CN114712292B - Anti-inflammatory pain-relieving toothpaste and preparation method thereof - Google Patents
Anti-inflammatory pain-relieving toothpaste and preparation method thereof Download PDFInfo
- Publication number
- CN114712292B CN114712292B CN202210504276.8A CN202210504276A CN114712292B CN 114712292 B CN114712292 B CN 114712292B CN 202210504276 A CN202210504276 A CN 202210504276A CN 114712292 B CN114712292 B CN 114712292B
- Authority
- CN
- China
- Prior art keywords
- toothpaste
- extraction
- extract
- tung
- petroleum ether
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000000606 toothpaste Substances 0.000 title claims abstract description 59
- 229940034610 toothpaste Drugs 0.000 title claims abstract description 58
- 230000003110 anti-inflammatory effect Effects 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title description 20
- 206010065390 Inflammatory pain Diseases 0.000 title description 2
- 239000000284 extract Substances 0.000 claims abstract description 76
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 70
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims abstract description 62
- 235000010678 Paulownia tomentosa Nutrition 0.000 claims abstract description 43
- 239000003208 petroleum Substances 0.000 claims abstract description 37
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 18
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 10
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 9
- 238000000605 extraction Methods 0.000 claims description 56
- 244000153888 Tung Species 0.000 claims description 44
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- PEDCQBHIVMGVHV-UHFFFAOYSA-N glycerol group Chemical group OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 10
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical group [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 9
- 230000000202 analgesic effect Effects 0.000 claims description 9
- 235000019333 sodium laurylsulphate Nutrition 0.000 claims description 9
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 6
- FTLYMKDSHNWQKD-UHFFFAOYSA-N (2,4,5-trichlorophenyl)boronic acid Chemical group OB(O)C1=CC(Cl)=C(Cl)C=C1Cl FTLYMKDSHNWQKD-UHFFFAOYSA-N 0.000 claims description 5
- 229940085605 saccharin sodium Drugs 0.000 claims description 5
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 claims description 4
- 239000004088 foaming agent Substances 0.000 claims description 4
- 235000011187 glycerol Nutrition 0.000 claims description 4
- 239000003906 humectant Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 239000003607 modifier Substances 0.000 claims description 4
- 239000003755 preservative agent Substances 0.000 claims description 4
- 230000002335 preservative effect Effects 0.000 claims description 4
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical group [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 claims description 4
- 239000004299 sodium benzoate Substances 0.000 claims description 4
- 235000010234 sodium benzoate Nutrition 0.000 claims description 4
- 239000000600 sorbitol Substances 0.000 claims description 4
- 239000002562 thickening agent Substances 0.000 claims description 4
- 239000000230 xanthan gum Substances 0.000 claims description 4
- 229920001285 xanthan gum Polymers 0.000 claims description 4
- 229940082509 xanthan gum Drugs 0.000 claims description 4
- 235000010493 xanthan gum Nutrition 0.000 claims description 4
- FUFJGUQYACFECW-UHFFFAOYSA-L calcium hydrogenphosphate Chemical compound [Ca+2].OP([O-])([O-])=O FUFJGUQYACFECW-UHFFFAOYSA-L 0.000 claims description 3
- 235000019700 dicalcium phosphate Nutrition 0.000 claims description 3
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 claims description 2
- 229940095079 dicalcium phosphate anhydrous Drugs 0.000 claims description 2
- 125000001033 ether group Chemical group 0.000 claims description 2
- 239000002260 anti-inflammatory agent Substances 0.000 claims 1
- 230000001741 anti-phlogistic effect Effects 0.000 claims 1
- 238000000638 solvent extraction Methods 0.000 abstract description 17
- 230000001760 anti-analgesic effect Effects 0.000 abstract description 10
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 abstract description 6
- 239000011575 calcium Substances 0.000 abstract description 6
- 229910052791 calcium Inorganic materials 0.000 abstract description 6
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 6
- 240000002834 Paulownia tomentosa Species 0.000 abstract 5
- 241000699670 Mus sp. Species 0.000 description 18
- 240000001866 Vernicia fordii Species 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 13
- 239000012071 phase Substances 0.000 description 13
- 239000002904 solvent Substances 0.000 description 10
- 238000003810 ethyl acetate extraction Methods 0.000 description 9
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 8
- 230000000694 effects Effects 0.000 description 8
- 238000010992 reflux Methods 0.000 description 7
- 230000008961 swelling Effects 0.000 description 7
- 238000000034 method Methods 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 238000010298 pulverizing process Methods 0.000 description 6
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 5
- 241000183291 Aleuritopteris Species 0.000 description 5
- 241000628997 Flos Species 0.000 description 5
- 206010061218 Inflammation Diseases 0.000 description 5
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 5
- 238000004140 cleaning Methods 0.000 description 4
