CN116421515A - Houttuynia cordata washing product for caries prevention and bacteriostasis and production line thereof - Google Patents
Houttuynia cordata washing product for caries prevention and bacteriostasis and production line thereof Download PDFInfo
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- CN116421515A CN116421515A CN202310305414.4A CN202310305414A CN116421515A CN 116421515 A CN116421515 A CN 116421515A CN 202310305414 A CN202310305414 A CN 202310305414A CN 116421515 A CN116421515 A CN 116421515A
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- extract
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- washing
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- Medicines Containing Plant Substances (AREA)
Abstract
A herba Houttuyniae washing product for preventing dental caries and inhibiting bacteria and its production line are provided, wherein the effective components of the washing product are herba Houttuyniae extract or its derivatives, and green tea related extract, and the herba Houttuyniae extract or its derivatives with good water solubility and poor water solubility are respectively defined. The production line is connected with each other through the connecting pipeline, and a complete production system is formed by arranging different containers, electromagnetic valves, water pumps and the like on the connecting pipeline, so that not only is the feeding of the washing product and the control of each reaction process realized, but also the occupied area is less, the space utilization is facilitated, the automation degree of the production of the washing product is improved, and the washing product can be further used for producing other products such as dentifrice, tooth gel, oral cavity spray and the like. The invention not only can obviously inhibit the main pathogenic bacteria of caries-streptococcus mutans, but also has good biocompatibility and production benefit, and is helpful for solving the urgent demands of oral health care and oral disease prevention on effective, safe and long-term use of oral washing products.
Description
Technical Field
The invention relates to the technical field of production equipment of oral cavity washing products, in particular to an anticarious oral cavity washing product containing houttuynia cordata extracts or derivatives thereof and an automatic production line thereof.
Background
According to the fourth national epidemiological survey data, the caries rate of adult caries in China is up to more than 80%, which is the main cause of tooth defect and pain. Streptococcus mutans is the primary pathogen responsible for caries. At present, the common method of controlling S.mutans is to control plaque by mechanical means of brushing and to clean the oral cavity using a wash product with an added antibacterial ingredient. However, brushing is difficult to penetrate deep into the crevices and under the gingival margin. The washing product can remove oral bacteria to a certain extent even though penetrating deep into the crevices and under the edge of the gum. However, most of antibacterial components in the existing washing products are substances such as alcohol, chlorohexidine, metronidazole and the like, so that white lesions of mucous membranes are easily caused after long-term use, and the problems of tartar formation, tooth surface staining, taste change and the like are caused. Therefore, it is important to find new safe and effective anticaries substances.
The houttuynia cordata can be taken as a medicinal and edible plant, and is also a Chinese medicinal material with clinical application value. The herba Houttuyniae extract contains houttuynin as main effective component, and has good antibacterial, antiviral and antiinflammatory effects. Sodium houttuyfonate and sodium new houttuyfonate are sodium bisulfite derivatives of natural houttuyfonate. Studies show that houttuynin derivatives have more stable properties and retain antibacterial effects on staphylococcus aureus, bacillus dysenteriae, candida albicans, escherichia coli and the like. Meanwhile, researches show that the houttuynia cordata extract or the derivatives thereof have positive effects on preventing and treating oral bacterial infectious diseases. Therefore, the houttuynia cordata extract or the derivative thereof is an ideal anticaries substance for the oral cavity washing products.
The water solubility of houttuynia cordata oil, houttuynin sodium, new houttuynin sodium and other houttuynia cordata extracts or derivatives thereof is poor, the application of the houttuynia cordata oil is limited to a certain extent, and how to improve the solubility of the houttuynia cordata oil is a key problem affecting the use of the houttuynia cordata oil. Chinese patent CN113143904a (an application of houttuynin analog in preparing streptococcus mutans growth and its biofilm inhibitor) discloses an application of houttuynin analog in preparing streptococcus mutans growth and biofilm inhibitor, which can inhibit streptococcus mutans growth and biofilm formation, and has potential as anticarious medicine. But this technique has the following drawbacks: (1) The dissolved mother solution is dimethyl sulfoxide which is an organic solvent, has certain toxicity and can stimulate eyes, skin and respiratory systems; (2) The technology does not design a corresponding production line, and prevents further product conversion and application.
In addition, the existing washing products are mostly in a liquid form in a mouthwash form, so that the existing washing products occupy a large volume and are inconvenient to carry; the existing production process of the mouthwash product involves more materials and production devices, and the materials and the production devices are generally distributed, occupy larger space and increase space cost; moreover, the reaction process of the existing mouthwash product in the manufacturing process is relatively complex, is not easy to control, and affects the safety and efficiency of the production of the existing mouthwash product.
In summary, there is a need to develop a production line with a relatively simple reaction process, and to prepare an oral rinse product which is convenient to carry, has no obvious irritation to oral mucosa, and has good oral antibacterial effect, so that the urgent needs of people in the aspects of oral health care and oral disease prevention for effective, safe and long-term use of the oral rinse product can be solved.
Disclosure of Invention
The invention aims to provide an anticarious antibacterial oral cavity washing product containing houttuynia cordata extract or a derivative thereof and an automatic production line thereof, so as to solve the problems in the background technology.
