CN115813805A - Novel oral cavity and tooth cleaning agent and preparation method thereof - Google Patents
Novel oral cavity and tooth cleaning agent and preparation method thereof Download PDFInfo
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- CN115813805A CN115813805A CN202211488763.6A CN202211488763A CN115813805A CN 115813805 A CN115813805 A CN 115813805A CN 202211488763 A CN202211488763 A CN 202211488763A CN 115813805 A CN115813805 A CN 115813805A
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- phase change
- cleaning agent
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- 210000000214 mouth Anatomy 0.000 title claims abstract description 67
- 239000012459 cleaning agent Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims description 37
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 85
- 230000008859 change Effects 0.000 claims abstract description 65
- 238000006243 chemical reaction Methods 0.000 claims abstract description 53
- 239000011159 matrix material Substances 0.000 claims abstract description 35
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 31
- CDMADVZSLOHIFP-UHFFFAOYSA-N disodium;3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane;decahydrate Chemical compound O.O.O.O.O.O.O.O.O.O.[Na+].[Na+].O1B([O-])OB2OB([O-])OB1O2 CDMADVZSLOHIFP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 31
- 239000011734 sodium Substances 0.000 claims abstract description 31
- 239000000022 bacteriostatic agent Substances 0.000 claims abstract description 23
- 239000004014 plasticizer Substances 0.000 claims abstract description 23
- 239000002904 solvent Substances 0.000 claims abstract description 8
- 239000000126 substance Substances 0.000 claims abstract description 3
- 239000012071 phase Substances 0.000 claims description 62
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 54
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 54
- 238000004140 cleaning Methods 0.000 claims description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 36
- NOOLISFMXDJSKH-UTLUCORTSA-N (+)-Neomenthol Chemical group CC(C)[C@@H]1CC[C@@H](C)C[C@@H]1O NOOLISFMXDJSKH-UTLUCORTSA-N 0.000 claims description 18
- NOOLISFMXDJSKH-UHFFFAOYSA-N DL-menthol Natural products CC(C)C1CCC(C)CC1O NOOLISFMXDJSKH-UHFFFAOYSA-N 0.000 claims description 18
- DOOTYTYQINUNNV-UHFFFAOYSA-N Triethyl citrate Chemical compound CCOC(=O)CC(O)(C(=O)OCC)CC(=O)OCC DOOTYTYQINUNNV-UHFFFAOYSA-N 0.000 claims description 18
- 229960001927 cetylpyridinium chloride Drugs 0.000 claims description 18
- YMKDRGPMQRFJGP-UHFFFAOYSA-M cetylpyridinium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+]1=CC=CC=C1 YMKDRGPMQRFJGP-UHFFFAOYSA-M 0.000 claims description 18
- 229940041616 menthol Drugs 0.000 claims description 18
- 239000001069 triethyl citrate Substances 0.000 claims description 18
- VMYFZRTXGLUXMZ-UHFFFAOYSA-N triethyl citrate Natural products CCOC(=O)C(O)(C(=O)OCC)C(=O)OCC VMYFZRTXGLUXMZ-UHFFFAOYSA-N 0.000 claims description 18
- 235000013769 triethyl citrate Nutrition 0.000 claims description 18
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 230000001131 transforming effect Effects 0.000 claims description 6
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 5
- 239000007791 liquid phase Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims description 2
- CHHHXKFHOYLYRE-UHFFFAOYSA-M 2,4-Hexadienoic acid, potassium salt (1:1), (2E,4E)- Chemical compound [K+].CC=CC=CC([O-])=O CHHHXKFHOYLYRE-UHFFFAOYSA-M 0.000 claims description 2
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 2
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 2
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims description 2
- 235000015165 citric acid Nutrition 0.000 claims description 2
- 239000001630 malic acid Substances 0.000 claims description 2
- 235000011090 malic acid Nutrition 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 239000004302 potassium sorbate Substances 0.000 claims description 2
- 235000010241 potassium sorbate Nutrition 0.000 claims description 2
- 229940069338 potassium sorbate Drugs 0.000 claims description 2
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 claims description 2
- 239000004299 sodium benzoate Substances 0.000 claims description 2
- 235000010234 sodium benzoate Nutrition 0.000 claims description 2
- 229960003885 sodium benzoate Drugs 0.000 claims description 2
- 239000011975 tartaric acid Substances 0.000 claims description 2
- 235000002906 tartaric acid Nutrition 0.000 claims description 2
- 235000011187 glycerol Nutrition 0.000 claims 1
- 239000007788 liquid Substances 0.000 abstract description 28
- 238000003756 stirring Methods 0.000 description 75
- 239000000243 solution Substances 0.000 description 66
- 239000000203 mixture Substances 0.000 description 51
- 238000009472 formulation Methods 0.000 description 33
- 239000008213 purified water Substances 0.000 description 30
- 230000000052 comparative effect Effects 0.000 description 27
- 239000004372 Polyvinyl alcohol Substances 0.000 description 18
- 229920002451 polyvinyl alcohol Polymers 0.000 description 18
- 235000010339 sodium tetraborate Nutrition 0.000 description 17
- 238000004519 manufacturing process Methods 0.000 description 15
- 239000000499 gel Substances 0.000 description 8
- 241000628997 Flos Species 0.000 description 6
