CN113579243B - Honeysuckle nanometer flower and preparation method and application thereof - Google Patents
Honeysuckle nanometer flower and preparation method and application thereof Download PDFInfo
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- CN113579243B CN113579243B CN202110608534.2A CN202110608534A CN113579243B CN 113579243 B CN113579243 B CN 113579243B CN 202110608534 A CN202110608534 A CN 202110608534A CN 113579243 B CN113579243 B CN 113579243B
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- honeysuckle
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- polylysine
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- 241000205585 Aquilegia canadensis Species 0.000 title claims abstract description 81
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 108010039918 Polylysine Proteins 0.000 claims abstract description 31
- 229920000656 polylysine Polymers 0.000 claims abstract description 31
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910052737 gold Inorganic materials 0.000 claims abstract description 21
- 239000010931 gold Substances 0.000 claims abstract description 21
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052709 silver Inorganic materials 0.000 claims abstract description 13
- 239000004332 silver Substances 0.000 claims abstract description 13
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 6
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 24
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 24
- 239000002245 particle Substances 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 229960005070 ascorbic acid Drugs 0.000 claims description 12
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 12
- 239000002253 acid Substances 0.000 claims description 11
- 239000002086 nanomaterial Substances 0.000 claims description 9
- 235000010323 ascorbic acid Nutrition 0.000 claims description 7
- 239000011668 ascorbic acid Substances 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 6
- FUSNOPLQVRUIIM-UHFFFAOYSA-N 4-amino-2-(4,4-dimethyl-2-oxoimidazolidin-1-yl)-n-[3-(trifluoromethyl)phenyl]pyrimidine-5-carboxamide Chemical compound O=C1NC(C)(C)CN1C(N=C1N)=NC=C1C(=O)NC1=CC=CC(C(F)(F)F)=C1 FUSNOPLQVRUIIM-UHFFFAOYSA-N 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
- 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 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 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
- WPEJSSRSFRWYJB-UHFFFAOYSA-K azanium;tetrachlorogold(1-) Chemical compound [NH4+].[Cl-].[Cl-].[Cl-].[Cl-].[Au+3] WPEJSSRSFRWYJB-UHFFFAOYSA-K 0.000 claims description 2
- 235000015165 citric acid Nutrition 0.000 claims description 2
- 239000012493 hydrazine sulfate Substances 0.000 claims description 2
- 229910000377 hydrazine sulfate Inorganic materials 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- 239000011591 potassium Substances 0.000 claims description 2
- CQLFBEKRDQMJLZ-UHFFFAOYSA-M silver acetate Chemical compound [Ag+].CC([O-])=O CQLFBEKRDQMJLZ-UHFFFAOYSA-M 0.000 claims description 2
- 229940071536 silver acetate Drugs 0.000 claims description 2
- 229940096017 silver fluoride Drugs 0.000 claims description 2
- REYHXKZHIMGNSE-UHFFFAOYSA-M silver monofluoride Chemical compound [F-].[Ag+] REYHXKZHIMGNSE-UHFFFAOYSA-M 0.000 claims description 2
- 229910000367 silver sulfate Inorganic materials 0.000 claims description 2
- YPNVIBVEFVRZPJ-UHFFFAOYSA-L silver sulfate Chemical compound [Ag+].[Ag+].[O-]S([O-])(=O)=O YPNVIBVEFVRZPJ-UHFFFAOYSA-L 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 239000011975 tartaric acid Substances 0.000 claims description 2
- 235000002906 tartaric acid Nutrition 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 14
- 238000001308 synthesis method Methods 0.000 abstract description 5
- 239000000126 substance Substances 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000005580 one pot reaction Methods 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 48
- 239000000047 product Substances 0.000 description 28
- 230000000052 comparative effect Effects 0.000 description 19
- 238000000862 absorption spectrum Methods 0.000 description 17
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 13
- 238000003756 stirring Methods 0.000 description 12
- 238000012360 testing method Methods 0.000 description 10
- 230000000694 effects Effects 0.000 description 9
- 238000002835 absorbance Methods 0.000 description 8
- 229910021642 ultra pure water Inorganic materials 0.000 description 8
- 239000012498 ultrapure water Substances 0.000 description 8
- 238000010521 absorption reaction Methods 0.000 description 7
- 230000003197 catalytic effect Effects 0.000 description 7
- 238000000034 method Methods 0.000 description 7
- 239000002057 nanoflower Substances 0.000 description 7
- 238000004627 transmission electron microscopy Methods 0.000 description 7
- 230000000844 anti-bacterial effect Effects 0.000 description 6