In order to achieve the above purpose, the invention is realized by adopting the following technical scheme:
a cordate houttuynia washing product for caries prevention and bacteriostasis, which is characterized in that the effective components of the washing product comprise an A component and a B component, wherein:
the component A is herba Houttuyniae extract or its derivative, and contains one or more of herba Houttuyniae extract, herba Houttuyniae oil, houttuynin, sodium houttuyfonate, and sodium new houttuyfonate; wherein,,
the water-poor houttuynia cordata oil, houttuynin, sodium houttuyfonate, sodium new houttuyfonate and the like are represented as a houttuynia cordata extract or a derivative thereof;
the herba Houttuyniae extract has good water solubility and is represented by b-type herba Houttuyniae extract or its derivative;
and when the component A is used for preparing the washing product, dissolving the cordate houttuynia extract or the derivative thereof in absolute ethyl alcohol, and dissolving the cordate houttuynia extract or the derivative thereof in deionized water;
the component B is green tea related extract including one or more of green tea extract, tea polyphenols and catechin;
the mass ratio of the A to the B is such that the washing product has both antibacterial effect and color and taste.
Preferably, the cordate houttuynia washing product for caries prevention and bacteria inhibition is characterized in that:
the washing product also comprises a proper amount of auxiliary materials, wherein the auxiliary materials comprise: one or more of humectants, preservatives, antioxidants, emulsifiers, thickeners, sweeteners, mucilage, fragrances, and flavoring agents.
In addition, the invention also discloses a production line of the cordate houttuynia washing product for caries prevention and bacteriostasis, which comprises the following steps:
a first container (1), a second container (2), a third container (3), a fourth container (401), a fifth container (17), a placing barrel (9), a second drying device (18) and a freezing device (19), wherein:
the placing barrel (9) and the second drying device (18) and the freezing device (19) are communicated through pipelines;
the top ends of the first container (1) and the second container (2) are connected with a first stirring barrel (101) through a bracket, and a liquid flowmeter (102) is connected to a pipeline connected with the first container (1) and the first stirring barrel (101);
the two sides of the top end of the first stirring barrel (101) are communicated with a feed pipe (12) and a hopper (13), and a feed inlet formed in the top end of the third container (3) is respectively connected with discharge ports at the bottom ends of the first container (1) and the second container (2) through a connecting pipeline (11);
the discharge port of the third container (3) is connected with the feed port at the top end of the fourth container (401) through a connecting pipeline (11);
the top ends of the fourth container (401) and the placing barrel (9) are communicated with a second liquid inlet pipe (10), and a discharge hole at the bottom end of the fourth container (401) is communicated with a feed inlet at the top end of the second stirring barrel (4) through a connecting pipe;
a first drying device (7) is arranged on one side of the second stirring barrel (4), a discharge hole at the bottom end of the first drying device (7) is connected with a fifth container (17) through a connecting pipe, a first liquid inlet pipe (8) is communicated with the top of the fifth container (17), and the discharge hole of the fifth container (17) is communicated with a dialysis bag (23) arranged in the placing barrel (9) through a connecting pipeline (11).
Preferably, the production line is characterized in that:
the production line further comprises a comminuting device (20); the refrigerating device (19) is communicated with the crushing device (20) through a pipeline.
Preferably, the production line is characterized in that:
the utility model discloses a drying device, including placing bucket (9), including a plurality of and being one row setting, the quantity of dialysis bag (23) is unanimous with placing bucket (9), and the export of one dialysis bag (23) is linked together through connecting tube (11) with the import of another dialysis bag (23), and last dialysis bag (23) discharge gate is linked together through connecting tube (11) with the feed inlet of second drying device (18).
Preferably, the production line is characterized in that:
the third container (3), the second stirring barrel (4) and the fifth container (17) are respectively arranged at the tops of the third magnetic stirring device (16), the first magnetic stirring device (5) and the second magnetic stirring device (6).
Preferably, the production line is characterized in that:
the first stirring barrel (101), the fourth container (401) and the first drying device (7) are internally provided with a power stirring device (14).
Preferably, the production line is characterized in that: the connecting pipeline (11) is connected with an electromagnetic valve and a water pump.
Preferably, the production line is characterized in that:
and a first discharge valve (21) and a second discharge valve (22) are respectively connected on pipelines connected between the second drying device (18) and the refrigerating device (19) and between the refrigerating device (19) and the crushing device (20).
Preferably, the production line is characterized in that: the bottoms of the first container (1), the second container (2), the third container (3), the fourth container (401) and the fifth container (17) are connected with a supporting frame (15).
In addition, the invention also discloses a method for producing the washing product by the production line, which is characterized by comprising the following steps:
(1) In the first container, the houttuynia cordata extract or the derivative thereof is dissolved in deionized water or absolute ethyl alcohol to prepare a solution of the houttuynia cordata extract or the derivative thereof, wherein the houttuynia cordata extract or the derivative thereof is dissolved in absolute ethyl alcohol, and the houttuynia cordata extract or the derivative thereof is dissolved in deionized water.