- 239000000469 ethanolic extract Substances 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 230000004054 inflammatory process Effects 0.000 description 4
- 230000005764 inhibitory process Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 230000000844 anti-bacterial effect Effects 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 239000012153 distilled water Substances 0.000 description 3
- 238000009472 formulation Methods 0.000 description 3
- 239000003517 fume Substances 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 229960000583 acetic acid Drugs 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000002481 ethanol extraction Methods 0.000 description 2
- 206010016766 flatulence Diseases 0.000 description 2
- 230000002496 gastric effect Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- LXCFILQKKLGQFO-UHFFFAOYSA-N methylparaben Chemical compound COC(=O)C1=CC=C(O)C=C1 LXCFILQKKLGQFO-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000005191 phase separation Methods 0.000 description 2
- 230000008719 thickening Effects 0.000 description 2
- 238000003809 water extraction Methods 0.000 description 2
- 206010014025 Ear swelling Diseases 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 241000699666 Mus <mouse, genus> Species 0.000 description 1
- 206010034018 Parosmia Diseases 0.000 description 1
- 208000004880 Polyuria Diseases 0.000 description 1
- 241000220221 Rosales Species 0.000 description 1
- 210000000683 abdominal cavity Anatomy 0.000 description 1
- 230000005856 abnormality Effects 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 230000036592 analgesia Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 230000035619 diuresis Effects 0.000 description 1
- 239000002038 ethyl acetate fraction Substances 0.000 description 1
- 230000003203 everyday effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 230000023597 hemostasis Effects 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- ZDGGJQMSELMHLK-UHFFFAOYSA-N m-Trifluoromethylhippuric acid Chemical compound OC(=O)CNC(=O)C1=CC=CC(C(F)(F)F)=C1 ZDGGJQMSELMHLK-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000004292 methyl p-hydroxybenzoate Substances 0.000 description 1
- 235000010270 methyl p-hydroxybenzoate Nutrition 0.000 description 1
- 229960002216 methylparaben Drugs 0.000 description 1
- 239000006072 paste Substances 0.000 description 1
- 238000005325 percolation Methods 0.000 description 1
- 239000002798 polar solvent Substances 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000001648 tannin Substances 0.000 description 1
- 235000018553 tannin Nutrition 0.000 description 1
- 229920001864 tannin Polymers 0.000 description 1
- 239000002383 tung oil Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 230000029663 wound healing Effects 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
- A61K8/9783—Angiosperms [Magnoliophyta]
- A61K8/9789—Magnoliopsida [dicotyledons]
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/24—Phosphorous; Compounds thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/25—Silicon; Compounds thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P29/00—Non-central analgesic, antipyretic or antiinflammatory agents, e.g. antirheumatic agents; Non-steroidal antiinflammatory drugs [NSAID]
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P31/00—Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
- A61P31/02—Local antiseptics
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q11/00—Preparations for care of the teeth, of the oral cavity or of dentures; Dentifrices, e.g. toothpastes; Mouth rinses
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/20—Chemical, physico-chemical or functional or structural properties of the composition as a whole
- A61K2800/28—Rubbing or scrubbing compositions; Peeling or abrasive compositions; Containing exfoliants
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/805—Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Veterinary Medicine (AREA)
- Public Health (AREA)
- General Health & Medical Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Chemical & Material Sciences (AREA)
- Birds (AREA)
- Epidemiology (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Pharmacology & Pharmacy (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Medicinal Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Rheumatology (AREA)
- Pain & Pain Management (AREA)
- Communicable Diseases (AREA)
- Oncology (AREA)
- Oral & Maxillofacial Surgery (AREA)
- Engineering & Computer Science (AREA)
- Biotechnology (AREA)
- Botany (AREA)
- Microbiology (AREA)
- Mycology (AREA)
- Cosmetics (AREA)
Abstract
The invention belongs to the technical field of biology, and in particular relates to application of a tung flower extract in preparing anti-inflammatory and analgesic toothpaste and toothpaste. According to the invention, the tung flower extract with good stability is obtained by adopting ethyl acetate and petroleum ether double-solvent extraction, and the tung flower extract can be found to exist stably by adding the tung flower extract into a calcium hydrophosphate system, a silicon dioxide system or a natural calcium carbonate system toothpaste, and the tung flower extract has small impact on the stability of the toothpaste formula and excellent high-temperature and low-temperature stability.
Description
Technical Field
The invention belongs to the field of biotechnology. More particularly, relates to an anti-inflammatory and analgesic toothpaste and a preparation method thereof.