- YRNWIFYIFSBPAU-UHFFFAOYSA-N 4-[4-(dimethylamino)phenyl]-n,n-dimethylaniline Chemical compound C1=CC(N(C)C)=CC=C1C1=CC=C(N(C)C)C=C1 YRNWIFYIFSBPAU-UHFFFAOYSA-N 0.000 description 5
- 102000004190 Enzymes Human genes 0.000 description 5
- 108090000790 Enzymes Proteins 0.000 description 5
- 239000002211 L-ascorbic acid Substances 0.000 description 5
- 235000000069 L-ascorbic acid Nutrition 0.000 description 5
- 102000006833 Multifunctional Enzymes Human genes 0.000 description 5
- 108010047290 Multifunctional Enzymes Proteins 0.000 description 5
- 238000004090 dissolution Methods 0.000 description 5
- 238000011160 research Methods 0.000 description 5
- 239000012085 test solution Substances 0.000 description 5
- 230000000259 anti-tumor effect Effects 0.000 description 4
- 239000003937 drug carrier Substances 0.000 description 4
- 238000007789 sealing Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 239000003446 ligand Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000007974 sodium acetate buffer Substances 0.000 description 3
- BHZOKUMUHVTPBX-UHFFFAOYSA-M sodium acetic acid acetate Chemical compound [Na+].CC(O)=O.CC([O-])=O BHZOKUMUHVTPBX-UHFFFAOYSA-M 0.000 description 3
- 238000006467 substitution reaction Methods 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000006073 displacement reaction Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000003381 stabilizer Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 101710134784 Agnoprotein Proteins 0.000 description 1
- 240000006829 Ficus sundaica Species 0.000 description 1
- 241000628997 Flos Species 0.000 description 1
- 244000269722 Thea sinensis Species 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012984 biological imaging Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000003593 chromogenic compound Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- RAABOESOVLLHRU-UHFFFAOYSA-N diazene Chemical compound N=N RAABOESOVLLHRU-UHFFFAOYSA-N 0.000 description 1
- 229910000071 diazene Inorganic materials 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005669 field effect Effects 0.000 description 1
- PQTCMBYFWMFIGM-UHFFFAOYSA-N gold silver Chemical compound [Ag].[Au] PQTCMBYFWMFIGM-UHFFFAOYSA-N 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000002500 ions Chemical group 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000007626 photothermal therapy Methods 0.000 description 1
- 229920001184 polypeptide Polymers 0.000 description 1
- 150000008442 polyphenolic compounds Chemical class 0.000 description 1
- 235000013824 polyphenols Nutrition 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 108090000765 processed proteins & peptides Proteins 0.000 description 1
- 102000004196 processed proteins & peptides Human genes 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 229940083025 silver preparation Drugs 0.000 description 1
- 238000002198 surface plasmon resonance spectroscopy Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- XYYVDQWGDNRQDA-UHFFFAOYSA-K trichlorogold;trihydrate;hydrochloride Chemical compound O.O.O.Cl.Cl[Au](Cl)Cl XYYVDQWGDNRQDA-UHFFFAOYSA-K 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- 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
- A61K41/0052—Thermotherapy; Hyperthermia; Magnetic induction; Induction heating therapy
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
- A61K47/34—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polyesters, polyamino acids, polysiloxanes, polyphosphazines, copolymers of polyalkylene glycol or poloxamers
-
- 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
-
- 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
- A61P31/10—Antimycotics
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P35/00—Antineoplastic agents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y15/00—Nanotechnology for interacting, sensing or actuating, e.g. quantum dots as markers in protein assays or molecular motors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y5/00—Nanobiotechnology or nanomedicine, e.g. protein engineering or drug delivery
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3577—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing liquids, e.g. polluted water
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/359—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using near infrared light
-
- 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
Abstract
The invention discloses a honeysuckle nanometer flower and a preparation method and application thereof. The preparation method of the honeysuckle nanometer material coated by polylysine comprises the following steps: and mixing polylysine with a gold source, and then sequentially mixing and reacting with a silver source and a reducing agent to obtain the honeysuckle nanometer. The invention can obtain the honeysuckle material with good biocompatibility and high physical and chemical stability by a one-pot green synthesis method. The synthesis method has the advantages of simple steps, green and safe, high efficiency and rapidness, and mass production.
