CN111298115A - Light-operated tea flavone silver/silver oxide nano preparation and preparation method and application thereof - Google Patents
Light-operated tea flavone silver/silver oxide nano preparation and preparation method and application thereof Download PDFInfo
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- CN111298115A CN111298115A CN202010197995.0A CN202010197995A CN111298115A CN 111298115 A CN111298115 A CN 111298115A CN 202010197995 A CN202010197995 A CN 202010197995A CN 111298115 A CN111298115 A CN 111298115A
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- silver
- tea flavone
- light
- flavone
- silver oxide
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- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 241001122767 Theaceae Species 0.000 title claims abstract description 54
- VRKKUDZYIGLTIC-UHFFFAOYSA-N 2-phenylchromen-4-one silver Chemical compound [Ag].O1C(=CC(=O)C2=CC=CC=C12)C1=CC=CC=C1 VRKKUDZYIGLTIC-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 229910001923 silver oxide Inorganic materials 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 35
- 239000003504 photosensitizing agent Substances 0.000 claims abstract description 18
- 239000003814 drug Substances 0.000 claims abstract description 15
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 claims abstract description 13
- 229930003944 flavone Natural products 0.000 claims abstract description 13
- 235000011949 flavones Nutrition 0.000 claims abstract description 13
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 150000002212 flavone derivatives Chemical class 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 11
- 229910052709 silver Inorganic materials 0.000 claims abstract description 9
- 230000001954 sterilising effect Effects 0.000 claims abstract description 8
- 238000004659 sterilization and disinfection Methods 0.000 claims abstract description 8
- TWCMVXMQHSVIOJ-UHFFFAOYSA-N Aglycone of yadanzioside D Natural products COC(=O)C12OCC34C(CC5C(=CC(O)C(O)C5(C)C3C(O)C1O)C)OC(=O)C(OC(=O)C)C24 TWCMVXMQHSVIOJ-UHFFFAOYSA-N 0.000 claims abstract description 6
- PLMKQQMDOMTZGG-UHFFFAOYSA-N Astrantiagenin E-methylester Natural products CC12CCC(O)C(C)(CO)C1CCC1(C)C2CC=C2C3CC(C)(C)CCC3(C(=O)OC)CCC21C PLMKQQMDOMTZGG-UHFFFAOYSA-N 0.000 claims abstract description 6
- PFOARMALXZGCHY-UHFFFAOYSA-N homoegonol Natural products C1=C(OC)C(OC)=CC=C1C1=CC2=CC(CCCO)=CC(OC)=C2O1 PFOARMALXZGCHY-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000002105 nanoparticle Substances 0.000 claims abstract description 6
- 239000004332 silver Substances 0.000 claims abstract description 6
- UKHWJBVVWVYFEY-UHFFFAOYSA-M silver;hydroxide Chemical group [OH-].[Ag+] UKHWJBVVWVYFEY-UHFFFAOYSA-M 0.000 claims abstract description 5
- 238000013329 compounding Methods 0.000 claims abstract description 3
- KHJDQHIZCZTCAE-UHFFFAOYSA-N oxosilver;silver Chemical group [Ag].[Ag]=O KHJDQHIZCZTCAE-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000005979 thermal decomposition reaction Methods 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- 239000000047 product Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 229930003935 flavonoid Natural products 0.000 claims description 9
- 150000002215 flavonoids Chemical class 0.000 claims description 9
- 235000017173 flavonoids Nutrition 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 8
- VFLDPWHFBUODDF-FCXRPNKRSA-N curcumin Chemical compound C1=C(O)C(OC)=CC(\C=C\C(=O)CC(=O)\C=C\C=2C=C(OC)C(O)=CC=2)=C1 VFLDPWHFBUODDF-FCXRPNKRSA-N 0.000 claims description 8
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 7
- 239000002244 precipitate Substances 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 239000003995 emulsifying agent Substances 0.000 claims description 6
- -1 polyoxyethylene stearate Polymers 0.000 claims description 6
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 claims description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 239000004148 curcumin Substances 0.000 claims description 4
- 229940109262 curcumin Drugs 0.000 claims description 4
- 235000012754 curcumin Nutrition 0.000 claims description 4
- VFLDPWHFBUODDF-UHFFFAOYSA-N diferuloylmethane Natural products C1=C(O)C(OC)=CC(C=CC(=O)CC(=O)C=CC=2C=C(OC)C(O)=CC=2)=C1 VFLDPWHFBUODDF-UHFFFAOYSA-N 0.000 claims description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 4
- 229930006000 Sucrose Natural products 0.000 claims description 3
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 3
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 3