Background
Tung flower belongs to the class Rosales and is plant Tung (Tung) belonging to the order EuphorbialesVernicia fordii（Hemsl）Airy Shaw) Researches show that the tung flower has the effects of detumescence, analgesia, hemostasis, diuresis, disinsection and promotion of wound healing, but the application of the tung flower or the extract thereof in preparing antibacterial, anti-inflammatory and analgesic toothpaste is not studied at present.
Disclosure of Invention
The invention provides a toothpaste which contains a tung flower extract, can stably exist in various abrasive systems, has small impact on the toothpaste systems and has good antibacterial, anti-inflammatory and analgesic effects.
The invention aims to provide an extract of tung tree flowers and application thereof in preparing antibacterial, anti-inflammatory and analgesic toothpaste.
In some preferred embodiments, the tung flower extract is extracted with an ethanol solution, in particular an ethanol solution with a volume fraction of 85-95%, in particular an ethanol solution with a volume fraction of 85%, 90%, 95%.
The method for extraction with ethanol solution is not particularly limited as long as the active ingredient can be extracted, and specifically, an immersion method, a percolation method, a reflux extraction method, a continuous reflux extraction method, or the like can be used. Preferably, a reflux extraction method is used.
For the degree of pulverization of medicinal materials in the extraction process by adopting a reflux extraction method: in principle, the finer the medicinal powder is, the larger the specific surface area is, which is more favorable for the permeation, dissolution and diffusion of the solvent, and the higher the extraction efficiency is; however, the finer the powder of the medicinal material, the larger the specific surface area, the adsorption effect is enhanced, but the diffusion is affected, and a large amount of insoluble substances and more polysaccharide, protein and tannin extracts are caused by a large amount of breakage of tissue cells of the medicinal material, so that the viscosity of the extract is high and the impurities are more. Therefore, when pulverizing the tung flowers, it is preferable to pulverize the tung flowers so as to pass through a 20-60 mesh sieve, and it is preferable to pulverize the tung flowers so as to be 20 mesh. For the extraction temperature in the extraction process by adopting the reflux extraction method: compared with cold extraction, the extraction efficiency of hot extraction is higher, but the higher the temperature is, the better the higher the temperature is, the damage to effective components is easy to cause, and the impurities are easier to dissolve out, so the preferable temperature is 40-60 ℃, and the preferable temperature is 40-55 ℃; more preferably 50℃and 55 ℃. For the extraction time employed in the extraction process using reflux extraction: the extraction efficiency of the effective components is in direct proportion to the extraction time, but the long time causes energy waste, the production cost is increased, and the long-time extraction easily causes the dissolution of impurities to be increased, so that the quality of the extract is affected. In the invention, the preferable extraction time is 1-2 hours for each extraction, and 1-3 times for each extraction; more preferably, the extraction time is 1h each time, and 2 times of extraction are performed. For the extraction solvent dosage in the extraction process by adopting a reflux extraction method: the extraction efficiency is low due to the fact that the solvent consumption is too small, the extraction times are required to be increased, the subsequent concentration is time-consuming due to the fact that the solvent consumption is too large, and particularly in the invention, the ethanol solution consumption is generally 6-10 times that of medicinal materials; preferably 6 times, 8 times and 10 times, and when the number of extraction times exceeds 1 time, the amount of the extraction solvent may be sequentially reduced. After extraction, ethanol is removed by vacuum concentration to obtain extract.
In some embodiments, the tung flower is extracted with ethanol and then extracted with ethyl acetate and/or petroleum ether.
In some embodiments, ethyl acetate extraction is used after obtaining the ethanol extract of the tung flower to obtain ethyl acetate sites that exhibit better anti-inflammatory and analgesic effects but do not exhibit greater stability in toothpaste systems. In the process of obtaining the ethyl acetate part, extraction can be generally performed in a separating funnel, a lower mouth bottle or an extraction tank; for the concentration of the water phase in the extraction process, the relative density is generally controlled to be 1.0-1.2, the extraction is not easy to complete due to the fact that the concentration is too high, and the operation is affected due to the fact that the dosage is too large due to the fact that the concentration is too dilute. In the invention, deionized water can be adopted to dilute the extract to obtain the extract with the relative density of 1.0-1.2 g/cm 3 Is a water phase of (a) a (b). The dosage of the extraction solvent is preferably 1/3-1/2 of that of the water phase, preferably 1/2; the number of extraction is preferably 3 to 4.
