CN115444799A - A herba Houttuyniae wash product for preventing caries and inhibiting bacteria and production line thereof - Google Patents
A herba Houttuyniae wash product for preventing caries and inhibiting bacteria and production line thereof Download PDFInfo
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- CN115444799A CN115444799A CN202211232878.9A CN202211232878A CN115444799A CN 115444799 A CN115444799 A CN 115444799A CN 202211232878 A CN202211232878 A CN 202211232878A CN 115444799 A CN115444799 A CN 115444799A
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- China
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- container
- extract
- product
- derivative
- houttuynia cordata
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- A61K31/35—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin having six-membered rings with one oxygen as the only ring hetero atom
- A61K31/352—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin having six-membered rings with one oxygen as the only ring hetero atom condensed with carbocyclic rings, e.g. methantheline
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- A61K8/4973—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with oxygen as the only hetero atom
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- Medicines Containing Plant Substances (AREA)
Abstract
A herba Houttuyniae wash product for preventing dental caries and inhibiting bacteria and its preparation method are provided, wherein the effective components of the wash 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 limited. The production line is connected with each other through the connecting pipeline, and the connecting pipeline is provided with different containers, electromagnetic valves, water pumps and the like to form a complete production system, so that the feeding of the washing product and the control of each reaction process are realized, 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 spray and the like. The invention not only can obviously inhibit the main pathogenic bacteria of caries, namely the streptococcus mutans, but also has good biocompatibility and production benefit, and is beneficial to solving the urgent need of effective, safe and long-term use of oral cavity washing products in the aspects of oral cavity health care and oral cavity disease prevention.
Description
Technical Field
The invention relates to the technical field of production equipment of oral cavity washing products, in particular to an anti-caries oral cavity washing product containing houttuynia cordata extract or derivatives thereof and an automatic production line thereof.
Background
According to the fourth national oral epidemiological survey data, the caries prevalence rate of adults in China is up to more than 80 percent, and the caries prevalence rate is the main reason causing tooth defect and pain. Mutans streptococci are the leading causative bacteria of caries. Currently, the common method of controlling streptococcus mutans is to mechanically control plaque by brushing and to clean the mouth using a rinse product with added antibacterial ingredients. However, it is difficult to brush teeth deep into the crevices and under the gingival margin. The washing product can deeply penetrate into the deep part of the tooth slit and under the gingival margin to remove oral bacteria to a certain degree. However, most of the antibacterial components in the existing washing products are substances such as alcohol, chlorohexidine, metronidazole and the like, and the long-term use of the washing products can easily cause white lesions of mucous membranes, and cause the problems of tartar formation, tooth surface coloring, taste change and the like. Therefore, it is important to find new safe and effective anticaries substances.
The houttuynia cordata can be directly eaten as a medicinal and edible plant and is also a traditional Chinese medicinal material with high clinical application value. The main effective component of the houttuynia cordata extract is houttuynine sodium bisulfite, which has good antibacterial, antiviral and anti-inflammatory effects. Sodium houttuyfonate and sodium new houttuyfonate are artificially synthesized sodium bisulfite derivatives of natural houttuyfonate. Research shows that the houttuynine sodium bisulfite derivatives have more stable properties and retain the bacteriostatic action on staphylococcus aureus, dysentery bacillus, candida albicans, colon bacillus and the like. Meanwhile, researches show that the houttuynia cordata extract or the derivative thereof has positive effects on prevention and treatment of oral bacterial infectious diseases. Therefore, the houttuynia cordata extract or the derivative thereof is an ideal anticarious substance for oral cavity washing products.
The water solubility of houttuynia cordata extracts or derivatives thereof such as houttuynia cordata oil, houttuynine sodium bisulfite, sodium houttuyfonate and sodium new houttuyfonate is poor, so the application of the extract is limited to a certain extent, and how to improve the solubility of the extract is a key problem influencing the use of the extract. Chinese patent CN113143904A (application of houttuynine sodium bisulfite analogue in preparing streptococcus mutans growth and biomembrane inhibitor) discloses application of houttuynine sodium bisulfite analogue in preparing streptococcus mutans growth and biomembrane inhibitor, which can inhibit growth and biomembrane formation of streptococcus mutans, and has potential as anticariogenic drug. However, this technique has the following drawbacks: (1) The dissolving mother liquor is an organic solvent dimethyl sulfoxide, has certain toxicity, and can stimulate eyes, skin and respiratory system; (2) The technology does not design a corresponding production line, and further product conversion and application are hindered.