- 239000000194 fatty acid Substances 0.000 claims description 3
- 229930195729 fatty acid Natural products 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 238000001556 precipitation Methods 0.000 claims description 3
- 239000005720 sucrose Substances 0.000 claims description 3
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 2
- KGHNSNSWRMJVND-UHFFFAOYSA-N Hypocrellin Natural products COC1=CC(=O)C2=C3C4C(C(C(=O)C)C(C)(O)Cc5c(OC)c(O)c6C(=O)C=C(OC)C(=C13)c6c45)C(=C2O)OC KGHNSNSWRMJVND-UHFFFAOYSA-N 0.000 claims description 2
- 229920001214 Polysorbate 60 Polymers 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 235000019253 formic acid Nutrition 0.000 claims description 2
- VANSZAOQCMTTPB-SETSBSEESA-N hypocrellin Chemical compound C1[C@@](C)(O)[C@@H](C(C)=O)C2=C(OC)C(O)=C3C(=O)C=C(OC)C4=C3C2=C2C3=C4C(OC)=CC(=O)C3=C(O)C(OC)=C21 VANSZAOQCMTTPB-SETSBSEESA-N 0.000 claims description 2
- 230000001376 precipitating effect Effects 0.000 claims description 2
- 239000012716 precipitator Substances 0.000 claims description 2
- BQJKVFXDDMQLBE-UHFFFAOYSA-N shiraiachrome A Natural products COC1=C2C3=C(OC)C=C(O)C4=C3C3=C5C(CC(C)(O)C(C(C)=O)C3=C(OC)C4=O)=C(OC)C(=O)C(C(O)=C1)=C25 BQJKVFXDDMQLBE-UHFFFAOYSA-N 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 10
- 230000002195 synergetic effect Effects 0.000 abstract description 3
- 230000009982 effect on human Effects 0.000 abstract 1
- 230000002708 enhancing effect Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 12
- 239000007788 liquid Substances 0.000 description 6
- CQLFBEKRDQMJLZ-UHFFFAOYSA-M silver acetate Chemical compound [Ag+].CC([O-])=O CQLFBEKRDQMJLZ-UHFFFAOYSA-M 0.000 description 6
- 229940071536 silver acetate Drugs 0.000 description 6
- 238000012360 testing method Methods 0.000 description 5
- 230000000844 anti-bacterial effect Effects 0.000 description 4
- 230000001580 bacterial effect Effects 0.000 description 4
- 229940079593 drug Drugs 0.000 description 4
- 241000894006 Bacteria Species 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000005286 illumination Methods 0.000 description 3
- IYRMWMYZSQPJKC-UHFFFAOYSA-N kaempferol Chemical group C1=CC(O)=CC=C1C1=C(O)C(=O)C2=C(O)C=C(O)C=C2O1 IYRMWMYZSQPJKC-UHFFFAOYSA-N 0.000 description 3
- 150000003378 silver Chemical group 0.000 description 3
- 230000008685 targeting Effects 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- 241000588701 Pectobacterium carotovorum Species 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 2
- 230000001186 cumulative effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000005764 inhibitory process Effects 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 239000008223 sterile water Substances 0.000 description 2
- 229910001369 Brass Inorganic materials 0.000 description 1
- UBSCDKPKWHYZNX-UHFFFAOYSA-N Demethoxycapillarisin Natural products C1=CC(O)=CC=C1OC1=CC(=O)C2=C(O)C=C(O)C=C2O1 UBSCDKPKWHYZNX-UHFFFAOYSA-N 0.000 description 1
- 239000012880 LB liquid culture medium Substances 0.000 description 1
- 239000006142 Luria-Bertani Agar Substances 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 230000000259 anti-tumor effect Effects 0.000 description 1
- 230000000840 anti-viral effect Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 239000000022 bacteriostatic agent Substances 0.000 description 1
- 239000010951 brass Substances 0.000 description 1
- 239000007853 buffer solution Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000013267 controlled drug release Methods 0.000 description 1
- 238000012258 culturing Methods 0.000 description 1
- 230000022811 deglycosylation Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 230000013595 glycosylation Effects 0.000 description 1
- 238000006206 glycosylation reaction Methods 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- MWDZOUNAPSSOEL-UHFFFAOYSA-N kaempferol Natural products OC1=C(C(=O)c2cc(O)cc(O)c2O1)c3ccc(O)cc3 MWDZOUNAPSSOEL-UHFFFAOYSA-N 0.000 description 1
- 235000008777 kaempferol Nutrition 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 230000011987 methylation Effects 0.000 description 1
- 238000007069 methylation reaction Methods 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- UXOUKMQIEVGVLY-UHFFFAOYSA-N morin Natural products OC1=CC(O)=CC(C2=C(C(=O)C3=C(O)C=C(O)C=C3O2)O)=C1 UXOUKMQIEVGVLY-UHFFFAOYSA-N 0.000 description 1
- 239000008363 phosphate buffer Substances 0.000 description 1
- 239000008055 phosphate buffer solution Substances 0.000 description 1