In some embodiments, the ethanol extract of tung oil flowers is obtained and then extracted with petroleum ether to obtain the petroleum ether fraction. These sites showed better anti-inflammatory and analgesic effects but did not show greater stability in the toothpaste system. In the process of obtaining the petroleum ether part, extraction can be generally performed in a separating funnel, a lower mouth bottle or an extraction tank; for the concentration of the water phase in the extraction process, the relative density is generally controlled to be 1.0-1.2, the concentration is too high to be easy to extract completely, and the concentration is too dilute to be used for being too large, so that the operation is influenced. In the invention, deionized water can be adopted to dilute the extract to obtain the extract with the relative density of 1.0-1.2 g/cm 3 Is a water phase of (a) a (b). The dosage of the extraction solvent is preferably 1/3-1/2 of that of the water phase, preferably 1/2; the number of extraction is preferably 3 to 4.
In some preferred embodiments, the ethanol extract of the tung flower is obtained and then sequentially extracted with petroleum ether and ethyl acetate to obtain the petroleum ether and ethyl acetate fractions, respectively. In some preferred embodiments, the weight ratio of the ethyl acetate portion to the petroleum ether portion is 3-8:1, preferably 3-6:1, preferably 3:1, 4:1, 5:1 and 6:1. For the respective extraction of petroleum ether and ethyl acetate by using different polar solvents, the petroleum ether with low polarity is generally used for the extraction, and the process of extracting the petroleum ether is already detailed above and will not be described again here; after petroleum ether extraction is completed, the petroleum ether in the raffinate is removed, and then the raffinate is extracted by using ethyl acetate with high polarity. The combination of these sites shows surprising stability in various toothpaste systems and exhibits excellent anti-inflammatory and analgesic effects.
Stability as used herein means that the tung flower extract has little or no effect on the stability of various toothpaste systems. Specifically, the tung flower extract is stably stored in a toothpaste formula at a content of 0.1-10wt% and has small impact on the toothpaste formula, and the impact result specifically shows that: swelling, water discharge, solid-liquid phase separation, color change, smell change, hardening and the like of the toothpaste. On the other hand, the stability is also reflected in that the tung flower extract with the content of 0.1-10wt% can be stably present when being added into various toothpaste systems, and the toothpaste system has small impact on a toothpaste formula, and the toothpaste system particularly refers to a calcium hydrophosphate system, a silicon dioxide system or a natural calcium carbonate system (distinguished by friction agent types). In general, the invention proves that the 0.1-10wt% of the tung flower extract is added into a calcium hydrophosphate system, a silicon dioxide system or a natural calcium carbonate toothpaste system, so that the phenomena of gas expansion, water discharge, solid-liquid phase separation, discoloration, flavor change, hardening and the like of the toothpaste are not caused.
The invention also aims to provide stable anti-inflammatory and analgesic toothpaste which comprises 0.1-10wt% of the tung flower extract.
In some preferred embodiments, a stable anti-inflammatory analgesic toothpaste comprises the following components in mass fraction:
0.1-10wt% of an extract of tung tree flower;
15-35 wt% of an abrasive;
6-15 wt% of humectant;
1-3wt% of a foaming agent;
0.1-2wt% of a thickening agent;
0.1-0.5wt% of taste modifier;
0.1-0.5wt% of preservative;
0.1-0.3 wt% of essence; and
the balance of water.
In some preferred embodiments, the abrasive is silica, natural calcium carbonate, or dibasic calcium phosphate.
In some preferred embodiments, the humectant is glycerin, sorbitol, or propylene glycol; the foaming agent is sodium dodecyl sulfate, sodium laurylsulfate or CAB; the thickener is xanthan gum or CMC; the taste modifier is saccharin sodium; the preservative is sodium benzoate.
In some more preferred embodiments, a stable anti-inflammatory analgesic toothpaste comprises the following components in mass fraction:
0.1-10wt% of an extract of tung tree flower;
15-20wt% of silicon dioxide;
6-15wt% of sorbitol;
0.5-1.5wt% of sodium dodecyl sulfate;
CAB 0.5~1.5 wt%；
CMC 0.1~2 wt%；
0.1-0.5wt% of saccharin sodium;
0.1-0.5 wt% of sodium benzoate;
0.1-0.3 wt% of essence; and
the balance of water.
In some more preferred embodiments, a stable anti-inflammatory analgesic toothpaste comprises the following components in mass fraction:
0.1-10wt% of an extract of tung tree flower;
15-35wt% of natural calcium carbonate;
6-10wt% of glycerol;
0.5-1.5 wt% of sodium dodecyl sulfate;
0.5-1.5 wt% of sodium lauryl sulfate;
0.1-2wt% of xanthan gum;
0.1-0.5wt% of saccharin sodium;
0.1wt% of methyl paraben;
0.1-0.3 wt% of essence; and
the balance of water.
