CN111904903B

CN111904903B - Oral cavity gargle and preparation method thereof

Info

Publication number: CN111904903B
Application number: CN202010669283.4A
Authority: CN
Inventors: 鲁可
Original assignee: Individual
Current assignee: Individual
Priority date: 2020-07-13
Filing date: 2020-07-13
Publication date: 2022-09-20
Anticipated expiration: 2040-07-13
Also published as: CN111904903A

Abstract

The invention discloses an oral collutory, which is prepared from three raw materials of blumea balsamifera, scutellaria baicalensis leaves and camptotheca acuminate leaves, wherein the weight ratio of the blumea balsamifera, the scutellaria baicalensis leaves and the camptotheca acuminate leaves is (4-12): 6-15: 2-8, the invention also discloses a preparation method of the oral collutory. The mouthwash provided by the invention has a good inhibition effect on common oral pathogenic bacteria such as streptococcus mutans, staphylococcus and candida albicans, can be used for preventing and treating diseases such as oral ulcer, stomatitis, caries and oral lichen, and has the effects of cleaning oral cavity, inhibiting bacteria, deodorizing, refreshing breath and the like.

Description

Oral cavity gargle and preparation method thereof

Technical Field

The invention relates to an oral collutory and a preparation method thereof.

Background

The consumption of tobacco, wine and spicy food is higher and higher, and the self-immunity is reduced due to fatigue, irregular life and high pressure, so that the incidence of oral diseases such as oral ulcer, stomatitis, caries, oral lichen, halitosis and the like is higher and higher, and the consumption of oral care products and medicines is also increased year by year. Research shows that the oral diseases are closely related to the dysregulation of microbial flora in the oral cavity, and most of the existing medicines play a role in treatment and health care by clearing away heat and toxic materials, resisting bacteria and diminishing inflammation.

Blumea balsamifera is perennial herb or subshrubular plant of blumea of Compositae, is used as a medicine by whole herbs, has various pharmacological effects of sweating, eliminating phlegm, dispelling wind, eliminating dampness, warming middle energizer, relieving diarrhea, promoting blood circulation, removing toxicity and the like, can be used for treating wind-cold type cold, headache due to wind-cold type, rheumatic arthralgia, cold-dampness diarrhea, dysentery, mosquito bites, trauma, tinea sore and the like, has a long medicine history in China, and is also one of raw materials for extracting borneol and preparing borneol. At present, blumea balsamifera has been reported to treat oral diseases, but has the defects of uncertain curative effect, low use compliance and the like.

Disclosure of Invention

The invention aims to solve the defects and provides the oral collutory which is definite in curative effect, high in active ingredient content and few in impurities and takes blumea balsamifera as a main component and the preparation method thereof.

The above purpose is realized by the following technical scheme:

an oral collutory is prepared from three raw materials of blumea balsamifera, scutellaria baicalensis leaves and camptotheca acuminate leaves, wherein the weight ratio of the blumea balsamifera, the scutellaria baicalensis leaves and the camptotheca acuminate leaves is 4-12: 6-15: 2-8.

Preferably, the weight ratio of the blumea balsamifera, the scutellaria baicalensis leaves and the camptotheca acuminate leaves is 7: 11: 5.

a method of preparing the oral rinse comprising the steps of:

1) distilling herba Blumeae Balsamiferae with water to obtain essential oil, and storing in another container;

2) adding Scutellariae radix leaf and folium Camptothecae Acuminatae into the residue obtained in step 1), extracting with water for 1-3 times, collecting extractive solution, and concentrating to obtain fluid extract;

3) adding an organic solvent into the clear paste obtained in the step 2) for extraction, separating the organic phase and concentrating into clear paste;

4) adding distilled water into the clear paste obtained in the step 3), adding the standby essential oil, a proper amount of Tween 80, glycerol and a preservative, stirring for dissolving, standing for 24 hours, filtering, and subpackaging the filtrate to obtain the traditional Chinese medicine.

The organic solvent includes, but is not limited to, methanol, ethanol, propylene glycol, n-butanol, ethyl acetate, tetrahydrofuran, diethyl ether, etc., preferably tetrahydrofuran.

Preferably, the extraction in step 2) is warm-infusion extraction, the extraction temperature being 80-95 ℃, most preferably 85 ℃. Compared with the conventional decoction extraction, the warm-soaking extraction is more favorable for improving the content of active ingredients such as total flavone, baicalin, camptothecin and the like and the antibacterial activity of the medicine.

Preferably, the number of times of warm-soaking extraction with water is 2, and the time of each extraction is 1.5 hours, under the condition that the content of the extracted active ingredients is the highest.