Description
Technical Field
The invention belongs to the technical field of composite nano particle preparation, and particularly relates to a honeysuckle flower and a preparation method and application thereof.
Background
Nanomaterials have unique optical, thermal, electrical, etc. properties and have been widely used in various fields, for example: sensors, photoelectric materials, photothermal therapy, biological imaging, etc. Research shows that the performance of the nano material is greatly dependent on the morphology, structure, size and composition of the material, so that the research on the nano material with a special morphology structure has important significance. Among them, noble metal nano-materials are favored by scientists because of tunable localized surface plasmon resonance effect. The special morphology of the gold nano material with anisotropy often has a field effect of a tip or a gap in particles, so that the plasma resonance absorption peak is red shifted to near infrared to generate a photo-thermal effect, and the gold nano material with anisotropy can be applied to researches such as photo-thermal anti-tumor, photo-thermal bacteriostasis, photo-thermal sensing and the like.
The gold nano-flower is a gold nano-material with a branched structure morphology, and the problems of complicated steps, harsh conditions, subsequent modification, requirement of a surfactant as a crystal face sealing agent and a stabilizing agent and the like generally exist in the synthesis at present, so that the wide application of the gold nano-material is further limited. Patent application CN110227816a discloses a gold-silver nanoflower with a core-shell structure and a preparation method thereof, wherein the preparation method needs to prepare inner core nano silver by reducing silver nitrate by introducing tea polyphenol, and then realizes the growth of branches of the nanoflower by displacement reaction between chloroauric acid and silver. The method has complicated steps, needs the steps of nano silver preparation, centrifugal washing and impurity removal, substitution reaction induced branch growth and the like, and has safety risks due to the high-temperature high-power requirement of the high-temperature microwave method. In addition, the displacement reaction between chloroauric acid and silver often requires longer reaction time, and the morphology and uniformity of the branches are not easily and accurately regulated. The surface of the honeysuckle prepared by the method is not protected by a biocompatible ligand, and often has unstable physical and chemical properties and larger biotoxicity, so that the biocompatible ligand needs to be modified on the surface of the honeysuckle before the honeysuckle is applied to a cell experiment, and the biocompatibility and stability of a synthetic material can be ensured. However, this step of modifying the biocompatible ligand may require the introduction of various organic reagents, centrifugal washing, which would destroy the physiological stability of the material. Patent application CN110605383A discloses a gold nano needle cluster material and a preparation method thereof, the steps of the synthesis method are complicated, heating conditions are needed in the preparation process, and the prepared gold nano needle cluster material has larger particle size, so that the popularization and application of the material are not facilitated. Therefore, it is necessary to provide a physicochemical stable honeysuckle flower which is simple to prepare, green and safe and can be synthesized in a large scale.
Disclosure of Invention
In order to overcome the problems of the prior art, one of the purposes of the present invention is to provide a honeysuckle nanometer flower; the second purpose of the invention is to provide a preparation method of the honeysuckle; the invention further aims to provide an application of the honeysuckle nanometer.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the first aspect of the invention provides a honeysuckle nanometer material coated by polylysine.