In some more preferred embodiments, a stable anti-inflammatory analgesic toothpaste comprises the following components in mass fraction:
0.1-10wt% of an extract of tung tree flower;
15-35wt% of calcium hydrophosphate;
3-6wt% of glycerol;
3-6% of sorbitol
0.5-1.5 wt% of sodium dodecyl sulfate;
0.5-1.5wt% of sodium lauryl sulfate;
0.1-1 wt% of xanthan gum;
0.1-0.5 wt% of saccharin sodium;
0.1-0.5 wt% of sodium benzoate;
0.1-0.3 wt% of essence; and
the balance of water.
The invention has the following beneficial effects:
according to the invention, the tung flower extract with good stability is obtained by adopting ethyl acetate and petroleum ether double-solvent extraction, and the tung flower extract can be found to exist stably by adding the tung flower extract into a calcium hydrophosphate system, a silicon dioxide system or a natural calcium carbonate system toothpaste, and the tung flower extract has small impact on the stability of the toothpaste formula and excellent high-temperature and low-temperature stability.
Description of the embodiments
The present invention will be further described by the following examples, however, the scope of the present invention is not limited to the following examples. Those skilled in the art will appreciate that various changes and modifications can be made to the invention without departing from the spirit and scope thereof.
Example one, preparation of Aleurites fordii flower extract
Cleaning flos Aleuritopteris Crispi, pulverizing into 20 mesh coarse powder, adding 6 times of 85% ethanol solution, extracting at 50deg.C for 2 times each for 1 hr, filtering, mixing filtrates, removing ethanol under reduced pressure, and concentrating to obtain extract;
diluting the extract with distilled water to obtain extract with relative density of 1.1g/cm 3 Adding 1/2 of the volume of petroleum ether in the water phase to extract for 3 times, and combining the extracts to obtain petroleum ether extraction parts;
volatilizing solvent in a fume hood, adding ethyl acetate with the volume of 1/2 of the water phase volume, extracting for 3 times, and combining the extracts to obtain an ethyl acetate extraction part;
and combining the ethyl acetate extraction part and the petroleum ether extraction part according to the weight ratio of 3:1 to obtain the tung flower extract.
Example two preparation of Aleurites fordii flower extract
Cleaning flos Aleuritopteris Crispi, pulverizing into 20 mesh coarse powder, adding 8 times of 90% ethanol solution, extracting at 55deg.C for 2 times each for 1 hr, filtering, mixing filtrates, removing ethanol under reduced pressure, and concentrating to obtain extract;
dissolving the extract with distilled water to obtain extract with relative density of 1.2g/cm 3 Adding 1/2 of the volume of petroleum ether in the water phase to extract for 3 times, and combining the extracts to obtain petroleum ether extraction parts;
volatilizing solvent in a fume hood, adding ethyl acetate with the volume of 1/2 of the water phase volume, extracting for 3 times, and combining the extracts to obtain an ethyl acetate extraction part; and combining the ethyl acetate extraction part and the petroleum ether extraction part according to the weight ratio of 5:1 to obtain the tung flower extract.
Example three preparation of Aleurites fordii flower extract
Cleaning flos Aleuritopteris Crispi, pulverizing into 20 mesh coarse powder, adding 10 times of 95% ethanol solution, extracting at 55deg.C for 2 times each for 1 hr, filtering, mixing filtrates, removing ethanol under reduced pressure, and concentrating to obtain extract;
dissolving the extract with distilled water to obtain extract with relative density of 1.2g/cm 3 Adding 1/2 of the volume of petroleum ether in the water phase to extract for 3 times, and combining the extracts to obtain petroleum ether extraction parts;
volatilizing solvent in a fume hood, adding ethyl acetate with the volume of 1/2 of the water phase volume, extracting for 3 times, and combining the extracts to obtain an ethyl acetate extraction part;
and combining the ethyl acetate extraction part and the petroleum ether extraction part according to the weight ratio of 6:1 to obtain the tung flower extract.
Comparative example one, preparation of Aleurites fordii flower extract
The third difference from the example is that the tung flower extract is a 95% ethanol extract, the preparation process does not comprise the step of extracting by petroleum ether and ethyl acetate, and the rest parameters are the same as the three phases of the example.
Comparative example two, preparation of Aleurites fordii flower extract
The difference from the third example is that the ethyl acetate extraction step is omitted in the preparation process, and the rest parameters are the same as those of the third example.
Comparative example three, preparation of Aleurites fordii flower extract
The third difference from the example is that the petroleum ether extraction step is omitted in the preparation process, and the rest parameters are the same as those of the example.
Comparative example IV, preparation of Aleurites fordii flower extract
The difference from the third example is that chloroform is used instead of ethyl acetate in the preparation process, and the rest parameters are the same as those of the third example.