(2) In the second container, cyclodextrin or a derivative thereof is dissolved in water to prepare cyclodextrin solution with the concentration of 10-500 mg/mL; wherein, the volume of the cyclodextrin solution is adjusted to be 9-11 times of the volume of the cordate houttuynia extract or the derivative solution thereof by the liquid flowmeter, and a detection tube arranged on a first stirring barrel on a second container is started at the same time to check that the concentration of the cyclodextrin solution is 10-500 mg/mL; clathrating the herba Houttuyniae extract or its derivatives with cyclodextrin or its derivatives; the houttuynia cordata extract or the derivative thereof does not need to be included by cyclodextrin or the derivative thereof;
(3) Mixing a houttuynia cordata extract or a derivative solution thereof with a cyclodextrin solution in the third container to form a first mixed solution;
(4) Stirring the first mixed solution in the first stirring barrel to uniformly mix the first mixed solution;
(5) Placing a proper amount of green tea related extract in the fourth container, and mixing the green tea related extract with the first mixed solution again to form a second mixed solution;
(6) Clathrating the herba Houttuyniae extract or its derivative with cyclodextrin or its derivative, and removing all solvents of the second mixed solution in the fourth container to obtain first product; for the cordate houttuynia extract or the derivative thereof in class b, removing all solvents of the second mixed solution in the fourth container is not needed to obtain a first product;
(7) Dissolving a first product of the houttuynia cordata extract or the derivative thereof in pure water in a fifth container, and sequentially adding a proper amount of auxiliary materials such as humectant, preservative, antioxidant, emulsifier, thickener, sweetener, mucilage, aromatic, flavoring agent and the like to obtain a second product; sequentially adding a proper amount of auxiliary materials such as humectant, preservative, antioxidant, emulsifier, thickener, sweetener, mucilage, aromatic, flavoring agent and the like into the second mixed solution to obtain a second product;
(8) Transferring the second product liquid to a dialysis bag, dialyzing with 100 times of pure water at room temperature for several times to remove free herba Houttuyniae extract or its derivative to obtain a mouthwash product in the form of collutory;
(9) And (3) freezing and drying the washing product in the form of mouthwash through the freezing device and the second drying device to obtain the washing product in the form of washing particles.
Preferably, the method further comprises the following steps:
(10) And further crushing the washing products in the form of washing particles by the crushing device according to the particle size requirement of the products.
Preferably, the cordate houttuynia washing product for caries prevention and bacteria inhibition is characterized in that:
the wash product is a wash particle for dissolution in water, or is a dentifrice, tooth gel or oral spray.
Compared with the prior art, the invention has the following beneficial effects:
(1) The automatic production line of the oral cavity washing product has the advantages of simple reaction process, easy control of the preparation process, and relatively higher safety and efficiency. The production line connects the material processing devices in a plurality of processes with each other through the connecting pipeline, and different components such as containers, electromagnetic valves, water pumps and the like are arranged on the connecting pipeline, thus forming a complete production system. The production line not only realizes the control of feeding and each reaction process of the processing device, but also has less occupied area, is beneficial to space utilization, and greatly improves the automation degree of washing product production.
(2) On the basis of the production line, the invention can realize the production of the conventional mouthwash product in the form of mouthwash and simultaneously realize the convenient-to-carry washing particles. When in use, a user only needs to use the washing particles after dissolving the washing particles by using water, and the washing particles can be stored for a long time.
(3) The final product, namely the caries prevention and bacteria inhibition washing product containing the houttuynia cordata extract or the derivative thereof, and the preparation method thereof also have the following advantages:
(a) The cyclodextrin or its derivative can improve the solubility of herba Houttuyniae extract or its derivative, and improve its taste, and is acceptable.
(b) The final product is effectively adhered to the tooth surface, so that the adhesion of bacteria is reduced, the antibacterial capacity is improved, and meanwhile, the product has good biocompatibility.
Drawings
FIG. 1 is a left side view of an automated manufacturing line for preparing oral rinse products;
FIG. 2 is a right front side view of an automated manufacturing line for preparing oral rinse products;
FIG. 3 is a top view of an automated manufacturing line for preparing oral rinse products;
FIG. 4 is an exploded view of an automated manufacturing line for preparing oral rinse products;
FIGS. 5A to 5B are diagrams showing characterization of sodium houttuyfonate-beta-cyclodextrin inclusion compound in sodium houttuyfonate wash products; FIG. 5A is a nuclear magnetic resonance spectrum; FIG. 5B is a phase solubility study;
FIGS. 6A to 6B are diagrams for examining biocompatibility of sodium houttuyfonate washing products; FIG. 6A is a cytotoxicity assay format; FIG. 6B is a graph of H & E staining of animal tissue;
fig. 7A to 7C are graphs showing antibacterial efficacy detection of sodium houttuyfonate wash products; FIG. 7A is an effect on S.mutans growth; wherein "11" represents a negative control group treated with deionized water alone without the addition of a rinse product; "1", "2", "3", "4", "5", "6", "7", "8", "9", "10" represent different experimental groups treated with the sodium houttuyfonate 3200, 1600, 600, 400, 200, 100, 50, 25, 12.5, 6.25 μg/mL of wash product, respectively; FIG. 7B is the effect on bacterial adhesion to the enamel tooth surface; FIG. 7C is the effect on bacterial biofilm on enamel tooth surfaces;
FIGS. 8A-8B show inhibition of growth of Streptococcus mutans by a houttuynia cordata extract wash product; FIG. 8A shows the effect of houttuynia cordata extract (HHE) and Green Tea Extract (GTE) or Tea Polyphenols (TPE) on mutans Streptococcus growth; FIG. 8B shows inhibition of S.mutans growth by different concentrations of houttuynia cordata extract (HHE) and Green Tea Extract (GTE) or Tea Polyphenols (TPE);
reference numerals:
1: a first container; 101: a first stirring barrel; 102: a liquid flow meter; 2: a second container; 3: a third container; 4: a second stirring barrel; 401: a fourth container; 5: a first magnetic stirring device; 6: a second magnetic stirring device; 7: a first drying device; 8: a first liquid inlet pipe; 9: placing a barrel; 10: a second liquid inlet pipe; 11: a connecting pipe; 12: a feed pipe; 13: a hopper; 14: a power stirring device; 15: a support frame; 16: a third magnetic stirring device; 17: a fifth container; 18: a second drying device; 19: a refrigerating device; 20: a pulverizing device; 21: a first discharge valve; 22: a second discharge valve; 23: and (5) a dialysis bag.