- 230000001680 brushing effect Effects 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 229920002472 Starch Polymers 0.000 description 5
- 239000003599 detergent Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000003292 glue Substances 0.000 description 5
- 235000019698 starch Nutrition 0.000 description 5
- 239000008107 starch Substances 0.000 description 5
- 229920003023 plastic Polymers 0.000 description 4
- 239000004033 plastic Substances 0.000 description 4
- 239000002324 mouth wash Substances 0.000 description 3
- 229940051866 mouthwash Drugs 0.000 description 3
- 239000000606 toothpaste Substances 0.000 description 3
- 229920000742 Cotton Polymers 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000010794 food waste Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000004088 simulation Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 229940034610 toothpaste Drugs 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 208000006558 Dental Calculus Diseases 0.000 description 1
- 206010044029 Tooth deposit Diseases 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 229940112822 chewing gum Drugs 0.000 description 1
- 235000015218 chewing gum Nutrition 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 239000009322 erkang Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000003239 periodontal effect Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000011505 plaster Substances 0.000 description 1
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- 238000011160 research Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000012056 semi-solid material Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
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- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Abstract
The invention provides a novel oral tooth cleaning agent, which comprises an oral cleaning agent and a phase change conversion agent; wherein the oral cavity cleanser comprises a gel-forming matrix, a freshener, a bacteriostatic agent, a plasticizer, a first pH value regulator and a solvent; the pH value of the oral cavity cleanser is less than 7.0 and more than or equal to 5.1; the phase change conversion agent comprises the following components in a mass ratio of 1:2 to 1.5:1, sodium metaaluminate, sodium borate decahydrate, a second pH value regulator and a solvent, wherein the pH value of the phase change conversion agent is more than 7.0 and less than or equal to 8.9; the mass of the gel-forming matrix accounts for 74-88% of the total mass of dry substances in the oral cavity cleaning agent, and the ratio of the mass of the gel-forming matrix to the total mass of sodium metaaluminate and sodium borate decahydrate is 60-140. The oral cavity tooth cleaning agent prepared by the invention is deeply infiltrated by liquid, then is transformed into a viscoelastic body through phase change, can wrap the surfaces of teeth, slits of teeth, cavities of teeth and the like without difference, and then is taken out to ensure that the oral cavity is deeply cleaned without residue.
Description
Technical Field
The invention belongs to the field of oral cleaning, and particularly relates to a novel oral tooth cleaning agent and a preparation method thereof.
Background
The oral cavity problem is a problem which is easy to neglect, the oral cavity cleaning is the first barrier for preventing the oral cavity problem, the mainstream oral cavity cleaning products in the market at present mainly comprise toothbrushes, toothpaste, dental floss, tooth pastes, tooth powders, mouthwash, chewing gum and the like, and the products need to be matched for use from the aspects of cleaning tooth surfaces, cleaning tooth gaps, cleaning the oral cavity and the like, and various cleaning modes have certain limitation and are not deep enough for cleaning.
Tooth brushing is the most common basic oral cavity cleaning mode, the tooth brushing method, the tooth brushing force, the tooth brushing frequency and the like all affect the cleaning effect, the tooth brushing method cannot achieve the cleaning effect, teeth still have yellow color and dental calculus even decay for a long time, and the tooth brushing force is too large and too frequent, and the enamel can be damaged, so that the teeth are sensitive. The dental floss is a classic product for cleaning gaps between teeth, food residues which cannot be brushed are found again after teeth are brushed and then the gaps between the teeth are cleaned many times, but the dental floss still has limitation in use, the gaps between the teeth measured in the oral cavity are inconvenient to use, and the gaps between the teeth and the gums are damaged due to improper use. The mouthwash is also a classic product for cleaning oral cavity, has certain effects on oral cavity sterilization, residue cleaning, breath freshening and the like, but cannot deeply clean teeth and slits between teeth, can cause imbalance of oral flora after long-term use, and can cause taste sense weakness of oral cavity due to a large amount of essence, ethanol and the like.
Therefore, the oral cleaning product which is convenient to use, has pure physical effect and can deeply clean the oral cavity, the tooth surface and the slit between the teeth has great market space and competitiveness.