In addition, most of the existing washing products are in a mouth wash form, are in a liquid form, 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 usually arranged in a dispersed manner, occupy larger space and increase the space cost; moreover, the reaction process of the existing mouthwash product in the manufacturing process is relatively complex and is not easy to control, so that the safety and the efficiency of the production are influenced.
In conclusion, there is a need to develop a production line with a relatively simple reaction process to produce an oral cavity washing product which is convenient to carry, has no obvious stimulation to oral mucosa and has a good oral cavity antibacterial effect, so that the urgent need of people for effective, safe and long-term use of the oral cavity washing product in the aspects of oral cavity health care and oral cavity disease prevention can be solved.
Disclosure of Invention
The invention aims to provide an anti-caries and antibacterial oral cavity washing product containing houttuynia cordata extract or derivatives thereof and an automatic production line thereof, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
the houttuynia cordata washing product for preventing caries and inhibiting bacteria is characterized in that the effective components of the washing product comprise a component A and a component B, wherein:
the component A is herba Houttuyniae extract or its derivative, which contains one or more of herba Houttuyniae extract, herba Houttuyniae oil, houttuynin, sodium houttuynin, and sodium new houttuynin; wherein,
herba Houttuyniae oil, houttuynin, sodium new houttuynin, etc. with poor water solubility are represented as type a herba Houttuyniae extract or its derivatives;
houttuynia cordata extract or the like having good water solubility is represented as a type b houttuynia cordata extract or a derivative thereof;
and when the component A is used for preparing the washing product, the houttuynia cordata extract or the derivative thereof in the category a is dissolved by absolute ethyl alcohol, and the houttuynia cordata extract in the category b or the derivative thereof in the category b is dissolved by 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 A to B is that the washing product has antibacterial effect, color and taste.
Preferably, the houttuynia cordata washing product for preventing caries and inhibiting bacteria is characterized in that:
the washing product also comprises a proper amount of auxiliary materials, and the auxiliary materials comprise: one or more of a humectant, a preservative, an antioxidant, an emulsifier, a thickener, a sweetener, a mucilage, an aromatic and a flavoring agent.
In addition, the invention also discloses a production line of the houttuynia cordata washing product for preventing caries and inhibiting bacteria, 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 tub (9), a second drying device (18) and a freezing device (19), wherein:
the placing barrel (9) and the second drying device (18) and the refrigerating 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 connecting the first container (1) and the first stirring barrel (101);
a feeding pipe (12) and a hopper (13) are communicated with two sides of the top end of the first stirring barrel (101), and a feeding hole formed in the top end of the third container (3) is respectively connected with discharging holes at the bottom ends of the first container (1) and the second container (2) through a connecting pipeline (11);
the discharge hole of the third container (3) is connected with the feed hole 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 hole in the top end of the second stirring barrel (4) through a connecting pipe;
first drying device (7) have been placed to second agitator (4) one side, and first drying device (7) bottom discharge gate is connected with fifth container (17) through the connecting pipe, and fifth container (17) top intercommunication has first feed liquor pipe (8), and fifth container (17) discharge gate is linked together through connecting tube (11) and dialysis bag (23) of placing in placing bucket (9).
Preferably, the production line is characterized in that:
the production line further comprises a shredding device (20); the freezing device (19) is communicated with the crushing device (20) through a pipeline.
Preferably, the production line is characterized in that:
place bucket (9) have a plurality ofly and be one row of setting, the quantity of dialysis bag (23) with place bucket (9) unanimous, the export of a dialysis bag (23) and the import of another dialysis bag (23) all are linked together through connecting tube (11), the feed inlet of last dialysis bag (23) discharge gate and second drying device (18) is linked together through connecting tube (11).
Preferably, the production line is characterized in that:
and the third container (3), the second stirring barrel (4) and the fifth container (17) are respectively placed 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:
and power stirring devices (14) are arranged in the first stirring barrel (101), the fourth container (401) and the first drying device (7).
Preferably, the production line is characterized in that: the pipeline of 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 to pipelines connected between the second drying device (18) and the freezing device (19) and between the freezing device (19) and the crushing device (20).