- 230000001766 physiological effect Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000041 toxicology testing Toxicity 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K41/00—Medicinal preparations obtained by treating materials with wave energy or particle radiation ; Therapies using these preparations
- A61K41/0057—Photodynamic therapy with a photosensitizer, i.e. agent able to produce reactive oxygen species upon exposure to light or radiation, e.g. UV or visible light; photocleavage of nucleic acids with an agent
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/33—Heterocyclic compounds
- A61K31/335—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin
- A61K31/35—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin having six-membered rings with one oxygen as the only ring hetero atom
- A61K31/352—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin having six-membered rings with one oxygen as the only ring hetero atom condensed with carbocyclic rings, e.g. methantheline
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K33/00—Medicinal preparations containing inorganic active ingredients
- A61K33/24—Heavy metals; Compounds thereof
- A61K33/38—Silver; Compounds thereof
-
- 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
- A61P31/04—Antibacterial agents
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Veterinary Medicine (AREA)
- Public Health (AREA)
- Medicinal Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Pharmacology & Pharmacy (AREA)
- Epidemiology (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oncology (AREA)
- Biochemistry (AREA)
- Molecular Biology (AREA)
- Communicable Diseases (AREA)
- Inorganic Chemistry (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention provides a light-operated tea flavone silver/silver oxide nano preparation which is characterized by comprising the following components in percentage by weight: a photosensitizer, a silver oxide and a tea flavone silver complex; the tea flavone silver complex is prepared by compounding tea flavone aglycone and silver, the silver oxide is obtained by thermal decomposition of silver hydroxide, and the photosensitizer is a natural traditional Chinese medicine photosensitizer; the nano particles are 60-100 nm, and the molar ratio of the tea flavone silver to the silver oxide silver atoms is 20:1-5: 1. The invention also provides a preparation method and application of the light-operated tea flavone silver/silver oxide nano preparation. The product and the method have small side effect on human bodies and have the effect of enhancing the synergistic sterilization.
Description
Technical Field
The invention relates to the field of medicines, in particular to a light-operated tea flavone silver/silver oxide nano preparation with an efficient sterilization effect, a preparation method and application thereof.
Background
The plant flavonoids have obvious antioxidation, and many plants contain the flavonoids, but the physiological activities of different types and sources of the flavonoids are greatly different. The tea seeds contain flavone with kaempferol structure, and kaempferol has antitumor, antiinflammatory, antioxidant, antibacterial and antiviral effects.
The biggest defects of the flavone compound are poor stability and targeting property. Although there are structural modification methods such as deglycosylation, esterification, glycosylation, methylation, etc., the process is complex and the effect is not obvious. The tea flavone and silver are coordinated to prepare the light-operated nano preparation, and the research on realizing the light-operated tissue targeting is not reported.
Silver oxide nanoparticles have a bactericidal effect, but the toxicity of the nanoparticles themselves is now unknown. Therefore, it is an effective means to load it on a carrier.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention aims to provide a light-operated tea flavone silver/silver oxide nano preparation, a preparation method thereof and application thereof.
The invention provides a light-operated tea flavone silver/silver oxide nano preparation which is characterized by comprising the following components in percentage by weight: a photosensitizer, a silver oxide and a tea flavone silver complex; the tea flavone silver complex is prepared by compounding tea flavone aglycone and silver, the silver oxide is obtained by thermal decomposition of silver hydroxide, and the photosensitizer is a natural traditional Chinese medicine photosensitizer; the nano particles are 60-100 nm, and the molar ratio of the tea flavone silver to the silver oxide silver atoms is 20:1-5: 1.