Disclosure of Invention
The main object of the present invention is to design a product for oral cavity cleaning, which is different from toothpaste, dental floss, and mouthwash, and has the function of cleaning the oral cavity, tooth surface, crevices, and even cavities, so that the product must be in a liquid state before and during cleaning the oral cavity to ensure deep contact, and the final cleaning step must be in a viscoelastic solid state to ensure complete removal of the liquid-wrapped dirt, residue, and even bacteria.
In order to achieve the above purpose, a formula with liquid-solid two-phase transformation potential needs to be designed creatively. Through screening and research, polyvinyl alcohol is adopted to form a gel matrix material, the gel matrix material is prepared into an aqueous solution, and the polyvinyl alcohol has the potential of becoming a solid or semisolid material after being crosslinked.
It is another object of the present invention to achieve a change in the mouth cleaning solution from a liquid phase to a viscoelastic solid in a short period of time. Therefore, a unique phase change curing agent needs to be found. The inventive use of sodium metaaluminate and sodium borate decahydrate as the phase change composition for the above purpose has the ability to achieve rapid conversion of liquid in the oral cavity to semisolid or solid, and the elasticity of viscoelastic body after solidification is controlled by pH, and the conversion speed is controlled by the amount of phase change conversion agent.
A novel oral tooth cleaning agent comprises oral cavity cleaning agent and phase transition conversion agent; wherein the oral cavity cleanser comprises a gel-forming matrix, a freshener, a bacteriostatic agent, a plasticizer, a first pH value regulator and a solvent; the pH value of the oral cavity cleanser is less than 7.0 and more than or equal to 5.1;
the phase change conversion agent comprises the following components in a mass ratio of 1:2 to 1.5:1, sodium metaaluminate, sodium borate decahydrate, a second pH value regulator and a solvent, wherein the pH value of the phase change conversion agent is more than 7.0 and less than or equal to 8.9;
the mass of the gel-forming matrix accounts for 74-88% of the total mass of dry substances in the oral cavity cleaning agent, and the ratio of the mass of the gel-forming matrix to the total mass of sodium metaaluminate and sodium borate decahydrate is 60:1-166:1.
further, the mass ratio of the oral cavity cleaning agent to the phase change conversion agent is 8.7.
Further, the mass ratio of sodium metaaluminate to sodium borate decahydrate is 1:2 to 1:1.
still further, the second pH regulator is selected from at least one of citric acid, tartaric acid and malic acid; and/or, the first pH regulator is selected from sodium hydroxide and/or potassium hydroxide; and/or the solvent in the oral cavity cleaning agent and the phase change conversion agent is water.
Further, the plasticizer is at least one of triethyl citrate, glycerol and polyethylene glycol; preferably, the mass ratio of the gel-forming matrix to the plasticizer is 3.
Further, the freshener is menthol; preferably, the oral cavity cleanser contains 0.02 to 0.03 weight percent of freshener.
Further, the bacteriostatic agent is selected from at least one of cetylpyridinium chloride, potassium sorbate and sodium benzoate; preferably, the oral cavity cleanser contains 0.03 to 0.05 weight percent of bacteriostatic agent.
Further, the total content of sodium metaaluminate and sodium borate decahydrate in the phase change conversion agent is 1.5-2.5wt%.
Further, an oral cavity cleaning agent and a phase change conversion agent are included; wherein the oral cleanser comprises 6-14 parts by weight of gel-forming matrix, 0.016 part by weight of freshener, 0.025 part by weight of bacteriostatic agent, 20 parts by weight of plasticizer and 50 parts by weight of water, and the oral cleanser further comprises a first pH regulator, wherein the first pH regulator regulates the pH value of the oral cleanser to be less than 7.0 and greater than or equal to 5.1; the phase change conversion agent comprises 0.024-0.06 parts by weight of sodium metaaluminate, 0.036-0.084 parts by weight of sodium tetraborate decahydrate and 3-7 parts by weight of water, and further comprises a second pH value regulator, wherein the second pH value regulator regulates the pH value of the phase change conversion agent to be more than 7.0 and less than or equal to 8.9; the ratio of the mass of the gel-forming matrix to the total mass of the sodium metaaluminate and the sodium borate decahydrate is 60-166.
Further, the preparation method of the novel oral tooth cleaning agent comprises the following steps: and respectively mixing the components of the oral cavity cleaning agent and the phase-change transforming agent to prepare the oral cavity cleaning agent and the phase-change transforming agent.
Furthermore, the novel oral cavity tooth cleaning agent prepared by the preparation method is used for cleaning teeth, before use, the oral cavity cleaning agent and the phase change conversion agent are mixed and are put into the mouth to be contacted with the teeth, and the novel oral cavity tooth cleaning agent is converted into an elastomer from a liquid phase and is taken out.
Furthermore, the oral cavity cleaning agent and the phase change conversion agent are mixed and then start to be solidified, and the cleaning glue formed after solidification has the tensile strength of 0.5-1.0 MPa and the elongation at break of 120-200%.