Preferably, the production line is characterized in that: 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 support 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) Dissolving herba Houttuyniae extract or its derivative in deionized water or anhydrous ethanol to obtain herba Houttuyniae extract or its derivative solution, wherein the a type herba Houttuyniae extract or its derivative is dissolved in anhydrous ethanol, and the b type herba Houttuyniae extract or its derivative is dissolved in deionized water.
(2) In the second container, cyclodextrin or a derivative thereof is dissolved in water to prepare a cyclodextrin solution with the concentration of 10-500 mg/mL; adjusting the volume of the cyclodextrin solution to be 9-11 times of the volume of the houttuynia cordata extract or derivative solution thereof through the liquid flow meter, simultaneously opening a detection tube arranged on a first stirring barrel on a second container, and checking that the concentration of the cyclodextrin solution is 10-500 mg/mL; for the extract of the houttuynia cordata or the derivative thereof, cyclodextrin or the derivative thereof is adopted for inclusion; for the extract of the houttuynia cordata or the derivative thereof, the extract of the houttuynia cordata b does not need to be included by cyclodextrin or the derivative thereof;
(3) Mixing a solution of the houttuynia cordata extract or the derivative thereof in the category a 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 extract or derivative of herba Houttuyniae a with cyclodextrin or its derivative, and removing all solvents in the second mixture in the fourth container to obtain first product; for the b-type houttuynia cordata extract or the derivative thereof, all solvents of the second mixed solution in the fourth container do not need to be removed, and a first product is obtained;
(7) Dissolving the first product of the extract of the houttuynia cordata or the derivative of the extract of the houttuynia cordata in the fifth container by pure water, and sequentially adding a proper amount of auxiliary materials such as a humectant, a preservative, an antioxidant, an emulsifier, a thickener, a sweetening agent, a mucilage, an aromatic, a flavoring agent and the like to obtain a second product; adding appropriate amount of humectant, antiseptic, antioxidant, emulsifier, thickener, sweetener, mucilage, aromatic and correctant into the second mixed solution to obtain second product;
(8) Transferring said second product liquid to a dialysis bag and dialyzing against 100 volumes of pure water at room temperature for a plurality of times to remove free houttuynia cordata extract or a derivative thereof to obtain a rinse product in the form of a mouthwash;
(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) The washing product in the form of washing particles is further comminuted by the comminuting device according to the product particle size requirement.
Preferably, the houttuynia cordata washing product for preventing caries and inhibiting bacteria is characterized in that:
the washing product is washing particles dissolved in water, or 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 of 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, so that a complete production system is formed. 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 the production of washing products.
(2) On the basis of the production line, the invention can realize the production of the washing product in the form of the conventional mouthwash and can also realize the washing particle which is convenient to carry. When the washing particle is used, a user only needs to dissolve the washing particle by using water, and the washing particle can be stored for a long time.
(3) The final product contains the houttuynia cordata extract or the derivative thereof, and the caries-preventing and bacteria-inhibiting washing product and the preparation method thereof also have the following advantages:
(a) The cyclodextrin or the derivative thereof can improve the solubility of the houttuynia cordata extract or the derivative thereof and improve the mouthfeel, and is easy to accept.
(b) The final product is effectively adhered to the surface of the tooth, so that the adhesion of bacteria is reduced, the bacteriostatic ability is improved, and the biocompatibility is good.