The invention also provides a preparation method of the light-operated tea flavone silver/silver oxide nano preparation, which is characterized by comprising the following steps of: the method comprises the following steps: (1) carrying out acidolysis on tea flavonoids by using an ethanol solution of acid to obtain acidolysis solution; concentrating to obtain concentrated solution; precipitating the concentrated solution by adopting a precipitator to obtain a precipitate;
(2) dissolving the precipitate, adding silver salt, emulsifier and water, adjusting pH to 7-8, carrying out hydrothermal reaction at 80 ℃ for 2 hours, filtering and washing;
(3) dispersing the product obtained in the step 2 in an ethanol water solution, adding a photosensitizer, anhydrous sodium carbonate and a silver salt, adjusting the pH value to 10, and carrying out hydrothermal reaction at 80 ℃ for 2 hours;
(4) standing for precipitation, washing and drying to obtain the light-operated tea flavone silver/silver oxide nano preparation.
Further, in the step (1), the acid is more than one of hydrochloric acid, sulfuric acid or formic acid, and the mass concentration of the acid in ethanol in an ethanol solution of the acid is 2-5%; in the step (1), the acidolysis temperature is 70-80 ℃, and the acidolysis time is 5-8 hours.
Further, the addition amount of the anhydrous sodium carbonate in the step (2) is 10-20% of the mass of the tea flavone.
Further, the emulsifier is one or more of tween 60, polyoxyethylene stearate or sucrose fatty acid ester.
Further, the traditional Chinese medicine photosensitizer is more than one of pheophorbide, curcumin or hypocrellin.
Further, the adding amount of the emulsifier is 0.5-3% of the mass of the tea flavone silver complex, the using amount of the water is 5-10 times of the mass of the tea flavone silver complex, and the adding amount of the traditional Chinese medicine photosensitizer is 0.1-1% of the mass of the tea flavone silver complex.
Further, the molar amount of silver salt added in step 3 is 5% -20% of the product of step 2 added.
Further, the light-operated tea flavone silver/silver oxide nano preparation is used as a high-efficiency sterilization medicament.
Compared with the prior art, the invention has the following advantages and effects:
(1) according to the flavone silver/silver oxide nano preparation prepared by the invention, brass aglycone and silver are used in a matched manner, so that the synergistic effect is achieved, and the sterilization effect of the nano preparation is enhanced; the flavonoids in the Chinese patent medicines are used as main sterilization components, and the silver oxide is used as an auxiliary effect, so that the toxic effect of the silver oxide is reduced; meanwhile, the silver oxide has a promoting effect on flavonoid sterilization, has a better sterilization effect than single silver oxide or flavonoid, has a synergistic promoting effect, further reduces the usage amount of the medicament, and reduces side effects;
(2) the tea flavone is acidolyzed to obtain flavone aglycone, the flavone aglycone is matched with silver to form a tea flavone silver complex, after the pH value is adjusted, a silver hydroxide colloid is formed in a solution and is coated on the surface of the flavone silver, then the silver hydroxide colloid is decomposed in a hydrothermal emulsification method, the flavone silver and the silver oxide are combined with each other, the traditional Chinese medicine photosensitizer and the silver oxide are positioned at an outer layer, the tea flavone silver is coated at an inner layer, and the formed nano particles are stable in structure;
(3) the photosensitizer can be used as the targeting guide of flavonoid drugs on one hand, and can absorb photons on the other hand to promote the silver oxide to generate bactericidal efficacy.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
Example 1
Preparation of product with silver atom molar ratio of tea flavone silver to silver oxide of 5:1
(1) Adding 1kg of tea flavone into 4kg of ethanol solution of 2.5% hydrochloric acid, and performing acidolysis at 73 ℃ for 8 hours to obtain acidolysis solution; concentrating at 80 deg.C and 0.1 atm to 1/3 of acidolysis solution volume to obtain concentrated solution; adding 3.5 times of the volume of the concentrated solution into water for precipitation to obtain a precipitate;
(2) dissolving the precipitate with 3.5 times of anhydrous ethanol, performing hydrothermal reaction on 1g of sucrose fatty acid ester, 450g of silver acetate and 700g of water at 80 ℃ for 2h, and filtering;
(3) taking 1mol of the product obtained in the step 2, ultrasonically dispersing the product in an ethanol water solution, adding 10g of anhydrous sodium carbonate, 0.1mol of curcumin and 0.2mol of silver acetate, adjusting the pH value to 10 by using NaOH, and carrying out hydrothermal reaction at 80 ℃ for 2 hours;
(4) collecting precipitate, washing with ethanol, and vacuum drying at 80 deg.C for 3 hr to obtain tea flavone silver/silver oxide complex.