Preferably, the Tween 80 accounts for 0.01-0.1%, preferably 0.05%, of the volume of the collutory, and has solubilization effect in the collutory, so as to improve the stability of the collutory and prevent the generation of precipitate.

Preferably, the glycerin accounts for 0.5-2%, optimally 1% of the volume of the gargle, and mainly plays roles of promoting seepage and thickening.

The invention has the beneficial effects that:

the mouthwash provided by the invention has a good inhibition effect on common oral pathogenic bacteria such as streptococcus mutans, staphylococcus and candida albicans, can be used for preventing and treating diseases such as oral ulcer, stomatitis, caries and oral lichen, and has the effects of cleaning oral cavity, inhibiting bacteria, deodorizing, refreshing breath and the like.

The invention has the advantages of high active ingredient content and less impurities, can improve the curative effect, has better taste, can improve the compliance of use, reduce the precipitation and improve the validity period of storage, thereby having good market prospect.

Detailed Description

The present invention will be described in detail below with reference to specific examples.

Example 1 influence of bulk drug formulation on bacteriostatic effect

The raw material ratios of the samples are shown in the following table:

TABLE 1 raw material formulation for each sample

Weighing the above materials, soaking in 10 times of water for 3 hr, filtering, rotary steaming the filtrate to dryness, dissolving with glycerol, and diluting to obtain medicinal liquid with concentration of 25, 12.5, 6.25, 3.125, and 1.5625mg/ml by multiple dilution method.

Dissolving Streptococcus mutans, Staphylococcus aureus, and Candida albicans with broth culture solution respectively to obtain 10% solution ⁸ cfu/ml bacterial suspension.

Respectively sucking 0.5ml of liquid medicine with different concentrations under each sample number into a 96-hole microporous plate, adding 0.1ml of bacterial suspension into each hole correspondingly, uniformly blowing and mixing by using a liquid transfer gun, then putting into a constant-temperature incubator at 37 ℃, culturing for 24 hours, and observing the minimum medicine concentration without bacterial growth by naked eyes to obtain the MIC value of the sample number.

TABLE 2 inhibitory Effect of each sample on Streptococcus mutans

It can be seen that samples 1-9 all have a certain inhibitory effect on Streptococcus mutans, wherein the inhibitory rate of the composition formula on Streptococcus mutans is obviously better than that of the single sample, especially the inhibitory rate of sample 3 is the lowest, and the MIC value on Streptococcus mutans is lower than 1.5625 mg/ml.

TABLE 3 inhibitory Effect of each sample on Staphylococcus

It can be seen that samples 1-9 all have a certain inhibitory effect on staphylococcus, the inhibitory rate of the composition formula on staphylococcus is obviously superior to that of single samples, wherein the inhibitory rates of samples 2, 3 and 4 are the lowest, and the MIC value of the composition formula on Streptococcus mutans reaches 3.125 mg/ml.

TABLE 4 inhibitory Effect of each sample on Candida albicans

It can be seen that samples 1-7 all have a certain inhibitory effect on candida albicans, while samples 8 and 9 have a poor inhibitory effect, samples 3 and 5 have the lowest inhibitory rate, and the MIC value on candida albicans reaches 6.25 mg/ml.

After comprehensive comparison, the weight ratio of blumea balsamifera, scutellaria baicalensis leaves and camptotheca acuminate leaves is 7: 11: sample 3 of 5 has better inhibitory effect on streptococcus mutans, staphylococcus and candida albicans simultaneously, so that the oral cavity disease inhibitor can be widely applied to oral cavity diseases, and finally sample 3 is selected for subsequent tests.

Example 2 extraction solvent screening test

700g of blumea balsamifera, 1100g of scutellaria baicalensis leaves and 500g of camptotheca acuminata leaves

1) Taking blumea balsamifera, scutellaria baicalensis leaves and camptotheca acuminata leaves, adding 15Kg of water, heating to 85 ℃, soaking for 1.5 hours, filtering, collecting the extracting solution, adding 10Kg of water again into the dregs of a decoction, heating to 85 ℃, soaking for 1.5 hours, filtering, collecting the extracting solution, combining the two extracting solutions, and concentrating into clear paste with the relative density of 1.25;

2) dividing the fluid extract into 9 parts by weight, wherein one part is not treated as blank control, and the remaining 8 parts are respectively added with methanol, propylene glycol, n-butanol, ethyl acetate, tetrahydrofuran, diethyl ether, chloroform and petroleum ether for extraction, separating organic phase and concentrating into fluid extract with relative density of 1.35;

3) and (3) pressurizing and drying the clear paste to constant weight, and respectively detecting the contents of total flavone, baicalin and camptothecin in the dry paste, wherein the results are shown in the following table.