Detailed Description
The present invention will now be described in further detail with reference to the following examples and figures 1 to 8B, which are intended to illustrate, but not to limit, the invention.
All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
It should be noted that, in the description of the present invention, the terms "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply a specific orientation or configuration and operation that the device or element referred to must have, and thus should not be construed as limiting the present invention.
Furthermore, it should be understood that the dimensions of the various elements shown in the figures are not drawn to actual scale, e.g., the thickness or width of some layers may be exaggerated relative to other layers for ease of description.
It should be noted that like reference numerals and letters refer to like items in the following figures. Accordingly, once an item is defined or illustrated in one of the figures, it will not be further discussed or illustrated in detail in the description of the figures that follows.
Example 1:
an automated production line for preparing mouthwash and rinse particle rinse products, comprising:
as shown in fig. 1 to 4, the automated production line includes a first container 1, a second container 2, a third container 3, a fourth container 401, a fifth container 17, a placement barrel 9, a second drying device 18, a freezing device 19, and a pulverizing device 20. The placing barrel 9 is communicated with the second drying device 18, the second drying device 18 is communicated with the freezing device 19 and the freezing device 19 is communicated with the crushing device 20 through pipelines. The first container 1, the second container 2, the third container 3, the fourth container 401 and the fifth container 17 are all stainless steel containers, and the type of stainless steel is specifically 304 stainless steel. The top ends of the first container 1 and the second container 2 are connected with a first stirring barrel 101 through a bracket, and a liquid flowmeter 102 is connected to a pipeline connected with the first container 1 and the first stirring barrel 101, and the liquid flowmeter 102 can calculate the volume of liquid flowing into the container according to the flow rate of the liquid in the pipeline and the aperture of the pipeline; the two sides of the top end of the first stirring barrel 101 are communicated with a feed pipe 12 and a hopper 13, and a feed inlet formed in the top end of the third container 3 is respectively connected with discharge ports at the bottom ends of the first container 1 and the second container 2 through a connecting pipeline 11; the discharge port of the third container 3 is connected with the feed port at the top end of the fourth container 401 through a connecting pipeline 11; the first stirring barrel 101, the fourth container 401 and the first drying device 7 are internally provided with a power stirring device 14; the top ends of the fourth container 401 and the placing barrel 9 are communicated with a second liquid inlet pipe 10, and a discharge hole at the bottom end of the fourth container 401 is communicated with a feed inlet at the top end of the second stirring barrel 4 through a connecting pipe; a first drying device 7 is arranged on one side of the second stirring barrel 4, and a discharge port at the bottom end of the first drying device 7 is connected with a fifth container 17 through a connecting pipe; the top of the fifth container 17 is communicated with a first liquid inlet pipe 8, a discharge hole of the fifth container 17 is communicated with a dialysis bag 23 placed in the placing barrel 9 through a connecting pipeline 11, and the connecting pipeline 11 is connected with an electromagnetic valve and a water pump. Wherein, the placing barrels 9 are arranged in a plurality and a row, in the embodiment, the specific number of the placing barrels 9 is 5, and the number of the dialysis bags 23 is consistent with the number of the placing barrels 9; the outlet of one dialysis bag 23 is communicated with the inlet of the other dialysis bag 23 through a connecting pipeline 11, and the discharge port of the last dialysis bag 23 is communicated with the feed port of the second drying device 18 through the connecting pipeline 11; the third container 3, the second stirring tank 4 and the fifth container 17 are placed on top of the third magnetic stirring device 16, the first magnetic stirring device 5 and the second magnetic stirring device 6, respectively. The third magnetic stirring device 16, the first magnetic stirring device 5 and the second magnetic stirring device 6 utilize the characteristic that like poles of magnetic substances repel each other, and the polarities at the two ends of the base are continuously changed to push the magnetic stirring rod to rotate, so that the sample is further driven to rotate, and the sample is uniformly mixed. And then the sample is heated by the bottom temperature control plate, and the sample is uniformly heated by matching with the rotation of the magnetic stirrer to reach the designated temperature. A first discharge valve 21 and a second discharge valve 22 are connected to the pipes connecting the second drying device 18 and the freezing device 19 and the pulverizing device 20, respectively. The bottom ends of the first container 1, the second container 2, the third container 3, the fourth container 401 and the fifth container 17 are all connected with a supporting frame 15.