Example 2
Preparation of product with silver atom molar ratio of tea flavone silver to silver oxide being 20:1
Same as example 1 except that 0.05mol of silver acetate was added in step 3.
Example 3
Preparation of product with silver atom molar ratio of tea flavone silver to silver oxide of 10:1
Same as example 1 except that 0.1mol of silver acetate was added in step 3.
Comparative example 1
Same as example 1 except that 0.5mol of silver acetate was added in step 3.
Comparative example 2
Same as example 1 except that 0.01mol of silver acetate was added in step 3.
Comparative example 3
Same as example 1 except that curcumin was added in step 3 without adding a photosensitizer.
Comparative example 4
And (3) directly using the product obtained in the step (2) for testing.
Comparative example 5
The silver oxide is prepared by direct hydrothermal method for testing.
Light-controlled drug release experiment
The experimental method comprises the following steps: 2g of product was added to 50ml of pH 7.5 phosphate buffer and stirred at 50 rpm. 1mL of the buffer solution was sampled every 1 hour, and 1mL of phosphate buffer solution with pH 7.5 was added back until the reaction time was 12 hours. The samples were subjected to high performance liquid chromatography. Measuring the peak area of tea flavone, and calculating the cumulative release rate. The cumulative release rate of the product under 30W incandescent lamp irradiation was also determined.
The experimental results are as follows: the products prepared in examples 1, 2 and 3 release slowly in the absence of illumination, and release 90% cumulatively after 8-10 h, but release 90% cumulatively after illumination for 3-4 h, which indicates that the illumination accelerates the release of the drug. Comparative examples 3,4 had no significant acceleration effect.
Test of antibacterial Property
Activity test for inhibiting Erwinia carotovora
Toxicity testing was performed by the plate coating method. Selecting single colony of Erwinia carotovora preserved at 4 deg.C, inoculating in LB liquid culture medium, and culturing in a shaking water bath at 28 deg.C and 110rpm for 20 hr to obtain original bacterial liquid. Diluting the obtained original bacterial liquid with sterile water to 1.0 × 103CFU/ml, then 0.5ml of diluted bacteria liquid is added into 0.5ml of suspensions of products of examples and comparative examples which are irradiated by an incandescent lamp and ultrasonically treated for 30 minutes to prepare bacteria liquid with the bacteriostatic agent concentration of 0.0025g/L, and a sterile water control is set at the same time of the test. After the bacterial liquid was put in a dark shaking water bath at a constant temperature of 28 ℃ and sufficiently acted for 2 hours at 110rpm, 0.1ml of the bacterial liquid was sucked and added to a poured and solidified LB agar solid medium plate, and the plate was evenly smeared with a coating rod, and each treatment was repeated three times. The plate was placed upside down at 28 ℃ in the dark and cultured for 24 hours, and the number of colonies on each treatment plate was counted to calculate the inhibition (%) -at each concentration according to the following formula
| Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | Comparative example 5 | |
| Rate of inhibition of bacteria | 82% | 89% | 95% | 76% | 81% | 77% | 67% | 63%。 |
Claims (9)
1. The light-operated tea flavone silver/silver oxide nano preparation is characterized by comprising the following components in percentage by weight: a photosensitizer, a silver oxide and a tea flavone silver complex; the tea flavone silver complex is prepared by compounding tea flavone aglycone and silver, the silver oxide is obtained by thermal decomposition of silver hydroxide, and the photosensitizer is a natural traditional Chinese medicine photosensitizer; the nano particles are 60-100 nm, and the molar ratio of the tea flavone silver to the silver oxide silver atoms is 20:1-5: 1.