Drawings
FIG. 1 is a left side isometric view of an automated manufacturing line for preparing oral rinse products;
FIG. 2 is a right front side elevational 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;
figure 4 is an exploded view of an automated production line for preparing oral rinse products;
FIGS. 5A to 5B are diagrams showing the representation of sodium houttuyfonate-beta-cyclodextrin inclusion compound in a sodium houttuyfonate toiletry product; FIG. 5A is a nuclear magnetic resonance spectrum; FIG. 5B is a phase solubility investigation diagram;
FIGS. 6A-6B are views of the biocompatibility of the sodium houttuyfonate rinse product; FIG. 6A is a cytotoxicity assay; FIG. 6B is a H & E staining profile of animal tissue;
FIGS. 7A-7C are graphs showing the bacteriostatic efficacy of a sodium houttuyfonate rinse product; FIG. 7A is a graph of the effect on growth of S.mutans; 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" and "10" represent the different experimental groups treated with the contained sodium houttuyfonate 3200, 1600, 600, 400, 200, 100, 50, 25, 12.5, 6.25 μ g/mL of the washing product, respectively; FIG. 7B is a graph showing the effect of bacterial adhesion to the enamel tooth surface; FIG. 7C is the effect on bacterial biofilm on the enamel tooth surface;
FIGS. 8A-8B show the inhibitory effect of the houttuynia cordata extract rinse product on the growth of Streptococcus mutans; FIG. 8A shows the effect of houttuynia cordata extract (HHE) with Green Tea Extract (GTE) or Tea Polyphenols (TPE) on the growth of Streptococcus mutans; FIG. 8B shows the inhibition of Streptococcus mutans growth by different concentrations of houttuynia cordata extract (HHE) and Green Tea Extract (GTE) or Tea Polyphenols (TPE);
reference numerals are as follows:
1: a first container; 101: a first mixing tank; 102: a liquid flow meter; 2: a second container; 3: a third container; 4: a second mixing tank; 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 the barrel; 10: a second liquid inlet pipe; 11: connecting a pipeline; 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 freezing device; 20: a crushing device; 21: a first discharge valve; 22: a second discharge valve; 23: a dialysis bag.
Detailed Description
The present invention will now be described in further detail with reference to the following examples and accompanying figures 1 to 8B, which are illustrative and not limiting of the invention.
All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
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, and are only for convenience of description and simplification of description, and do not indicate or imply specific orientations that the devices or elements referred to must have or the configuration and operation of the specific orientations, and thus, the present invention should not be construed as being limited.
Further, it will be appreciated that the dimensions of the various elements shown in the figures are not drawn to scale, for ease of description, e.g., the thickness or width of some layers may be exaggerated relative to other layers.
It should be noted that like reference numerals and letters refer to like items in the following figures. Thus, once an item is defined or illustrated in a drawing, it will not be further specifically discussed or illustrated in the following description of the drawing.
Example 1:
an automated production line for preparing oral mouthwash and granule rinse products, comprising:
as shown in fig. 1 to 4, the automated manufacturing line includes a first container 1, a second container 2, a third container 3, a fourth container 401, a fifth container 17, a placing tub 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 refrigerating device 19, and the refrigerating 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 stainless steel containers, and the kind of stainless steel is 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 support, a pipeline connected with the first container 1 and the first stirring barrel 101 is connected with a liquid flowmeter 102, and the liquid flowmeter 102 can measure and calculate the volume of liquid flowing into the containers according to the flow rate of the liquid in the pipeline and the aperture of the pipeline; a feeding pipe 12 and a hopper 13 are communicated with two sides of the top end of the first stirring barrel 101, and a feeding hole formed in the top end of the third container 3 is respectively connected with discharging holes at the bottom ends of the first container 1 and the second container 2 through a connecting pipeline 11; the discharge hole of the third container 3 is connected with the feed hole 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 1O, and a discharge hole at the bottom end of the fourth container 401 is communicated with a feed hole on 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, the 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, there are a plurality of placing barrels 9 and arrange in a row, in this embodiment, the specific number of placing barrels 9 is 5, and the number of dialysis bags 23 is the same as that of 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 outlet of the last dialysis bag 23 is communicated with the inlet of the second drying device 18 through the connecting pipeline 11; the third container 3, the second stirring barrel 4 and the fifth container 17 are respectively placed on the tops of the third magnetic stirring device 16, the first magnetic stirring device 5 and the second magnetic stirring device 6. 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 push the magnetic stirrer to rotate by constantly changing the polarities at the two ends of the base, so as to further drive the sample to rotate, and uniformly mix the sample. 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 specified temperature. A first discharge valve 21 and a second discharge valve 22 are connected to pipes connected between the second drying device 18 and the freezing device 19 and between 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 support frame 15.