Example 2:
the method for preparing the caries preventing and antibacterial oral cavity washing product mouthwash containing the houttuynia cordata extract or the derivatives thereof and the washing particles by utilizing the automatic production line comprises the following steps:
firstly, a houttuynia cordata extract or a derivative thereof in class a or class b is put into a first stirring barrel 101 through a hopper 13 and a feed pipe 12, deionized water or absolute ethyl alcohol is injected, and the mixture is stirred by a dynamic stirring device 14 to obtain a first solution. The cyclodextrin or its derivative and water are placed in a first stirring tank 101 of a second container 2 and stirred by a dynamic stirring device 14 to obtain a second solution. The volume of the second solution is adjusted to be 9-11 times of the volume of the first solution through the liquid flowmeter 102, and meanwhile, a detection pipe arranged on the first stirring barrel 101 on the second container 2 is opened, and the concentration of the second solution is checked to be 10-500 mg/mL. The first solution and the second solution are pumped into a third container 3 and stirred for 12 to 36 hours by a third magnetic stirring device 16 to obtain a third solution. The third solution is pumped into the fourth container 401, and a certain amount of green tea-related extract is injected into the fourth container 401 to form a fourth mixed solution. The fourth mixed solution is stirred by the first magnetic stirring device 5, and is pumped into the first drying device 7 for drying after being stirred to obtain a first product. Opening a valve at the bottom of the first drying device 7, allowing the first product to enter a fifth container 17, adding purified water into the fifth container 17, sequentially adding a proper amount of auxiliary materials such as humectant, preservative, antioxidant, emulsifier, thickener, sweetener, mucilage, aromatic and flavoring agent, and continuously stirring by a second magnetic stirring device 6 to obtain a second product. The second product is pumped into the dialysis bag 23 and 100 volumes of purified water are injected into the holding tank 9, ensuring a room temperature environment at all times. And (3) performing 5 times of dialysis by using a dialysis bag to remove free components of the houttuynia cordata extract or the derivative thereof, thereby obtaining the washing product in the form of mouthwash. Finally, the liquid in the dialysis bag is frozen and dried to obtain the washing product in the form of washing particles. In addition, the washing particles can be further crushed by the crushing device according to the particle size requirement of the product.
The present invention uses houttuynia cordata extract or its derivative and cyclodextrin or its derivative to develop a washing product because the inventors found that: the cyclodextrin is used as a carrier for carrying the a-type houttuynia cordata extract or the derivative thereof, and the spatial structure of the cyclodextrin is used for wrapping the a-type houttuynia cordata extract or the derivative thereof, so that the biocompatibility of the whole drug carrying body can be effectively improved.
The final product prepared by the invention is preferably nano-scale, so that the targeted drug release can be realized in the subsequent use, the drug can be closely attached to the affected part of the teeth, and the drug effect of inhibiting the streptococcus mutans can be effectively exerted.
Taking sodium houttuyfonate and beta-cyclodextrin as examples, preparing a sodium houttuyfonate washing product according to the production line and the method, and correspondingly characterizing sodium houttuyfonate-beta-cyclodextrin inclusion compound particles in the washing product, wherein the method comprises the following experimental steps:
(1) Nuclear magnetic resonance experiment
And respectively dissolving the prepared sodium houttuyfonate-beta-cyclodextrin inclusion compound, beta-cyclodextrin and sodium houttuyfonate in deionized water to prepare proper concentration, transferring the mixture into a nuclear magnetic resonance tube, and detecting the nuclear magnetic resonance spectrum change of the three. The results are shown in the graph A of fig. 5, and the hydrogen spectrum of the sodium houttuyfonate-beta-cyclodextrin inclusion compound is shifted to a certain extent compared with the hydrogen spectrum of the sodium houttuyfonate, so that the successful preparation of the sodium houttuyfonate-beta-cyclodextrin inclusion compound is proved.
(2) Phase solubility experiments
Sodium houttuyfonate was dissolved in deionized water and diluted to a series of concentration gradients by measuring OD 283nm Value calculation of sodium houttuyfonate concentration and OD 283nm Standard curves between values. And weighing a proper amount of beta-cyclodextrin, and dissolving the beta-cyclodextrin in deionized water to prepare solutions with the concentration of 0mmol/L, 2mmol/L, 4mmol/L, 6mmol/L, 8mmol/L and 10 mmol/L. 10mL of each solution was taken, and an excessive amount of sodium houttuyfonate was added thereto, followed by magnetic stirring at 37℃for 24 hours. Filtering the supernatant with 0.22 μm filter membrane, and measuring OD with 1mL of the filtrate 283nm Values. As shown in fig. 5B, it can be seen that the solubility of sodium houttuyfonate is significantly improved after the sodium houttuyfonate is prepared into an inclusion compound by using beta-cyclodextrin.