Comparative example five, preparation of Water extract of Aleurites fordii flower
The preparation method comprises the following steps: cleaning flos Aleuritopteris Crispi, pulverizing into 20 mesh coarse powder, adding 10 times of deionized water, decocting for 2 times each for 1 hr, filtering, and mixing filtrates to obtain flos Aleuritopteris Crispi water extract.
Comparative example six preparation of Aleurites fordii flower extract
The difference from the third example is that the weight ratio of the ethyl acetate extraction part to the petroleum ether extraction part is 1:1, and the rest parameters are the same as the third example.
Test example one, anti-inflammatory and analgesic test of Aleurites fordii flower extracts prepared by different methods
1.1 test for mice ear swelling caused by xylene
80 clean ICR mice are taken, the mass of the mice is 18-22 g, the mice are randomly divided into a model group, an example III and a comparison example I-six, 10 mice in each group are subjected to gastric lavage with the same volume of 10ml/kg each day, the mice are subjected to gastric lavage for 1 time each day, the continuous period is 7 days, 100% dimethylbenzene is sucked by a microsyringe for 1h after the last administration, 0.03ml of dimethylbenzene is uniformly coated on the inner side and the outer side of the right ear of each group of mice to cause inflammation, and the left ear is taken as a comparison group. After 1h of inflammation, mice were sacrificed, auricles on the left and right sides were cut off along the auricle baseline of the mice, round ear pieces were cut off at the same positions of the two auricles by using a punch with a diameter of 6mm, the weight of the two ear pieces was precisely weighed, and the swelling degree and inhibition ratio were calculated according to the following formulas.
Inflammatory swelling degree (mg) =weight of right ear piece-weight of left ear piece
Inflammation inhibition ratio (%) = [ (average swelling degree of model group-average swelling degree of administration group)/average swelling degree of model group ] ×100%
Table 1: results of swelling test on mouse auricle (n=10)
Note that: in contrast to the set of models, # P＜0.05， ## p is less than 0.05; in contrast to the three groups of examples, * P＜0.05， ** P＜0.01。
as can be seen from the analysis of the table, compared with the model group, the auricle inflammation swelling degree of the mice in the other groups except the group of the comparative example is obviously reduced, and the difference is obviously different (P < 0.05), wherein the three groups of the example are extremely obviously different (P < 0.01) compared with the model group; there were significant differences between the remaining groups compared to the three groups of the example. Inhibition ratio contrast: the ethanol extraction is less than the petroleum ether single-solvent extraction is less than the ethyl acetate single-solvent extraction is less than the chloroform+petroleum ether double-solvent extraction is less than the water extraction is less than the ethyl acetate+petroleum ether double-solvent extraction, and the inhibition effect of the extract obtained by the double-solvent extraction is better than that of the extract obtained by the single-solvent extraction, and the single-use 95% ethanol extraction effect is the worst.
1.2 acetic acid induced mice torsion test
Taking 80 magnetic mice, namely male and female mice with the mass of 18-26 g, randomly dividing the mice into a model group, an embodiment III and a comparison example I-six groups, filling the stomach of each group of 10 mice with the same volume of 10mL/kg, continuously administering for 3 days every day, injecting 0.6% glacial acetic acid (0.01 mL/g) into the abdominal cavity 1h after the last administration, recording the time and the times of torsion reaction of the mice within 15min, and calculating the analgesic rate.
Analgesic rate = ×100%
Table 2: effect on acetic acid torsion reaction in mice (n=10)
Note that: in contrast to the set of models, # P＜0.05， ## p is less than 0.05; in contrast to the three groups of examples, * P＜0.05， ** P＜0.01。
analysis of the test results in the table shows that the number of writhing times of mice is compared: ethyl acetate and petroleum ether double solvent extraction < water extraction < chloroform and petroleum ether double solvent extraction < ethyl acetate single solvent extraction < petroleum ether single solvent extraction < alcohol extraction < model group.
Test example two, study of stability of different Aleurites fordii flower extracts to three toothpaste System formulations
Preparing various toothpastes with different systems according to the basic formulas of tables 3-5, and performing high-temperature accelerated aging and cold resistance tests, wherein the results are shown in the following table;
table 3: formula of silicon dioxide system tung flower toothpaste
The tung flower extracts prepared in the comparative examples one to six are adopted to replace the tung flower extract in the embodiment three, and the toothpaste in the comparative examples one to six is prepared according to the conventional preparation process.
Table 4: formula of tung flower toothpaste with calcium carbonate system
The tung flower extracts prepared in the comparative examples one to six are adopted to replace the tung flower extract in the embodiment three, and the toothpaste in the comparative examples one to six is prepared according to the conventional preparation process.