Example 2:
the method for preparing the caries-preventing and bacteria-inhibiting mouth wash product mouthwash and the washing particles containing the houttuynia cordata extract or the derivatives thereof by utilizing the automatic production line comprises the following steps:
firstly, a type a or type b houttuynia cordata extract or a derivative thereof and deionized water or absolute ethyl alcohol are injected into a first stirring barrel 101 through a hopper 13 and a feeding pipe 12, and a first solution is obtained after stirring by a power stirring device 14. And putting the cyclodextrin or the derivative thereof and water into a first stirring barrel 101 of the second container 2, and stirring by a power 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 by the liquid flow meter 102, and the concentration of the second solution is checked to be 10-500 mg/mL by opening the detection tube arranged on the first stirring barrel 101 on the second container 2. Pumping the first solution and the second solution into a third container 3, and stirring for 12-36h by a third magnetic stirring device 16 to obtain a third solution. The third solution is pumped into a fourth vessel 401 and a quantity of green tea-related extract is injected into the fourth vessel 401 to form a fourth mixed liquor. And stirring the fourth mixed solution by using a first magnetic stirring device 5, and pumping the stirred fourth mixed solution into a first drying device 7 for drying to obtain a first product. And 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 a humectant, a preservative, an antioxidant, an emulsifier, a thickener, a sweetener, a mucilage, an aromatic, a flavoring agent and the like, and continuously stirring through a second magnetic stirring device 6 to obtain a second product. The second product is pumped into the dialysis bag 23 and 100 times the volume of purified water is injected into the placing tub 9, ensuring a room temperature environment at all times. Dialyzing with dialysis bag for 5 times to remove free components of herba Houttuyniae extract or its derivatives to obtain collutory in the form of collutory. 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 requirement of the particle size of the product.
The present invention has developed a washing product using houttuynia cordata extract or its derivative and cyclodextrin or its derivative 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 a-type houttuynia cordata extract or the derivative thereof is wrapped by the space structure of the cyclodextrin, so that the biocompatibility of the whole medicine carrying body can be effectively improved.
The final product prepared by the invention is preferably in nanometer level, so that the subsequent use can also realize targeted drug release, the drug is tightly attached to the affected part of the tooth, and the drug effect of inhibiting streptococcus mutans is effectively exerted.
Taking sodium houttuyfonate and beta-cyclodextrin as examples, the sodium houttuyfonate washing product is prepared according to the production line and the method, and the sodium houttuyfonate-beta-cyclodextrin inclusion compound particles in the washing product are correspondingly characterized, and the method comprises the following experimental steps:
(1) Nuclear magnetic resonance experiment
Respectively dissolving the prepared sodium houttuyfonate-beta-cyclodextrin inclusion compound, beta-cyclodextrin and sodium houttuyfonate in deionized water to prepare a proper concentration, transferring the solution into a nuclear magnetic tube, and detecting the nuclear magnetic resonance spectrum change of the three. As shown in a of fig. 5, it can be seen that the hydrogen spectrum of the sodium houttuyfonate-beta-cyclodextrin inclusion compound shifts somewhat compared with that of sodium houttuyfonate, which proves the successful preparation of the sodium houttuyfonate-beta-cyclodextrin inclusion compound.
(2) Phase solubility test
Dissolving sodium houttuyfonate in deionized water, diluting to obtain a series of concentration gradients, and determining OD 283nm Value calculation of sodium houttuyfonate concentration and OD 283nm Standard curve between values. Weighing deviceDissolving beta-cyclodextrin in deionized water to prepare solutions with the concentrations of 0mmol/L, 2mmol/L, 4mmol/L, 6mmol/L, 8mmol/L and 10 mmol/L. 10mL of each of the above solutions was added with an excess of sodium houttuyfonate, and the mixture was magnetically stirred at 37 ℃ for 24 hours. Filtering the supernatant with 0.22 μm filter membrane, collecting 1mL filtrate, and determining OD 283nm The value is obtained. As a result, as shown in B of fig. 5, it can be seen that the solubility of sodium houttuyfonate was significantly improved after the sodium houttuyfonate was prepared into an inclusion compound using β -cyclodextrin.
In addition, the prepared houttuynine sodium bisulfite washing product is examined for biocompatibility, and the method comprises the following experimental steps:
(1) In vitro cytotoxicity assay
Dissolving the washing product (containing sodium houttuyfonate 100 μ g/mL) in DMEM medium to give a certain concentration, adding 96-well plate inoculated with gingival fibroblast, and removing 5% of CO at 37 deg.C 2 Culturing in cell culture box for 24h and 72h, adding CCK-8 reagent, and measuring OD with enzyme labeling instrument 450 The results are shown as a in fig. 6, and it can be seen that the group treated with the washing product has no significant difference from the deionized water control group, indicating that the washing product has no cytotoxicity to gingival fibroblasts and good cell compatibility.