In addition, the prepared sodium houttuyfonate washing product is subjected to biocompatibility investigation, and the method comprises the following experimental steps:
(1) In vitro cytotoxicity experiments
Dissolving the washing product (containing sodium houttuyfonate 100 μg/mL) in DMEM medium to give a certain concentration, adding into 96-well plate inoculated with gingival fibroblast, and adding 5% CO at 37deg.C 2 Culturing in cell incubator for 24h and 72h respectively, adding CCK-8 reagent, and measuring OD with enzyme-labeled instrument 450 The values, as shown in figure 6a, show no significant difference between the rinse product treated group and the deionized water control group, indicating that the rinse product is non-cytotoxic to gingival fibroblasts and has good cell compatibility.
(2) Animal tissue toxicity test
20 mice (10 male and female mice each) weighing 18-22 g were randomly divided into 2 groups (control group and experimental group). The control mice were given 1.5mL of deionized water by gavage, the experimental mice were given 1.5mL of the rinse product (in the form of mouthwash, containing 100. Mu.g/mL sodium houttuyfonate) twice daily, and the mice survived healthy for 4 weeks without any symptoms associated with toxic or side effects. Mice were treated after 4 weeks and the major organs (heart, liver, lung, kidney, stomach) were isolated for H & E staining to examine whether the wash product was toxic to the mouse tissues. As shown in fig. 6B, it can be seen that the five main organs of the mice of the experimental group were morphologically normal, and no significant difference was seen from the mice of the control group. The washing product has no obvious toxicity to mice and good histocompatibility.
In addition, the antibacterial efficacy of the prepared sodium houttuyfonate washing product is examined, and the antibacterial efficacy comprises the following experimental steps:
(1) Bacteriostasis experiment
Bacterial species: the bacteria used were all international standard strains, streptococcus mutans (Streptcoccus mutans, ATCC 25175). 100. Mu.L of final concentration 10 was added to each well of a 96-well plate 5 ～10 6 Bacterial suspension of CFU/mL, sodium houttuyfonate washing products with different concentrations are dissolved in BHI liquid culture medium, and the temperature is kept constant at 37 ℃ and 85% N 2 、5％CO 2 And 10% H 2 Culturing for 24h under the anaerobic condition of the mixed gas, and confirming the minimum inhibitory concentration by coating the BHI solid culture medium. As a result, as shown in FIG. 7A, it was found that the washing product groups ("1", "2", "3", "4", "5", "6", "7", "8", "9", "10" represent sodium houttuyfonate 3200, 1600, 600, 400, 200, 100, 50, 25, 12.5, 6.25. Mu.g/mL concentration groups), respectively, had a concentration-dependent inhibitory effect on the growth of Streptococcus mutans compared with the deionized water control group ("11" labeled), wherein the minimum inhibitory concentration on Streptococcus mutans was 100. Mu.g/mL of sodium houttuyfonate in the washing product group ("6" labeled group). Subsequent additional experiments were performed with 100. Mu.g/mL of a wash product containing sodium houttuyfonate.
(2) Enamel surface bacterial adhesion experiments
Coating enamel part of human tooth with self-setting material to obtain enamel with bottom surface width of 4mm and height of 2mm, soaking in 37% phosphoric acid solution for 3min, and washing with deionized water. Placing enamel sheet and dentin sheet in a container containing 10 7 In CFU/mL of Streptococcus mutans bacterial liquid, anaerobic culturing at 37deg.C for 1 hr, and treating with deionized water (control group) and washing product (experimental group) respectively for 2min every 6 hr. After 24h, the cells were rinsed with PBSWashing, detecting adhesion of mutans balls on enamel surface by using a scanning electron microscope, and as shown in a result of B in FIG. 7, it can be seen that a large amount of mutans streptococcus is adhered on enamel surface of the control group, and is aggregated to form colony; while the number of streptococcus mutans on the enamel surface of the experimental group is obviously reduced. The washing product has obvious effect of inhibiting streptococcus mutans from adhering to the enamel surface.
(3) Dental enamel surface bacterial biofilm investigation experiment
Coating enamel part of human tooth with self-setting material to obtain enamel with bottom surface width of 4mm and height of 2mm, soaking in 37% phosphoric acid solution for 3min, and washing with deionized water. Placing enamel sheet and dentin sheet in a container containing 10 7 In CFU/mL of Streptococcus mutans bacterial liquid, anaerobic culturing at 37deg.C for 24 hr, and treating with deionized water (control group) and washing product (experimental group) respectively for 2min every 6 hr. After 24h, the bacterial biofilm was rinsed with PBS and detected using a bacterial dead-alive staining kit and a confocal laser microscope, the results of which are shown in FIG. 7C. It can be seen that a large number of active mutans streptococcus colonies remained in the enamel surface of the control group, while the number of mutans streptococcus colonies on the enamel surface of the experimental group was significantly reduced, and the number of dead bacteria was significantly increased compared with the control group. The washing product can obviously destroy the biological membrane of the streptococcus mutans, and the obvious inhibition effect of the washing product on the streptococcus mutans is proved again.