The invention has the following advantages:
1. the novel oral tooth cleaning agent provided by the invention comprises an oral cleaning agent and a phase change conversion agent, and a unique phase change conversion mechanism of the novel oral tooth cleaning agent utilizesThe composition of sodium metaaluminate and sodium borate decahydrate in a certain proportion is used as a phase change transforming agent of a gel-forming matrix, and the mass ratio of the gel-forming matrix to the phase change transforming agent is regulated and controlled 、 The content of the gel-forming matrix in the dry matter of the oral cavity cleanser and the pH values of the oral cavity cleanser and the phase change conversion agent are controlled within a proper range through the first pH value regulator and the second pH value regulator, so that liquid-solid conversion rapidly occurs to form a viscoelastic body.
2. According to the novel oral tooth cleaning agent provided by the invention, the mass ratio of the oral cleaning agent to the phase change conversion agent is controlled to be 8.7; controlling the mass ratio of sodium metaaluminate to sodium borate decahydrate to be 1:2 to 1:1, the novel solidified oral tooth cleaning agent has moderate tensile force and is more convenient to use.
3. The mouth cavity cleaning agent is convenient to use, and only needs to be poured into a measuring cup before the teeth in the mouth cavity are cleaned, then a fixed amount of the phase change conversion agent is dripped, the mouth cavity cleaning agent is simply shaken uniformly and is fed into the mouth, the mouth cavity cleaning agent is quickly gargled to infiltrate the teeth, the teeth are immersed in the mouth cavity, the teeth are submerged for about 30-45 s, the teeth are converted into a semi-solid viscoelastic body, and then the teeth are taken out.
4. The preparation method is simple in preparation process, can be prepared according to the prescription amount of the liquid preparation, and is particularly suitable for large-scale production and preparation.
Detailed Description
Example 1
Prescription:
the production process comprises the following steps:
1. preparation of oral liquid cleanser
Firstly, adding a first pH regulator citric acid into purified water, and fully stirring for dissolving. Adding bacteriostatic agent cetylpyridinium chloride, plasticizer triethyl citrate and refreshing agent menthol into the solution respectively, stirring for dissolving, finally adding colloid-forming matrix polyvinyl alcohol, and fully stirring for dissolving. The formulation solution actual pH =5.6.
2. Preparation of phase change conversion agent
Firstly, adding sodium hydroxide as a second pH regulator into purified water, fully stirring and dissolving, then adding a phase change agent composition sodium metaaluminate and sodium tetraborate decahydrate into the solution, and fully stirring and dissolving. The formulation solution actual pH =8.4.
Example 2
Prescription:
the production process comprises the following steps:
1. preparation of oral liquid cleanser
Firstly, adding a first pH regulator citric acid into purified water, and fully stirring for dissolving. Adding bacteriostatic agent cetylpyridinium chloride, plasticizer triethyl citrate and refreshing agent menthol into the solution respectively, stirring for dissolving, finally adding colloid-forming matrix polyvinyl alcohol, and fully stirring for dissolving. The formulation solution actual pH =5.1.
2. Preparation of phase change conversion agent
Firstly, adding sodium hydroxide as a second pH regulator into purified water, fully stirring and dissolving, then adding a phase change agent composition sodium metaaluminate and sodium tetraborate decahydrate into the solution, and fully stirring and dissolving. The formulation solution actual pH =7.7.
Example 3
Prescription:
the production process comprises the following steps:
1. preparation of oral liquid cleanser
Firstly, adding a first pH regulator citric acid into purified water, and fully stirring for dissolving. Adding bacteriostatic agent cetylpyridinium chloride, plasticizer triethyl citrate and refreshing agent menthol into the solution respectively, stirring for dissolving, finally adding colloid-forming matrix polyvinyl alcohol, and fully stirring for dissolving. The formulation solution actual pH =5.7.
2. Preparation of phase change conversion agent
Firstly, adding sodium hydroxide as a second pH regulator into purified water, fully stirring and dissolving, then adding a phase change agent composition sodium metaaluminate and sodium tetraborate decahydrate into the solution, and fully stirring and dissolving. The formulation solution actual pH =8.9.
Example 4
Prescription:
the production process comprises the following steps:
1. preparation of oral liquid cleanser
First, adding citric acid as a first pH regulator into purified water, and fully stirring for dissolving. And then respectively adding bacteriostatic agent cetylpyridinium chloride, plasticizer triethyl citrate and refreshing agent menthol into the solution, stirring and dissolving, finally adding gelling matrix polyvinyl alcohol, and fully stirring and dissolving. The formulation solution actual pH =5.6.
2. Preparation of phase change conversion agent
Firstly, adding sodium hydroxide as a second pH regulator into purified water, fully stirring and dissolving, then adding a phase change agent composition sodium metaaluminate and sodium tetraborate decahydrate into the solution, and fully stirring and dissolving. The formulation solution actual pH =8.4.