(2) Animal tissue toxicity test
20 mice (10 males and females) weighing 18 to 22g were divided into 2 groups (control group and experimental group) at random. The control group mice were gavaged with 1.5mL of deionized water, and the experimental group mice were gavaged with 1.5mL of the mouthwash product (in the form of mouthwash containing 100. Mu.g/mL of sodium houttuyfonate), twice a day, and observed for 4 weeks, so that the mice survived healthily without any symptoms related to toxic and side effects. Mice were treated after 4 weeks and major organs (heart, liver, lung, kidney, stomach) were isolated for H & E staining to investigate if the wash product was toxic to mouse tissues. As a result, as shown in fig. 6B, it was found that the morphology of five main organs was normal in the experimental group mouse, and no significant difference was observed compared with the control group mouse. The washing product has no obvious toxicity to mice and has good histocompatibility.
In addition, the investigation on the antibacterial efficacy of the prepared sodium houttuyfonate washing product comprises the following experimental steps:
(1) Experiment for inhibiting bacteria
The bacterial species: the bacteria used were all international standard strains, streptococcus mutans (Streptcoccus mutans, ATCC 25175). Adding 100 mul of the final concentration of 10 into each hole of a 96-hole plate 5 ～10 6 CFU/mL bacterial suspension, dissolving sodium houttuyfonate washing product with different concentrations in BHI liquid culture medium, maintaining at 37 deg.C, 85% by weight 2 、5％CO 2 And 10% of H 2 The mixed gas is cultured for 24 hours under anaerobic condition, and the minimum inhibitory concentration is confirmed by coating bacteria on BHI solid culture medium. As shown in a in fig. 7, it can be seen that the wash product groups ("1", "2", "3", "4", "5", "6", "7", "8", "9" and "10" represent the groups containing sodium houttuyfonate 3200, 1600, 600, 400, 200, 100, 50, 25, 12.5 and 6.25 μ g/mL respectively) had a concentration-dependent inhibitory effect on the growth of streptococcus mutans compared to the deionized water control group ("11" mark), wherein the minimum inhibitory concentration against streptococcus mutans was 100 μ g/mL of sodium houttuyfonate (the "6" mark group). Subsequent further experiments a rinse product containing 100 μ g/mL sodium houttuyfonate was selected for testing.
(2) Bacterial adhesion test on enamel surface
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 piece and dentin piece in 10 7 Culturing in CFU/mL Streptococcus mutans solution at 37 deg.C for 1 hr under anaerobic condition, and treating with deionized water (control group) and washing product (experimental group) for 2min once every 6 hr. After 24h, the cells are rinsed by PBS, and the adhesion condition of the mutans streptococci on the enamel surface is detected by using a scanning electron microscope, and the result is shown as B in figure 7, so that a large amount of mutans streptococci are adhered to the enamel surface of the control group and aggregated to form colonies; the number of the streptococcus mutans on the enamel surface of the test group is obviously reduced. The washing product is proved to have obvious function of inhibiting streptococcus mutans from adhering to the enamel surface.
(3) Examination experiment for investigating bacterial biomembrane on enamel surface
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 and dentin sheets in 10 7 Culturing in CFU/mL Streptococcus mutans solution at 37 deg.C under anaerobic condition for 24 hr, and treating with deionized water (control group) and washing product (experimental group) for 2min once every 6 hr. After 24h, the membrane was rinsed with PBS and the bacterial biofilm was detected using a bacterial viability staining kit and confocal laser microscopy, the results are shown in FIG. 7C. As can be seen, a large number of active Streptococcus mutans colonies still remained on the enamel surface of the control group, while the number of Streptococcus mutans colonies on the enamel surface of the experimental group is obviously reduced, and the number of dead bacteria is obviously increased compared with the control group. The washing product can obviously destroy the biomembrane of the streptococcus mutans, and the washing product has obvious inhibiting effect on the streptococcus mutans.