Table 5: formula of tung flower toothpaste with calcium hydrophosphate system
The tung flower extracts prepared in the comparative examples one to six are adopted to replace the tung flower extract in the embodiment three, and the toothpaste in the comparative examples one to six is prepared according to the conventional preparation process.
Table 6: effect of different Aleurites fordii flower extracts on high temperature stability of various toothpaste systems (45 ℃ C., three months)
Note that: qc0, no anomaly; qc1, separating liquid at a pipe orifice; qc2, toothpaste flatulence; qc3: the toothpaste has peculiar smell; qc4: color change of the toothpaste; qc5: thickening toothpaste; qc6, shelling; qc7, hardening the toothpaste.
TABLE 7 Effect of different Aleurites fordii flower extracts on Low temperature stability of various toothpaste systems (-8 ℃ C., one month)
Note that: qc0, no anomaly; qc1, separating liquid at a pipe orifice; qc2, toothpaste flatulence; qc3: the toothpaste has peculiar smell; qc4: color change of the toothpaste; qc5: thickening toothpaste; qc6, shelling; qc7, hardening the toothpaste.
As is clear from the results in Table 6 and Table 7, the extract of Aleurites fordii flower obtained by double solvent extraction of ethyl acetate and petroleum ether was stable in 10wt% in toothpaste of silica system, natural calcium carbonate system and calcium hydrogen phosphate system, and had less impact on stability of formulation, and the toothpaste containing the extract of Aleurites fordii flower was free from abnormality in paste after cold resistance and high temperature aging test, showing excellent stability. Compared with double solvent extraction, the tung flower extract obtained by petroleum ether single solvent extraction or ethyl acetate single solvent extraction has poor stability in various toothpaste systems, larger impact on toothpaste formulation and poor high-temperature and low-temperature stability of toothpaste. Also, surprisingly, the same double solvent extraction was used, but the tung flower obtained with chloroform + petroleum ether did not show the same properties.
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.
Claims (3)
1. A stable anti-inflammatory analgesic toothpaste, characterized by comprising the following components in mass fraction:
0.1-10wt% of an extract of tung tree flower;
15-35 wt% of an abrasive;
6-15 wt% of humectant;
1-3wt% of a foaming agent;
0.1-2wt% of a thickening agent;
0.1-0.5wt% of taste modifier;
0.1-0.5wt% of preservative;
0.1-0.3 wt% of essence; and
the balance of water;
the tung flower extract is extracted by adopting an ethanol solution with the concentration of 85-95%, then ethyl acetate and petroleum ether are respectively used for extraction, the ethyl acetate part and the petroleum ether part are obtained, and the mixture is mixed according to the weight ratio of 3-8:1.
2. The anti-inflammatory analgesic toothpaste of claim 1, wherein the abrasive is silica, natural calcium carbonate, or dibasic calcium phosphate.
3. The antiphlogistic and analgesic toothpaste according to claim 1 or 2, wherein the humectant is glycerin, sorbitol or propylene glycol; the foaming agent is sodium dodecyl sulfate, sodium laurylsulfate or CAB; the thickener is xanthan gum or CMC; the taste modifier is saccharin sodium; the preservative is sodium benzoate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210504276.8A CN114712292B (en) | 2022-05-10 | 2022-05-10 | Anti-inflammatory pain-relieving toothpaste and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210504276.8A CN114712292B (en) | 2022-05-10 | 2022-05-10 | Anti-inflammatory pain-relieving toothpaste and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114712292A CN114712292A (en) | 2022-07-08 |
| CN114712292B true CN114712292B (en) | 2023-10-20 |
Family
ID=82231194
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210504276.8A Active CN114712292B (en) | 2022-05-10 | 2022-05-10 | Anti-inflammatory pain-relieving toothpaste and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114712292B (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102613255A (en) * | 2012-03-09 | 2012-08-01 | 中南林业科技大学 | Method for preparing insecticide from vernicia fordii hemsley hull extract |
| CN104510665A (en) * | 2013-12-21 | 2015-04-15 | 莫治玲 | Traditional Chinese medicinal toothpaste for inflammation preventing and pain easing |
| FR3013985A1 (en) * | 2013-12-03 | 2015-06-05 | Galephar M F | MOISTURIZING COMPOSITIONS COMPRISING AT LEAST ONE CAESALPINIA SPINOSA EXTRACT WITH AT LEAST VASELIN AND GLYCERIN |