In addition, taking houttuynia cordata extract, green tea extract and tea polyphenol (more than or equal to 98%) as examples, different houttuynia cordata extract washing products are prepared according to the production line and the method, and the influence of the growth of streptococcus mutans is examined, and the method comprises the following experimental steps:
100. Mu.L of final concentration was ensured to be 10 per well in 96-well plates 5 ～10 6 CFU/mL bacterial liquid and houttuynia cordata extract washing products with different concentrations are subjected to anaerobic condition culture for 24 hours, then diluted to a certain proportion, 5 mu L of the mixture is dripped on a solid culture medium, the antibacterial effect of the houttuynia cordata extract washing products is examined after the anaerobic condition culture for 24 hours, and the results are shown in fig. 8A to 8B. 5mg/mL of herba Houttuyniae extract and 5mg/mL of green tea extract, 1mg/mL of herba Houttuyniae extract and 5mg/mL of green tea extract1mg/mL of tea polyphenol, and the obtained washing products respectively show remarkable antibacterial effect on the growth of streptococcus mutans (A in figure 8), and the inhibition rate is close to 100% (B in figure 8).
The foregoing description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and any simple modification, variation and equivalent structural transformation made according to the technical matter of the present invention still fall within the scope of the technical solution of the present invention.
Claims (13)
1. A cordate houttuynia washing product for caries prevention and bacteriostasis, which is characterized in that the effective components of the washing product comprise an A component and a B component, wherein:
the component A is herba Houttuyniae extract or its derivative, and contains one or more of herba Houttuyniae extract, herba Houttuyniae oil, houttuynin, sodium houttuyfonate, and sodium new houttuyfonate; wherein,,
the water-poor houttuynia cordata oil, houttuynin, sodium houttuyfonate, sodium new houttuyfonate and the like are represented as a houttuynia cordata extract or a derivative thereof;
the herba Houttuyniae extract has good water solubility and is represented by b-type herba Houttuyniae extract or its derivative;
and when the component A is used for preparing the washing product, dissolving the cordate houttuynia extract or the derivative thereof in absolute ethyl alcohol, and dissolving the cordate houttuynia extract or the derivative thereof in deionized water;
the component B is green tea related extract including one or more of green tea extract, tea polyphenols and catechin;
the mass ratio of the A to the B is such that the washing product has both antibacterial effect and color and taste.
2. A cordate houttuynia washing product for caries prevention and bacteria inhibition according to claim 1, wherein: preferably, the method comprises the steps of,
the washing product also comprises a proper amount of auxiliary materials, wherein the auxiliary materials comprise: one or more of humectants, preservatives, antioxidants, emulsifiers, thickeners, sweeteners, mucilage, fragrances, and flavoring agents.
3. A production line for producing a dental caries preventing and inhibiting cordate houttuynia washing product according to claim 1 or 2, comprising:
a first container (1), a second container (2), a third container (3), a fourth container (401), a fifth container (17), a placing barrel (9), a second drying device (18) and a freezing device (19), wherein:
the placing barrel (9) and the second drying device (18) and the freezing device (19) are communicated through pipelines;
the top ends of the first container (1) and the second container (2) are connected with a first stirring barrel (101) through a bracket, and a liquid flowmeter (102) is connected to a pipeline connected with the first container (1) and the first stirring barrel (101);
the two sides of the top end of the first stirring barrel (101) are communicated with a feed pipe (12) and a hopper (13), and a feed inlet formed in the top end of the third container (3) is respectively connected with discharge ports at the bottom ends of the first container (1) and the second container (2) through a connecting pipeline (11);
the discharge port of the third container (3) is connected with the feed port at the top end of the fourth container (401) through a connecting pipeline (11);
the top ends of the fourth container (401) and the placing barrel (9) are communicated with a second liquid inlet pipe (10), and a discharge hole at the bottom end of the fourth container (401) is communicated with a feed inlet at the top end of the second stirring barrel (4) through a connecting pipe;
a first drying device (7) is arranged on one side of the second stirring barrel (4), a discharge hole at the bottom end of the first drying device (7) is connected with a fifth container (17) through a connecting pipe, a first liquid inlet pipe (8) is communicated with the top of the fifth container (17), and the discharge hole of the fifth container (17) is communicated with a dialysis bag (23) arranged in the placing barrel (9) through a connecting pipeline (11).
4. A production line according to claim 3, characterized in that:
the production line further comprises a comminuting device (20); the refrigerating device (19) is communicated with the crushing device (20) through a pipeline.
5. A production line according to claim 3, characterized in that:
the utility model discloses a drying device, including placing bucket (9), including a plurality of and being one row setting, the quantity of dialysis bag (23) is unanimous with placing bucket (9), and the export of one dialysis bag (23) is linked together through connecting tube (11) with the import of another dialysis bag (23), and last dialysis bag (23) discharge gate is linked together through connecting tube (11) with the feed inlet of second drying device (18).
6. A production line according to claim 3, characterized in that:
the third container (3), the second stirring barrel (4) and the fifth container (17) are respectively arranged at the tops of the third magnetic stirring device (16), the first magnetic stirring device (5) and the second magnetic stirring device (6).
7. A production line according to claim 3, characterized in that:
the first stirring barrel (101), the fourth container (401) and the first drying device (7) are internally provided with a power stirring device (14).
8. A production line according to claim 3, characterized in that: the connecting pipeline (11) is connected with an electromagnetic valve and a water pump.