Preferably, the particle size of the honeysuckle is 80nm-250nm.
According to a second aspect of the invention, there is provided a method for preparing a honeysuckle flower according to the first aspect of the invention, comprising the steps of:
and mixing polylysine with a gold source, and then sequentially mixing and reacting with a silver source and a reducing agent to obtain the honeysuckle nanometer.
Preferably, in the preparation method of the honeysuckle, the reaction temperature is 20-30 ℃; further preferably, the reaction temperature is room temperature (25 ℃).
Preferably, in the preparation method of the honeysuckle, the polylysine and the gold source are mixed with the silver source and then mixed with the reducing agent for reaction within 45 seconds.
Preferably, in the preparation method of the honeysuckle nanometer flower, the polylysine has the mass concentration of 4 multiplied by 10 - 4 wt％-6×10 -4 An aqueous solution of polylysine in wt%; further preferably, the polylysine has a mass concentration of 5×10 -4 An aqueous solution of polylysine in wt%.
Preferably, in the preparation method of the honeysuckle, the mass ratio of the polylysine to the gold source is (0.03-0.1): 1, a step of; further preferably, the mass ratio of the polylysine to the gold source is (0.05-0.08): 1.
preferably, in the preparation method of the honeysuckle, the molar ratio of the silver source to the gold source is 1 (9-15); further preferably, the molar ratio of the silver source to the gold source is 1 (11-13).
Preferably, in the preparation method of the honeysuckle, the silver source comprises at least one of silver nitrate, silver fluoride, silver sulfate and silver acetate; further preferably, the silver source comprises silver nitrate.
Preferably, in the preparation method of the honeysuckle nanometer flower, the gold source comprises at least one of chloroauric acid, potassium chloroaurate, sodium chloroaurate and ammonium chloroaurate; further preferably, the gold source comprises chloroauric acid.
Preferably, in the preparation method of the honeysuckle, the reducing agent comprises at least one of citric acid, ascorbic acid, tartaric acid and hydrazine sulfate; further preferably, the reducing agent comprises ascorbic acid.
A third aspect of the present invention provides the use of a honeysuckle flower according to the first aspect of the present invention in the photo-thermal and/or biomedical fields.
Preferably, in the application, the photo-thermal field includes photo-thermal anti-tumor, photo-thermal bacteriostasis or photo-thermal sensing.
Preferably, in said application, the biomedical field comprises a pharmaceutical carrier or a nanoenzyme.
The beneficial effects of the invention are as follows:
the invention can obtain the honeysuckle material with good biocompatibility and high physical and chemical stability by a one-pot green synthesis method. The synthesis method has the advantages of simple steps, green and safe, high efficiency and rapidness, and mass production.
In particular, the invention has the following advantages:
1. according to the invention, polylysine is introduced as a crystal face sealing agent and a stabilizing agent of the honeysuckle, so that uniform growth of a branch structure of the honeysuckle is accurately controlled, and the preparation of the honeysuckle with controllable morphology, uniform particle size, high biological safety and stable physicochemical property is realized.
2. The preparation method of the honeysuckle nanometer flower is completed by a one-pot method, and has the advantages of simple preparation steps, green, safe, high efficiency, high speed and mass production.
3. The surface of the honeysuckle prepared by the invention is coated by polylysine, and the polylysine is a polypeptide with good biocompatibility, antibacterial property and rich cations, so that the honeysuckle material has good biological safety, antibacterial property, biological membrane penetrability, excellent drug carrier and other properties. In addition, the honeysuckle prepared by the invention has higher nano enzyme catalytic activity and near infrared absorption characteristic, so that the honeysuckle has important functions in photo-thermal anti-tumor, photo-thermal bacteriostasis, photo-thermal sensing, drug carriers or nano enzymes.