2. A preparation method of a light-operated tea flavone silver/silver oxide nano preparation is characterized by comprising the following steps: the method comprises the following steps:
1) carrying out acidolysis on tea flavonoids by using an ethanol solution of acid to obtain acidolysis solution; concentrating to obtain concentrated solution; precipitating the concentrated solution by adopting a precipitator to obtain a precipitate;
2) dissolving the precipitate, adding silver salt, emulsifier and water, adjusting pH to 7-8, carrying out hydrothermal reaction at 80 ℃ for 2 hours, filtering and washing;
3) dispersing the product obtained in the step 2 in an ethanol water solution, adding a photosensitizer, anhydrous sodium carbonate and a silver salt, adjusting the pH value to 10, and carrying out hydrothermal reaction at 80 ℃ for 2 hours;
4) standing for precipitation, washing and drying to obtain the light-operated tea flavone silver/silver oxide nano preparation.
3. The method for preparing the light-operated tea flavone silver/silver oxide nano preparation as claimed in claim 2, is characterized in that: in the step (1), the acid is more than one of hydrochloric acid, sulfuric acid or formic acid, and the mass concentration of the acid in ethanol solution of the acid is 2-5%; in the step (1), the acidolysis temperature is 70-80 ℃, and the acidolysis time is 5-8 hours.
4. The method for preparing the light-operated tea flavone silver/silver oxide nano preparation as claimed in claim 2, is characterized in that: in the step (2), the addition amount of the anhydrous sodium carbonate is 10-20% of the mass of the tea flavone.
5. The method for preparing the light-operated tea flavone silver/silver oxide nano preparation as claimed in claim 2, is characterized in that: the emulsifier is one or more of tween 60, polyoxyethylene stearate or sucrose fatty acid ester.
6. The method for preparing the light-operated tea flavone silver nano preparation as claimed in claim 2, is characterized in that: the traditional Chinese medicine photosensitizer is more than one of pheophorbide, curcumin or hypocrellin.
7. The method for preparing the light-operated tea flavone silver/silver oxide nano preparation as claimed in claim 2, is characterized in that: the adding amount of the emulsifier is 0.5-3% of the mass of the tea flavone silver complex, the using amount of the water is 5-10 times of the mass of the tea flavone silver complex, and the adding amount of the traditional Chinese medicine photosensitizer is 0.1-1% of the mass of the tea flavone silver complex.
8. The method for preparing the light-operated tea flavone silver/silver oxide nano preparation as claimed in claim 2, is characterized in that: the molar amount of silver salt added in step 3 is 5% -20% of the product of step 3 added.
9. The use of the light-operated tea flavone silver/silver oxide nano preparation as claimed in claim 1, wherein the nano preparation comprises the following components in percentage by weight: the light-operated tea flavone silver/silver oxide nano preparation is used as an efficient sterilization medicament.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111956817A (en) * | 2020-08-10 | 2020-11-20 | 武娟 | Indoor environment photodynamic broad spectrum sterilization and disinfection method |
| CN112403522A (en) * | 2020-11-12 | 2021-02-26 | 江南大学 | Mesoporous zirconium quercetin catalyst and application thereof in preparation of alpha, beta-unsaturated alcohol |
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| CN105461781A (en) * | 2015-12-17 | 2016-04-06 | 华南理工大学 | Tea sapogenin zinc complex and preparation method as well as use thereof |
| CN105535969A (en) * | 2015-12-17 | 2016-05-04 | 华南理工大学 | An optically-controlled tea flavone-zinc nanometer preparation, a preparing method thereof and uses of the nanometer preparation |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105461781A (en) * | 2015-12-17 | 2016-04-06 | 华南理工大学 | Tea sapogenin zinc complex and preparation method as well as use thereof |
| CN105535969A (en) * | 2015-12-17 | 2016-05-04 | 华南理工大学 | An optically-controlled tea flavone-zinc nanometer preparation, a preparing method thereof and uses of the nanometer preparation |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111956817A (en) * | 2020-08-10 | 2020-11-20 | 武娟 | Indoor environment photodynamic broad spectrum sterilization and disinfection method |
| CN112403522A (en) * | 2020-11-12 | 2021-02-26 | 江南大学 | Mesoporous zirconium quercetin catalyst and application thereof in preparation of alpha, beta-unsaturated alcohol |
| CN112403522B (en) * | 2020-11-12 | 2021-11-23 | 江南大学 | Mesoporous zirconium quercetin catalyst and application thereof in preparation of alpha, beta-unsaturated alcohol |
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