Example 5
Prescription:
the production process comprises the following steps:
1. preparation of oral liquid cleanser
Firstly, adding a first pH regulator citric acid into purified water, and fully stirring for dissolving. Adding bacteriostatic agent cetylpyridinium chloride, plasticizer triethyl citrate and refreshing agent menthol into the solution respectively, stirring for dissolving, finally adding colloid-forming matrix polyvinyl alcohol, and fully stirring for dissolving. The formulation solution actual pH =5.6.
2. Preparation of phase change conversion agent
Firstly, adding sodium hydroxide as a second pH regulator into purified water, fully stirring and dissolving, then adding a phase change agent composition sodium metaaluminate and sodium tetraborate decahydrate into the solution, and fully stirring and dissolving. The formulation solution actual pH =8.4.
Example 6
Prescription:
the production process comprises the following steps:
1. preparation of oral liquid cleanser
Firstly, adding a first pH regulator citric acid into purified water, and fully stirring for dissolving. Adding bacteriostatic agent cetylpyridinium chloride, plasticizer triethyl citrate and refreshing agent menthol into the solution respectively, stirring for dissolving, finally adding colloid-forming matrix polyvinyl alcohol, and fully stirring for dissolving. The formulation solution actual pH =5.8.
2. Preparation of phase change conversion agent
Firstly, adding sodium hydroxide as a second pH regulator into purified water, fully stirring and dissolving, then adding a phase change agent composition sodium metaaluminate and sodium tetraborate decahydrate into the solution, and fully stirring and dissolving. The formulation solution actual pH =8.3.
Example 7
Prescription:
the production process comprises the following steps:
1. preparation of oral liquid cleanser
Firstly, adding a first pH regulator citric acid into purified water, and fully stirring for dissolving. Adding bacteriostatic agent cetylpyridinium chloride, plasticizer triethyl citrate and refreshing agent menthol into the solution respectively, stirring for dissolving, finally adding colloid-forming matrix polyvinyl alcohol, and fully stirring for dissolving. The formulation solution actual pH =5.5.
2. Preparation of phase change conversion agent
Firstly, adding sodium hydroxide serving as a second pH regulator into purified water, fully stirring and dissolving, then adding a phase change agent composition sodium metaaluminate and sodium tetraborate decahydrate into the solution, and fully stirring and dissolving. The formulation solution actual pH =8.9.
Example 8
Prescription:
the production process comprises the following steps:
1. preparation of oral liquid cleanser
Firstly, adding a first pH regulator citric acid into purified water, and fully stirring for dissolving. Adding bacteriostatic agent cetylpyridinium chloride, plasticizer triethyl citrate and refreshing agent menthol into the solution respectively, stirring for dissolving, finally adding colloid-forming matrix polyvinyl alcohol, and fully stirring for dissolving. The formulation solution actual pH =5.6.
2. Preparation of phase change conversion agent
Firstly, adding sodium hydroxide as a second pH regulator into purified water, fully stirring and dissolving, then adding a phase change agent composition sodium metaaluminate and sodium tetraborate decahydrate into the solution, and fully stirring and dissolving. The formulation solution actual pH =7.3.
Comparative example 1
Prescription:
the production process comprises the following steps:
1. oral liquid cleanser formulation
Firstly, adding a first pH regulator citric acid into purified water, and fully stirring for dissolving. Adding bacteriostatic agent cetylpyridinium chloride, plasticizer triethyl citrate and refreshing agent menthol into the solution respectively, stirring for dissolving, finally adding colloid-forming matrix polyvinyl alcohol, and fully stirring for dissolving. The formulation solution actual pH =5.6.
2. Preparation of phase change conversion agent
Firstly, adding sodium hydroxide as a second pH regulator into purified water, fully stirring and dissolving, then adding sodium metaaluminate as a phase change agent into the solution, and fully stirring and dissolving. The formulation solution actual pH =8.4.
Comparative example 2
Prescription:
the production process comprises the following steps:
1. preparation of oral liquid cleanser
Firstly, adding a first pH regulator citric acid into purified water, and fully stirring for dissolving. And then respectively adding bacteriostatic agent cetylpyridinium chloride, plasticizer triethyl citrate and refreshing agent menthol into the solution, stirring and dissolving, finally adding gelling matrix polyvinyl alcohol, and fully stirring and dissolving. The formulation solution actual pH =5.3.
2. Preparation of phase change conversion agent
Firstly, adding sodium hydroxide serving as a second pH regulator into purified water, fully stirring and dissolving, then adding sodium tetraborate decahydrate serving as a phase change agent into the solution, and fully stirring and dissolving. The formulation solution actual pH =8.2.