Drawings
Fig. 1 is a scanning image of a honeysuckle flower by transmission electron microscopy prepared in example 1.
Fig. 2 is a scanning image of a single honeysuckle flower by transmission electron microscopy prepared in example 1.
Fig. 3 is an ultraviolet-visible-near infrared absorption spectrum of the honeysuckle flower prepared in example 1.
FIG. 4 is a graph showing the absorption spectrum of the honeysuckle flower p-tetramethyl benzidine by catalytic oxidation, which is prepared in example 1.
Fig. 5 is a photo-thermal effect diagram of the honeysuckle prepared in example 1.
FIG. 6 is an ultraviolet-visible-near infrared absorption spectrum of the product prepared in comparative example 1.
FIG. 7 is a scanning image of the product of comparative example 3 by transmission electron microscopy.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Specific implementations of the invention are further described below with reference to the drawings and examples, but the implementation and protection of the invention are not limited thereto. It should be noted that the following processes, if not specifically described in detail, can be realized or understood by those skilled in the art with reference to the prior art. The reagents or instruments used did not identify the manufacturer and were considered conventional products available commercially.
0.4g of polylysine ((C) was weighed out 6 H 12 N 2 O) n Molecular weight less than 5000) powder is added into 40mL of ultrapure water, and is dissolved by ultrasonic to obtain 1.0wt% polylysine solution for standby; adding 4mL of the 1.0wt% polylysine solution into 36mL of ultrapure water, and performing ultrasonic dissolution to obtain 0.1wt% polylysine solution for later use; adding 4mL of the 0.1wt% polylysine solution into 36mL of ultrapure water, and performing ultrasonic dissolution to obtain 0.01wt% polylysine solution for later use; 0.0102g of silver nitrate (AgNO) 3 ) Adding the particles into 10mL of ultrapure water, and performing ultrasonic dissolution to obtain a silver nitrate solution with the concentration of 6mmol/L for later use; 0.176g of ascorbic acid (C) 6 H 8 O 6 ) Adding the powder into 10mL of ultrapure water, and performing ultrasonic dissolution to obtain 0.1mol/L ascorbic acid solution for later use; 1g of chloroauric acid trihydrate (HAuCl) was weighed out 4 ·3H 2 And O) adding the powder into 80mL of deionized water, and performing ultrasonic dissolution to obtain 1wt% chloroauric acid solution for later use.
The examples and comparative examples in the following sections were completed at room temperature unless otherwise specified.
Example 1
Taking 50 mu L of 0.1wt% polylysine solution, stirring for 2min at room temperature in a glass reaction bottle containing 10mL of ultrapure water, adding 75 mu L of 1wt% chloroauric acid solution, continuously stirring for 2min, adding 30 mu L of 6mmol/L silver nitrate solution, adding 40 mu L of 0.1mol/L ascorbic acid solution in 45s, observing that the solution turns into blue from colorless rapidly, and stopping stirring after the reaction is continued for 10min, thus obtaining the product prepared in the embodiment.
The product prepared in this example was subjected to transmission electron microscopy, fig. 1 is a transmission electron microscopy scan of the honeysuckle prepared in example 1, and fig. 2 is a transmission electron microscopy scan of a single honeysuckle prepared in example 1. From fig. 1 and fig. 2, it can be seen that the product prepared in this embodiment is the target honeysuckle, and the honeysuckle has full particles, uniform morphology and particle size, and particle size distribution in the range of 80nm-250nm.
The honeysuckle prepared in the embodiment is subjected to ultraviolet-visible light-near infrared absorption spectrum test, and the preparation process of an absorption spectrum test solution sample is as follows:
and placing a 96-well plate containing 200 mu L of the honeysuckle solution in a multifunctional enzyme-labeled instrument, setting the wavelength range to 300-900 nm and the bandwidth to 3.5nm, and then carrying out ultraviolet absorption spectrum test.