| CN108440477A (en) * | 2018-04-23 | 2018-08-24 | 江苏耐雀生物工程技术有限公司 | A method of preparing Quercetin from tungoiltree juvenile leaf |
| KR20180106997A (en) * | 2017-03-20 | 2018-10-01 | (주)지에프씨생명과학 | Cosmetic Compositions Containing Fermented Extracts of Vernicia fordii |
-
2022
- 2022-05-10 CN CN202210504276.8A patent/CN114712292B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102613255A (en) * | 2012-03-09 | 2012-08-01 | 中南林业科技大学 | Method for preparing insecticide from vernicia fordii hemsley hull extract |
| FR3013985A1 (en) * | 2013-12-03 | 2015-06-05 | Galephar M F | MOISTURIZING COMPOSITIONS COMPRISING AT LEAST ONE CAESALPINIA SPINOSA EXTRACT WITH AT LEAST VASELIN AND GLYCERIN |
| CN104510665A (en) * | 2013-12-21 | 2015-04-15 | 莫治玲 | Traditional Chinese medicinal toothpaste for inflammation preventing and pain easing |
| KR20180106997A (en) * | 2017-03-20 | 2018-10-01 | (주)지에프씨생명과학 | Cosmetic Compositions Containing Fermented Extracts of Vernicia fordii |
| CN108440477A (en) * | 2018-04-23 | 2018-08-24 | 江苏耐雀生物工程技术有限公司 | A method of preparing Quercetin from tungoiltree juvenile leaf |
Non-Patent Citations (2)
| Title |
|---|
| 国家食品药监督管理总局.《化妆品安全技术规范》.2015,(第1版),第116页. * |
| 张世凤等.油桐花不同部位提取物的抗炎镇痛作用研究.《贵阳中医学院学报》.2019,第41卷(第6期),第11-15页. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114712292A (en) | 2022-07-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101768514B (en) | Alhagi sparsifolia extract and preparation method and application thereof | |
| CN101293038B (en) | Leaf extract and its preparation method as well as its preparation and use | |
| JP5777774B1 (en) | Topical skin preparation | |
| CN102293997B (en) | Preparation method of dried ginger extract | |
| TWI364289B (en) | Antitussive agent and manufacture thereof | |
| CN114712292B (en) | Anti-inflammatory pain-relieving toothpaste and preparation method thereof | |
| CN109370785B (en) | A kind of amino acid soap containing tangerine peel extract and preparation method thereof | |
| CN111297756B (en) | Essence with moistening and moisturizing and anti-allergy effects and preparation method thereof | |
| CN105267261A (en) | Plant extract combination having skin repair promoting and healing promoting function | |
| CN102048857B (en) | Method for extracting alkaloid from Kratom | |
| CN101972220B (en) | Medicated toothpaste | |
| CN105919891A (en) | Lophantherum gracile skincare gel and preparation method thereof | |
| CN102283913A (en) | Radix aconiti carmichaeli extract and application thereof | |
| CN112662478A (en) | Chrysanthemum essence, oral cleaning product containing chrysanthemum essence and preparation method of oral cleaning product | |
| CN105534791A (en) | Medicinal toothpaste containing nutgall ethyl acetate extract and production method thereof | |
| CN100526327C (en) | Process for producing ursolic acid | |
| CN105476870B (en) | A kind of medicated toothpaste containing Gastrodin | |
| CN100335073C (en) | Process for preparing semen momordicae seed extract containing triterpene saponin component | |
| CN116391868A (en) | Liver-nourishing and liver-protecting medicinal and edible composition | |
| CN111184667B (en) | A kind of composition with moisturizing, moisturizing, anti-allergic effect and preparation method thereof | |
| KR20190057727A (en) | Composition for improving bronchial health improved palatability | |
| CN100528170C (en) | Mangiferin preparation and production thereof | |
| CN113907394A (en) | Preparation method of apple extract for cigarettes | |
| CN1865289A (en) | Preparation and uses of polysaccharide from urtica fissa | |
| EP3721891A1 (en) | Herbal composition for preventing or treating benign prostatic hyperplasia disease |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20230921 Address after: Room 502, No. 13, Zone 2, No. 3333 Qixin Road, Minhang District, Shanghai, 201101 Applicant after: Fu Tao Address before: 510670 room 1906, No. 48, Kexue Avenue, Huangpu District, Guangzhou, Guangdong Province (office only) Applicant before: Boya (Guangzhou) Biotechnology Research Institute Co.,Ltd. |
|
| TA01 | Transfer of patent application right | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20240329 Address after: Room A210, Building 1, No. 600 Huaxi Road, Minhang District, Shanghai, 2011 Patentee after: Shanghai Peptide Biotech Co.,Ltd. Country or region after: China Address before: Room 502, No. 13, Zone 2, No. 3333 Qixin Road, Minhang District, Shanghai, 201101 Patentee before: Fu Tao Country or region before: China |
|
| TR01 | Transfer of patent right |