TABLE 5 Effect of extraction solvent on active ingredient content

	Total Flavonoids (%)	Baicalin content (%)	Camptothecin content (%)
				Methanol	9.17	1.54	0.33
Propylene glycol	10.03	1.65	0.37
				N-butanol	11.29	1.88	0.40
Ethyl acetate	13.40	1.72	0.41
				Tetrahydro-alkanesFuran compounds	12.56	1.78	0.46
Ether (A)	10.14	1.27	0.27
				Chloroform	7.23	1.21	0.22
Petroleum ether	6.17	0.89	0.18
				Blank control	5.53	1.14	0.25

From the above results, it can be seen that the contents of total flavonoids, baicalin and camptothecin can be increased to a different degree by selecting methanol, propylene glycol, n-butanol, ethyl acetate, tetrahydrofuran and diethyl ether as the extraction solvent, while the contents of individual components can be decreased by using chloroform and petroleum ether as the extraction solvent, compared with the sample without extraction. Wherein, when tetrahydrofuran is used as an extraction solvent, the content of each component is in a higher level, and the comprehensive extraction effect is best.

Through extraction, the content of functional components in the oral collutory is increased, the antibacterial activity is further improved, and meanwhile, due to the reduction of impurities, the mouth feel of the collutory is improved, the use compliance is improved, in addition, the precipitation can be reduced, and the storage period is prolonged.

Example 3

1) Adding 5Kg of water into blumea balsamifera, distilling for 8h, collecting essential oil, and storing in another container for later use;

2) adding the scutellaria baicalensis leaves and the camptotheca acuminata leaves into the distilled medicine residues obtained in the step 1), adding water, heating to 80 ℃, extracting for 3 times, wherein the water addition amount is 8Kg each time, the extraction time is 0.5 hour, filtering, combining the three extracting solutions, and concentrating into clear paste with the relative density of 1.25;

3) adding tetrahydrofuran into the clear paste in the step 2) for extraction, separating an organic phase and concentrating into clear paste with the relative density of 1.35;

4) adding distilled water into the clear paste obtained in the step 3), adding the standby volatile oil, 0.05 percent (volume) of Tween 80, 1 percent (volume) of glycerol and 0.1 percent (weight) of sodium benzoate, stirring for dissolving, standing for 24 hours, filtering, and subpackaging the filtrate to obtain the traditional Chinese medicine.

Example 4

1) Distilling herba Blumeae Balsamiferae with 6Kg of water for 6 hr, collecting essential oil, and storing in another container;

2) adding Scutellariae radix leaf and folium Camptothecae Acuminatae into the residue obtained in step 1), adding water, heating to 92 deg.C, extracting for 1 time with water amount of 20Kg for 3 hr, filtering, and concentrating the extractive solution to obtain fluid extract with relative density of 1.25;

3) adding tetrahydrofuran into the clear paste in the step 2) for extraction, separating an organic phase and concentrating into clear paste with the relative density of 1.30;

4) adding distilled water into the clear paste obtained in the step 3), adding the standby volatile oil, 0.05% (volume) of Tween 80, 1% (volume) of glycerol and 0.1% (weight) of sodium benzoate, stirring to dissolve, standing for 24 hours, filtering, and subpackaging the filtrate to obtain the traditional Chinese medicine composition.

Claims

1. A preparation method of the oral collutory is characterized by comprising the following steps:

3) adding tetrahydrofuran into the clear paste in the step 2) for extraction, separating an organic phase and concentrating into clear paste;

4) adding distilled water into the fluid extract of step 3), adding the essential oil and appropriate amount of Tween 80, glycerol and antiseptic, stirring for dissolving, standing for 24 hr, filtering, packaging the filtrate,

the weight ratio of the blumea balsamifera, the scutellaria baicalensis leaves and the camptotheca acuminate leaves is 7: 11: 5,

the oral collutory contains total flavone, baicalin and camptothecin, and has inhibitory effect on Streptococcus mutans, Staphylococcus aureus and Candida albicans.

2. A process for the preparation of an oral rinse as claimed in claim 1 wherein: the extraction in the step 2) is warm leaching extraction, and the extraction temperature is 85 ℃.

3. A process for the preparation of an oral rinse as claimed in claim 2 wherein: the number of times of warm-soaking extraction with water is 2, and the extraction time of each time is 1.5 hours.

4. A process for the preparation of an oral rinse as claimed in claim 1 wherein: the Tween 80 accounts for 0.01-0.1% of the volume of the gargle.

5. A process for the preparation of an oral rinse as claimed in claim 1 wherein: the glycerin accounts for 0.5-2% of the volume of the gargle.