prepare toothpaste as the study sample for this time.

2. The test method comprises the following steps: the bactericidal effect of the examples on E.coli, S.aureus, S.albicans, S.mutans and P.gingivalis was determined with reference to the method specified in GB15979-2002 appendix C3.

3. And (3) test results:

the test results are shown in table 1.

TABLE 1 Sterilization Rate of anti-inflammatory analgesic toothpastes prepared in example 1 and comparative examples 1 to 3

。

As can be seen from Table 1, the anti-inflammatory analgesic toothpaste provided by the invention has extremely remarkable bactericidal effects on Escherichia coli, Staphylococcus aureus, Candida albicans, Streptococcus mutans and Porphyromonas gingivalis, and is obviously superior to comparative examples 1-3.

Test example two

Clinical test of anti-inflammatory analgesic toothpaste on dental ulcer

1. Test materials: the anti-inflammatory analgesic toothpaste prepared in example 1.

2. Test subjects: 80 patients with 20-65 years old Recurrent Aphthous Ulcers (RAU) were selected and randomized into trial and control groups of 40 each.

3. Test standards: subjects were healthy adult males and females meeting inclusion and exclusion criteria.

3.1, inclusion criteria include good general health, a history of RAU disease but no systemic diseases, ability to read, understand and sign informed consent, ability to record and take part in examination at any time during the test, at least oral ulcers in the oral cavity with ulcer occurrence time less than 48h, no allergy to toothpaste and components thereof, no use of other drugs for treating oral ulcers, no use of other oral cleaning measures except for toothbrushes, such as dental floss and mouthwash, chewing gum and the like, and no simultaneous participation in other similar test studies.

3.2, exclusion criteria: severe recurrent aphthous ulcer, behcet's disease; systemic disease background such as anemia, peptic ulcer, crohn's disease, acute infectious disease, autoimmune disease, etc.; analgesic or stomatocace treating medicine is administered within 24 h; antibiotics and anti-inflammatory drugs are used within 1 month, and corticosteroids and immunosuppressants are used systemically within 3 months; smokers and drinkers in 3 months; a patient with a tumor; (ii) has a history of allergy to the oral care product or component thereof; women in gestation and lactation.

4. Evaluation indexes are as follows:

4.1, mean ulcer stage (day, D): the sum of the durations of the individual ulcers divided by the total number of ulcers for the evaluation period.

4.2, pain index (score, P): the daily pain scores during the ulceration period were recorded using a Visual Analogue Scale (VAS). VAS indicates that a 10cm straight line is used, the 0 end of the straight line indicates "no pain", and the 10cm end indicates "most severe pain". The subjects recorded on the corresponding scale of the line 1 time per day, depending on the degree of pain perception.

Grading evaluation indexes: d₁: the average ulcer period is shortened (t test, P is less than 0.05); d₀: mean ulcer phase change (t test, P > 0.05); p₁: a decrease in pain index (t-test, P < 0.05); p₀: there was no change in pain index (t-test, P > 0.05). Evaluation criteria: show effect (D)₁P₁) (ii) a Effective (D)₁P₀Or D₀P₁) (ii) a Invalidation (D)₀P₀）。

5. The test method comprises the following steps:

the pain index of a patient in a conference is recorded and sent to a 'oral ulcer record table', contact calls of subjects are recorded, sets of the anti-inflammatory and analgesic toothpaste and toothbrush prepared by the invention are respectively used by each patient in a test group, the toothpaste is smeared on an affected part 10min before three meals, the patient takes food after 5min, the patient takes the toothpaste 2 times in the morning and evening, the teeth are brushed by the toothpaste according to a habit method, the patient in a control group sends certain Chinese herbal medicine toothpaste purchased in the market for use, the using method and the frequency are the same as those of the patient in the test group, then the patient is subjected to telephone return visit every day to know the ulcer development, oral cavity examination is carried out and the 'oral ulcer record table' is recovered after the oral ulcer is healed, and the test.

6. And (3) test results:

the test results are shown in table 2.

TABLE 2 comparison of pain index and ulcer recovery time

。

The results in table 2 show that the anti-inflammatory analgesic toothpaste provided by the invention can significantly reduce the pain of patients with oral ulcer, and has significant treatment effect on oral ulcer. Meanwhile, the ulcer time of the patient suffering from oral ulcer can be shortened, and the oral ulcer can be treated remarkably.

Test example three

Stability detection of anti-inflammatory analgesic toothpaste on dental ulcer

The detection method comprises the following steps: referring to the "Disinfection Specification" 2002 edition, the toothpastes of example 1 and comparative examples 1 to 3 were tested for stability after being left at 55 ℃ for 60 days.

1. The detection indexes are as follows:

(1) and (3) appearance detection: color, smell, layering;

(2) antibacterial efficacy: and (3) detecting the bacteriostatic action on escherichia coli, staphylococcus aureus and pseudomonas aeruginosa.

2. The test results are shown in Table 3

TABLE 3 comparison of stability of anti-inflammatory and analgesic toothpastes prepared in example 1 and comparative examples 1 to 3

。

As can be seen from the results in Table 3, when accelerated stability testing is performed at 55 ℃, the bactericidal or bacteriostatic rate of the toothpaste prepared in example 1 reaches the specified standard value, and apparently due to any groups in comparative examples 1-3, it can be seen that the highly effective period of the antibacterial activity of the eye light prepared by the invention can be preserved for at least 2 years at room temperature.

The foregoing is directed to preferred embodiments of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow. However, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the protection scope of the technical solution of the present invention.

Claims

1, kinds of anti-inflammatory analgesic toothpaste, characterized by that, this toothpaste is made of raw materials of the following weight proportion:

2, kinds of anti-inflammatory analgesic toothpaste, characterized by that, this toothpaste is made of raw materials of the following weight proportion:

3, method for preparing anti-inflammatory analgesic toothpaste according to claim 1 or 2, characterized in that it comprises the following steps:

4. The method according to claim 3, wherein the degassing in step (2) is carried out to a pressure of-0.092 to 0.098MPa for 15 min.

5. The preparation method according to claim 3, wherein the anti-inflammatory and analgesic active ingredient of step (2) is prepared by mixing Zanthoxylum bungeanum extract and extractive solution of tender leaves of Zanthoxylum bungeanum at a ratio of 4:7 (m/v).

6. The preparation method according to claim 5, wherein the Zanthoxylum bungeanum extract is prepared by the following method:

7. The preparation method according to claim 6, wherein the ultrasonic leaching parameter in the step (2) is 240V40kHz ultrasonic leaching for 20 min; the low-temperature centrifugation temperature is 4-10 ℃.

8. The preparation method according to claim 5, wherein the extraction solution of the tender leaves of zanthoxylum bungeanum is prepared by the following method:

9. The method according to claim 8, wherein the concentration by reduced pressure evaporation in step (3) is rotary evaporation concentration under the conditions of 0.04-0.06MPa absolute pressure, 45-55 ℃ temperature and 30-60r/min rotation speed.

10, toothpaste for diminishing inflammation and easing pain prepared by the preparation method of any as claimed in claims 3-9.