Comparative example 3
Prescription:
the production process comprises the following steps:
1. oral liquid cleanser formulation
Firstly, adding a first pH regulator citric acid into purified water, and fully stirring for dissolving. Adding bacteriostatic agent cetylpyridinium chloride, plasticizer triethyl citrate and refreshing agent menthol into the solution respectively, stirring for dissolving, finally adding colloid-forming matrix polyvinyl alcohol, and fully stirring for dissolving. The formulation solution actual pH =5.5.
2. Preparation of phase change conversion agent
Firstly, adding sodium hydroxide as a second pH regulator into purified water, fully stirring and dissolving, then adding a phase change agent composition sodium metaaluminate and sodium tetraborate decahydrate into the solution, and fully stirring and dissolving. The formulation solution actual pH =8.6.
Comparative example 4
Prescription:
the production process comprises the following steps:
1. preparation of oral liquid cleanser
Firstly, adding a first pH regulator citric acid into purified water, and fully stirring for dissolving. Adding cetylpyridinium chloride as bacteriostatic agent, triethyl citrate as plasticizer and menthol as freshener into the solution, stirring for dissolving, adding polyvinyl alcohol as colloid matrix, and stirring for dissolving. The formulation solution actual pH =5.4.
2. Preparation of phase change conversion agent
Firstly, adding sodium hydroxide as a second pH regulator into purified water, fully stirring and dissolving, then adding a phase change agent composition sodium metaaluminate and sodium tetraborate decahydrate into the solution, and fully stirring and dissolving. The formulation solution actual pH =8.2.
Comparative example 5
Prescription:
the production process comprises the following steps:
1. preparation of oral liquid cleanser
Firstly, adding a first pH regulator citric acid into purified water, and fully stirring for dissolving. Adding bacteriostatic agent cetylpyridinium chloride, plasticizer triethyl citrate and refreshing agent menthol into the solution respectively, stirring for dissolving, finally adding colloid-forming matrix polyvinyl alcohol, and fully stirring for dissolving. The formulation solution actual pH =5.2.
2. Preparation of phase change conversion agent
Firstly, adding sodium hydroxide serving as a second pH regulator into purified water, fully stirring and dissolving, then adding a phase change agent composition sodium metaaluminate and sodium tetraborate decahydrate into the solution, and fully stirring and dissolving. The formulation solution actual pH =8.3.
Comparative example 6
Prescription:
the production process comprises the following steps:
1. preparation of oral liquid cleanser
Firstly, adding a first pH regulator citric acid into purified water, and fully stirring for dissolving. Adding bacteriostatic agent cetylpyridinium chloride, plasticizer triethyl citrate and refreshing agent menthol into the solution respectively, stirring for dissolving, finally adding colloid-forming matrix polyvinyl alcohol, and fully stirring for dissolving. The formulation solution actual pH =4.2.
2. Preparation of phase change conversion agent
Firstly, adding sodium hydroxide as a second pH regulator into purified water, fully stirring and dissolving, then adding a phase change agent composition sodium metaaluminate and sodium tetraborate decahydrate into the solution, and fully stirring and dissolving. The formulation solution actual pH =8.3.
Comparative example 7
Prescription:
the production process comprises the following steps:
1. oral liquid cleanser formulation
First, adding citric acid as a first pH regulator into purified water, and fully stirring for dissolving. Adding bacteriostatic agent cetylpyridinium chloride, plasticizer triethyl citrate and refreshing agent menthol into the solution respectively, stirring for dissolving, finally adding colloid-forming matrix polyvinyl alcohol, and fully stirring for dissolving. The formulation solution actual pH =5.5.
2. Preparation of phase change conversion agent
Firstly, adding sodium hydroxide as a second pH regulator into purified water, fully stirring and dissolving, then adding a phase change agent composition sodium metaaluminate and sodium tetraborate decahydrate into the solution, and fully stirring and dissolving. The formulation solution actual pH =9.5.
All the auxiliary materials used in the invention are from the following manufacturers:
the polyvinyl alcohol manufacturer is Hunan Erkang pharmaceutical Co., ltd; the menthol manufacturer is Anhui Huaxin Biotechnology Co., ltd; the cetylpyridinium chloride manufacturer is Wuxi Shanghai Jiehi chemical engineering Co., ltd; the triethyl citrate manufacturer is Anhuifeng Yuanshan pharmaceutical Co., ltd; the citric acid supplier is Shanghai Luo auxiliary medicine; the sodium metaaluminate manufacturer is Shanghai Michelin Biochemical technology, inc.; sodium tetraborate decahydrate was Shanghai Michelin Biochemical technology, inc.; the sodium hydroxide manufacturer is Chengdu Hua Yi pharmaceutical Co.