9. The production line according to claim 4, characterized in that:
and a first discharge valve (21) and a second discharge valve (22) are respectively connected on pipelines connected between the second drying device (18) and the refrigerating device (19) and between the refrigerating device (19) and the crushing device (20).
10. A production line according to claim 3, characterized in that: the bottoms of the first container (1), the second container (2), the third container (3), the fourth container (401) and the fifth container (17) are connected with a supporting frame (15).
11. A method of producing the washing product according to any one of claims 3 to 10, characterized in that the method comprises the steps of:
(1) Dissolving herba Houttuyniae extract or its derivative in deionized water or anhydrous ethanol in the first container to obtain herba Houttuyniae extract or its derivative solution, wherein herba Houttuyniae extract or its derivative of class a is dissolved in anhydrous ethanol, and herba Houttuyniae extract or its derivative of class b is dissolved in deionized water;
(2) In the second container, cyclodextrin or a derivative thereof is dissolved in water to prepare cyclodextrin solution with the concentration of 10-500 mg/mL; wherein, the volume of the cyclodextrin solution is adjusted to be 9-11 times of the volume of the cordate houttuynia extract or the derivative solution thereof by the liquid flowmeter, and a detection tube arranged on a first stirring barrel on a second container is started at the same time to check that the concentration of the cyclodextrin solution is 10-500 mg/mL; clathrating the herba Houttuyniae extract or its derivatives with cyclodextrin or its derivatives; the houttuynia cordata extract or the derivative thereof does not need to be included by cyclodextrin or the derivative thereof;
(3) Mixing a houttuynia cordata extract or a derivative solution thereof with a cyclodextrin solution in the third container to form a first mixed solution;
(4) Stirring the first mixed solution in the first stirring barrel to uniformly mix the first mixed solution;
(5) Placing a proper amount of green tea related extract in the fourth container, and mixing the green tea related extract with the first mixed solution again to form a second mixed solution;
(6) Clathrating the herba Houttuyniae extract or its derivative with cyclodextrin or its derivative, and removing all solvents of the second mixed solution in the fourth container to obtain first product; for the cordate houttuynia extract or the derivative thereof in class b, removing all solvents of the second mixed solution in the fourth container is not needed to obtain a first product;
(7) Dissolving a first product of the houttuynia cordata extract or the derivative thereof in pure water in a fifth container, and sequentially adding a proper amount of auxiliary materials such as humectant, preservative, antioxidant, emulsifier, thickener, sweetener, mucilage, aromatic, flavoring agent and the like to obtain a second product; sequentially adding a proper amount of auxiliary materials such as humectant, preservative, antioxidant, emulsifier, thickener, sweetener, mucilage, aromatic, flavoring agent and the like into the second mixed solution to obtain a second product;
(8) Transferring the second product liquid to a dialysis bag, dialyzing with 100 times of pure water at room temperature for several times to remove free herba Houttuyniae extract or its derivative to obtain a mouthwash product in the form of collutory;
(9) And (3) freezing and drying the washing product in the form of mouthwash through the freezing device and the second drying device to obtain the washing product in the form of washing particles.
12. The method of claim 11, further comprising the step of:
(10) And further crushing the washing products in the form of washing particles by the crushing device according to the particle size requirement of the products.
13. A cordate houttuynia washing product for anticarious bacteria inhibition according to claim 1 or 2, characterized in that:
the wash product is a wash particle for dissolution in water, or is a dentifrice, tooth gel or oral spray.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2022112328789 | 2022-10-09 | ||
| CN202211232878.9A CN115444799A (en) | 2022-10-09 | 2022-10-09 | A herba Houttuyniae wash product for preventing caries and inhibiting bacteria and production line thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116421515A true CN116421515A (en) | 2023-07-14 |
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ID=84308147
Family Applications (3)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211232878.9A Withdrawn CN115444799A (en) | 2022-10-09 | 2022-10-09 | A herba Houttuyniae wash product for preventing caries and inhibiting bacteria and production line thereof |
| CN202310308640.8A Pending CN116531442A (en) | 2022-10-09 | 2023-03-27 | Houttuynia cordata green tea composition with caries preventing and antibacterial activity and application thereof |
| CN202310305414.4A Pending CN116421515A (en) | 2022-10-09 | 2023-03-27 | Houttuynia cordata washing product for caries prevention and bacteriostasis and production line thereof |
Family Applications Before (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211232878.9A Withdrawn CN115444799A (en) | 2022-10-09 | 2022-10-09 | A herba Houttuyniae wash product for preventing caries and inhibiting bacteria and production line thereof |
| CN202310308640.8A Pending CN116531442A (en) | 2022-10-09 | 2023-03-27 | Houttuynia cordata green tea composition with caries preventing and antibacterial activity and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (3) | CN115444799A (en) |
-
2022
- 2022-10-09 CN CN202211232878.9A patent/CN115444799A/en not_active Withdrawn
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2023
- 2023-03-27 CN CN202310308640.8A patent/CN116531442A/en active Pending
- 2023-03-27 CN CN202310305414.4A patent/CN116421515A/en active Pending
Also Published As
| Publication number | Publication date |
|---|---|
| CN115444799A (en) | 2022-12-09 |
| CN116531442A (en) | 2023-08-04 |
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