In addition, taking the houttuynia cordata extract, the green tea extract and the tea polyphenol (more than or equal to 98 percent) as examples, different houttuynia cordata extract washing products are prepared according to the production line and the method, and the influence on the growth of streptococcus mutans is studied, wherein the method comprises the following experimental steps:
each well of a 96-well plate ensures that the final concentration of 100 mu L is 10 5 ～10 6 CFU/mL bacterial solution and houttuynia cordata extract washing products with different concentrations are subjected to anaerobic condition culture for 24 hours, then diluted according to a certain proportion, 5 mu L of the diluted solution is dropwise applied to a solid culture medium, and the antibacterial efficacy of the houttuynia cordata extract washing products is inspected after the anaerobic condition culture for 24 hours, and the results are shown in figures 8A to 8B. The washing products respectively obtained from 5mg/mL houttuynia cordata extract, 5mg/mL green tea extract, 1mg/mL houttuynia cordata extract and 1mg/mL tea polyphenol show significant bacteriostatic action on the growth of streptococcus mutans (A in figure 8), and the inhibition rate is close to 100% (B in figure 8).
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and any simple modifications, alterations, modifications and equivalent structural changes made to the above embodiment according to the technical spirit of the present invention still fall within the protection scope of the technical solution of the present invention.
Claims (13)
1. The houttuynia cordata washing product for preventing caries and inhibiting bacteria is characterized in that the effective components of the washing product comprise a component A and a component B, wherein:
the component A is herba Houttuyniae extract or its derivative, which contains one or more of herba Houttuyniae extract, herba Houttuyniae oil, houttuynin, sodium houttuynin, and sodium new houttuynin; wherein,
herba Houttuyniae oil, houttuynin, sodium houttuyfonate, sodium new houttuyfonate, etc. with poor water solubility, and is represented as a type A herba Houttuyniae extract or its derivatives;
houttuynia cordata extract or the like having good water solubility is represented as a type b houttuynia cordata extract or a derivative thereof;
and when the component A is used for preparing the washing product, the houttuynia cordata extract or the derivative thereof in the category a is dissolved by absolute ethyl alcohol, and the houttuynia cordata extract in the category b or the derivative thereof in the category b is dissolved by 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 A to B is that the washing product has antibacterial efficacy, color and taste.
2. The houttuynia cordata washing product for preventing caries and inhibiting bacteria according to claim 1, wherein: preferably, the first and second liquid crystal materials are,
the washing product also comprises a proper amount of auxiliary materials, and the auxiliary materials comprise: one or more of a humectant, a preservative, an antioxidant, an emulsifier, a thickener, a sweetener, a mucilage, an aromatic and a flavoring agent.
3. A production line for producing a houttuynia cordata washing product for caries prevention and bacteria inhibition 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 bucket (9), a second drying device (18) and a freezing device (19), wherein:
the placing barrel (9) and the second drying device (18) and the refrigerating 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 pipeline connecting the first container (1) and the first stirring barrel (101) is connected with a liquid flowmeter (102);
a feed pipe (12) and a hopper (13) are communicated with two sides of the top end of the first stirring barrel (101), and a feed inlet formed in the top end of the third container (3) is respectively connected with discharge outlets at the bottom ends of the first container (1) and the second container (2) through a connecting pipeline (11);
a discharge hole of the third container (3) is connected with a feed hole 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 hole in the top end of the second stirring barrel (4) through a connecting pipe;
a first drying device (7) is placed on one side of a second stirring barrel (4), 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), and a discharge port of the fifth container (17) is communicated with a dialysis bag (23) placed in a placing barrel (9) through a connecting pipeline (11).
4. The production line of claim 3, wherein:
the production line further comprises a shredding device (20); the freezing device (19) is communicated with the crushing device (20) through a pipeline.
5. The production line of claim 3, wherein:
it has a plurality ofly and be one row of setting to place bucket (9), and the quantity of dialysis bag (23) is unanimous with placing bucket (9), and the export of a dialysis bag (23) and the import of another dialysis bag (23) all are linked together through connecting tube (11), and the feed inlet of last dialysis bag (23) discharge gate and second drying device (18) is linked together through connecting tube (11).
6. The production line of claim 3, wherein:
and the third container (3), the second stirring barrel (4) and the fifth container (17) are respectively placed at the tops of the third magnetic stirring device (16), the first magnetic stirring device (5) and the second magnetic stirring device (6).