Experimental example 1
The novel oral tooth cleaners prepared in examples and comparative examples were used to simulate cleaning of teeth using an oral tooth plaster model, all of which were identical (28 teeth up and down), using a total of 75 models divided into 15 groups of 5 models each. Each model is firstly filled with 26 slits of teeth by a thin cotton rope, redundant cotton ropes are subtracted, food residues in the slits of teeth are simulated, starch slurry (the concentration of the starch slurry is 60%) is coated on the surface of each model to simulate surface tooth stains after eating, the coating dosage of each set of the model is 20g, and the model is cleaned by using the cleaning agent provided by the embodiment and the comparative example of the invention, and the specific method comprises the following steps: putting each tooth model in a plastic bag, then dropping a corresponding phase change conversion agent into an oral liquid detergent solution, pouring the oral liquid detergent solution into the plastic bag, shaking the plastic bag gently for 10s to mix uniformly, ensuring that the detergent solution soaks the tooth model in the plastic bag, simulating the process of oral cavity gargling, taking out the oral liquid detergent solution after 5min after the detergent is solidified, measuring the number of the residual dental floss lines and the starch content in the tooth model (soaking the cleaned tooth model in 1L of water for 30 min, and detecting the starch content in the water), and obtaining the average dental floss line number and the residual starch content on the surface of the tooth of each group of tooth models, as shown in the following table.
According to the results of the oral cavity cleaning simulation test, the groups 1 to 8 adopt the novel oral cavity tooth cleaning agent of the embodiments 1 to 7, and the cleaning effect of the oral cavity simulation cleaning on the tooth surface and the tooth gaps is better, especially the groups 1 to 7, wherein the groups 1 to 5 and 7 have the advantages that the cleaning glue after the novel oral cavity tooth cleaning agent is solidified is easy to take out, and no fracture and no residue are left. Group 6 had no fracture and no residue, but the removal thereof was laborious. The 9 th group and the 15 th group respectively adopt the cleaning glue obtained by curing the novel oral tooth cleaning agent of the comparative examples 1 and 7, and the phenomena that the cured glue body has poor elasticity, is hard to pull and can be taken out after being broken occur. Groups 10-14 all experienced varying degrees of tensile failure, interdental or periodontal residue, affecting cleaning efficacy.
From the above experiments, it can be known that the proportion and the amount of the phase-change conversion composition, the amount of the gel-forming matrix, and the suitable pH values of the cleaning agent and the phase-change conversion composition should be controlled for the viscoelastic body with better deep cleaning effect. The phase change agent sodium metaaluminate or sodium tetraborate decahydrate which are used independently cannot ensure better viscoelasticity and toughness and cannot deeply clean the oral cavity.
Experimental example 2
And (3) testing the curing time, pouring the oral cavity cleaning agent prepared in the embodiment and the comparative example into a beaker by adopting the using method of the product, pouring the corresponding phase-change conversion agent into the beaker, slightly shaking for 10s, uniformly mixing, starting timing until no liquid shakes in the beaker, namely all the liquid is converted into a gel state, recording the time for completely curing the liquid, and stopping observation after the gel volume of some samples is not increased after the samples are cured for a certain time and the samples cannot be completely cured within 5 min.
| Test examples | Curing time | Whether or not it can be completely cured |
| Example 1 | 36s | Is that |
| Example 2 | 45s | Is that |
| Example 3 | 39s | Is that |
| Example 4 | 32s | Is that |
| Example 5 | 44s | Is that |
| Example 6 | 30s | Is that |
| Example 7 | 19s | Is that |
| Example 8 | 171s | Whether or not |
| Comparative example 2 | 290s | Is that |
| Comparative example 4 | —— | Whether or not |
| Comparative example 6 | 320s | Is that |
| Comparative example 7 | 8s | Is that |
According to the test of the sample curing time, the curing time of the samples 1-6 is between 30s and 45s, the oral use is suitable, and no liquid is layered. The tooth cleaning agent of the comparative example 4 can not be completely cured after 5min, and has liquid residue, which is not convenient for quick use in oral cavity, and shows that the curing speed and the curing degree are affected when the dosage of the gel-forming matrix is low, the dosage of the special phase-change conversion agent is low, and the pH of the cleaning solution is low. In comparative example 7, the curing time is too short, which easily causes the curing to start before entering the oral cavity, and the curing speed is also affected when the dosage of the special phase-change conversion agent is higher and the special phase-change conversion agent is more alkaline.