7. The production line according to claim 3, characterized in that:
and power stirring devices (14) are arranged in the first stirring barrel (101), the fourth container (401) and the first drying device (7).
8. The production line according to claim 3, characterized in that: the pipeline of the connecting pipeline (11) is connected with an electromagnetic valve and a water pump.
9. The production line of claim 4, wherein:
and a first discharge valve (21) and a second discharge valve (22) are respectively connected to pipelines connected between the second drying device (18) and the freezing device (19) and between the freezing device (19) and the crushing device (20).
10. The production line according to claim 3, characterized in that: 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 support frame (15).
11. A method of producing the toiletry product according to the production line of any of claims 3 to 10, characterized in that it comprises the following steps:
(1) Dissolving the houttuynia cordata extract or the derivative thereof in deionized water or absolute ethyl alcohol to prepare a solution of the houttuynia cordata extract or the derivative thereof in the first container, wherein the type a houttuynia cordata extract or the derivative thereof is dissolved in the absolute ethyl alcohol, and the type b houttuynia cordata extract or the derivative thereof is dissolved in the deionized water;
(2) In the second container, cyclodextrin or a derivative thereof is dissolved in water to prepare a cyclodextrin solution with the concentration of 10-500 mg/mL; adjusting the volume of the cyclodextrin solution to be 9-11 times of the volume of the houttuynia cordata extract or derivative solution thereof through the liquid flow meter, simultaneously opening a detection tube arranged on a first stirring barrel on a second container, and checking that the concentration of the cyclodextrin solution is 10-500 mg/mL; for the extract of the houttuynia cordata or the derivative thereof, cyclodextrin or the derivative thereof is adopted for inclusion; for the extract of the houttuynia cordata or the derivative thereof, the extract of the houttuynia cordata b does not need to be included by cyclodextrin or the derivative thereof;
(3) In the third container, mixing a solution of the extract of the houttuynia cordata class a or the derivative thereof with a cyclodextrin solution 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 with the first mixed solution again to form a second mixed solution;
(6) Clathrating the extract or derivative of herba Houttuyniae a with cyclodextrin or its derivative, and removing all solvents in the second mixture in the fourth container to obtain first product; for the b-type houttuynia cordata extract or the derivative thereof, all solvents of the second mixed solution in the fourth container do not need to be removed, and a first product is obtained;
(7) Dissolving the first product of the extract of the houttuynia cordata or the derivative of the extract of the houttuynia cordata in the fifth container by pure water, and sequentially adding a proper amount of auxiliary materials such as a humectant, a preservative, an antioxidant, an emulsifier, a thickener, a sweetening agent, a mucilage, an aromatic, a flavoring agent and the like to obtain a second product; adding appropriate amount of humectant, antiseptic, antioxidant, emulsifier, thickener, sweetener, mucilage, aromatic and correctant into the second mixed solution to obtain second product;
(8) Transferring said second product liquid to a dialysis bag and dialyzing against 100 volumes of purified water at room temperature for a plurality of times to remove free houttuynia cordata extract or derivatives thereof to obtain a mouthwash product in the form of a mouthwash;
(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 steps of:
(10) The washing product in the form of washing particles is further comminuted by the comminuting device according to the product particle size requirement.
13. A houttuynia cordata gargle product for caries prevention and bacteria inhibition according to claim 1 or 2, wherein:
the washing product is washing particles dissolved in water, or dentifrice, tooth gel or oral spray.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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 |
| CN202310305414.4A CN116421515A (en) | 2022-10-09 | 2023-03-27 | Houttuynia cordata washing product for caries prevention and bacteriostasis and production line thereof |
| CN202310308640.8A CN116531442A (en) | 2022-10-09 | 2023-03-27 | Houttuynia cordata green tea composition with caries preventing and antibacterial activity and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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 |
|---|---|
| CN115444799A true CN115444799A (en) | 2022-12-09 |
Family
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 After (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| 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 |
Country Status (1)
| Country | Link |
|---|---|
| CN (3) | CN115444799A (en) |
-
2022
- 2022-10-09 CN CN202211232878.9A patent/CN115444799A/en not_active Withdrawn
-
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 |
|---|---|
| CN116421515A (en) | 2023-07-14 |
| CN116531442A (en) | 2023-08-04 |
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Application publication date: 20221209 |