Experimental example 3
After the oral liquid cleanser and the phase change conversion agent prepared in each example and comparative example are uniformly mixed by gentle shaking for 10s, the mixture is stood at room temperature for 5min, and then each group of completely cured or partially cured gel is tested for tensile strength and elongation at break, wherein the test for the tensile strength and the elongation at break refers to the national standard GB/T528-2009.
| Test examples | Tensile strength MPa | Elongation at break% |
| Example 1 | 0.6721 | 161.2 |
| Example 2 | 0.6010 | 177.8 |
| Example 3 | 0.8722 | 152.5 |
| Example 4 | 0.7219 | 149.0 |
| Example 5 | 0.6610 | 158.1 |
| Example 6 | 1.0811 | 212.0 |
| Example 7 | 0.8122 | 148.3 |
| Example 8 | 0.2045 | 83.9 |
| Comparative example 1 | 1.7855 | 90.4 |
| Comparative example 2 | 0.0591 | 102.5 |
| Comparative example 3 | 0.1374 | 54.7 |
| Comparative example 4 | 0.0276 | 17.9 |
| Comparative example 5 | 0.8302 | 41.5 |
| Comparative example 6 | 0.0087 | 5.3 |
| Comparative example 7 | 1.5230 | 72.9 |
The cleaning gels of the novel oral tooth cleaners of examples 1-5 and 7 after curing are easy to take out, have no effort in stretching, good viscoelasticity and no residue at break, and the tensile strength of the cleaning gels is between 0.5 and 1.0MPa and the elongation at break is between 120 and 200 percent.
The cleaning glue obtained by curing the novel oral tooth cleaning agents of comparative examples 1 and 7 has the problems of overlarge tensile strength and undersize elongation at break, and the strength and toughness can not meet the requirements. The cleaning gels of the novel oral tooth cleaners of comparative examples 2-6, after curing, also had a slightly lower elongation at break.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. This need not be, nor should it be exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (10)
1. A novel oral cavity and tooth cleaning agent is characterized by comprising an oral cavity cleaning agent and a phase change conversion agent; wherein the oral cavity cleanser comprises a gel-forming matrix, a freshener, a bacteriostatic agent, a plasticizer, a first pH value regulator and a solvent; the pH value of the oral cavity cleanser is less than 7.0 and more than or equal to 5.1;
the phase change conversion agent comprises the following components in a mass ratio of 1:2 to 1.5:1, sodium metaaluminate, sodium borate decahydrate, a second pH value regulator and a solvent, wherein the pH value of the phase change conversion agent is more than 7.0 and less than or equal to 8.9;
the mass of the gel-forming matrix accounts for 74-88% of the total mass of dry substances in the oral cavity cleaning agent, and the ratio of the mass of the gel-forming matrix to the total mass of sodium metaaluminate and sodium borate decahydrate is 60:1 to 166 ： 1。
2. The novel oral tooth cleaning agent as claimed in claim 1, wherein the mass ratio of the oral cleaning agent to the phase change conversion agent is 8.7.
3. The novel oral tooth cleaner as claimed in claim 1 or 2, wherein the mass ratio of sodium metaaluminate to sodium borate decahydrate is 1:2 to 1:1.
4. the novel oral tooth cleaner according to claim 1, wherein the second pH regulator is at least one selected from citric acid, tartaric acid and malic acid; and/or, the first pH regulator is selected from sodium hydroxide and/or potassium hydroxide; and/or the solvent in the oral cavity cleaning agent and the phase change conversion agent is water.
5. The novel oral tooth cleaner as claimed in claim 1, wherein the plasticizer is at least one of triethyl citrate, glycerin, and polyethylene glycol; preferably, the mass ratio of the gel-forming matrix to the plasticizer is 3.
6. A novel oral dental cleanser according to claim 1, wherein said refreshing agent is menthol; preferably, the oral cavity cleanser contains 0.02 to 0.03 weight percent of freshener.
7. The novel oral dental cleaning agent of claim 1, wherein the bacteriostatic agent is selected from at least one of cetylpyridinium chloride, potassium sorbate, sodium benzoate; preferably, the oral cavity cleanser contains 0.03 to 0.05 weight percent of bacteriostatic agent.
8. A novel oral tooth cleaner as claimed in any one of claims 1 to 3, wherein said phase change conversion agent contains sodium metaaluminate and sodium borate decahydrate in a total amount of 1.5 to 2.5% by weight.
9. A method for preparing a novel oral dental cleanser as claimed in any one of claims 1 to 8, comprising the steps of: and respectively mixing the components of the oral cavity cleaning agent and the phase-change transforming agent to prepare the oral cavity cleaning agent and the phase-change transforming agent.
10. Use of the novel oral tooth cleaner according to any one of claims 1 to 8 or the novel oral tooth cleaner prepared by the preparation method according to claim 9 for cleaning teeth, wherein the oral tooth cleaner and the phase change conversion agent are mixed before use, and are introduced into the mouth to contact with the teeth, and the novel oral tooth cleaner is converted from a liquid phase to a viscoelastic body and then taken out.
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| CN101217933A (en) * | 2005-07-08 | 2008-07-09 | 株式会社Lg生活健康 | Phase transitive breath care products |
| KR20080049177A (en) * | 2006-11-30 | 2008-06-04 | (주)아모레퍼시픽 | Oral composition for sol-gel phase transition containing a thermo-sensitive polymer |
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