Fig. 3 is an ultraviolet-visible-near infrared absorption spectrum of the honeysuckle flower prepared in example 1. The figure shows that the honeysuckle prepared by the embodiment has strong optical absorption at the wavelength of 600-800 nm, which indicates that the material can efficiently absorb near infrared light under the radiation of near infrared light, and has the characteristic of converting light energy into heat energy.
Tetramethyl benzidine (TMB) is a green, safe and most common chromogenic substrate used as a nano enzyme catalytic hydrogen peroxide system at present, and has high sensitivity, high color purity and good stability of oxidation products. By researching the catalytic color reaction of the honeysuckle on the tetramethyl benzidine substrate in the presence of hydrogen peroxide, the honeysuckle can be proved to have good nano-enzyme characteristics. Based on the nano enzyme characteristic of the honeysuckle, hydrogen peroxide can be catalyzed to generate active free radicals, so that antibacterial research is performed. The absorption spectrum experiment is carried out on the catalytic effect of the honeysuckle (NPs) prepared in the embodiment on the substrate Tetramethylbenzidine (TMB), and the preparation process of the absorption spectrum test solution sample is as follows:
1)TMB+H 2 O 2 +nps absorbance test method: 870 mu L of acetic acid-sodium acetate buffer solution with pH=4.5 is taken in 1.5mL of EP plastic tube, 100 mu L of 0.1mol/L hydrogen peroxide solution, 10 mu L of 5mmol/L TMB solution and 20 mu L of honeysuckle Solution (NPs) are added, and the mixture is stirred and mixed at room temperature for 30s200 mu L of the sample is put into a 96-well plate, and ultraviolet absorption spectrum measurement is carried out by utilizing a multifunctional enzyme-labeled instrument, wherein the test condition is 400-800 nm, and the bandwidth is 3.5nm.
2) TMB+NPs absorbance test method: 870 mu L of acetic acid-sodium acetate buffer solution with pH=4.5 is taken to be placed in an EP plastic tube with 1.5mL, then 10 mu L of 5mmol/L TMB solution and 20 mu L of honeysuckle Solution (NPs) are added, vortex and mix evenly at room temperature for 30s, then 200 mu L of the mixture is taken to be placed in a 96-well plate, and ultraviolet absorption spectrum measurement is carried out by a multifunctional enzyme-labeled instrument under the test conditions of 400-800 nm and the bandwidth of 3.5nm.
3)TMB+H 2 O 2 Absorbance testing method: 870 mu L of acetic acid-sodium acetate buffer solution with pH=4.5 is taken to be placed in an EP plastic tube with 1.5mL, then 100 mu L of 0.1mol/L hydrogen peroxide solution and 10 mu L of 5mmol/L TMB solution are added, vortex and mix for 30s at room temperature, then 200 mu L of the mixture is taken to be placed in a 96-well plate, and ultraviolet absorption spectrum measurement is carried out by utilizing a multifunctional enzyme-labeled instrument, wherein the test condition is 400-800 nm, and the bandwidth is 3.5nm.
FIG. 4 is a graph showing the absorption spectrum of the honeysuckle flower of example 1 to tetramethyl benzidine by catalytic oxidation. Wherein the abscissa is the wavelength of light and the ordinate is the absorbance intensity of the reaction system. Comparing the curves in the graph, it can be found that when only the honeysuckle (NPs) and TMB prepared in the embodiment exist in the system, no absorption peak exists at 652nm, which indicates that the absorbance of the honeysuckle (NPs) does not interfere with the experiment. When TMB and hydrogen peroxide (H) 2 O 2 ) When present, oxidized TMB has a very weak absorbance at 652nm, which is essentially negligible. However, when TMB, hydrogen peroxide (H 2 O 2 ) And honeysuckle flowers (NPs) are simultaneously present, the absorbance of the test solution at 652nm is obviously enhanced. The method shows that the honeysuckle can rapidly catalyze and oxidize tetramethyl benzidine in the presence of an oxidant to generate a charge-transfer complex formed by blue electron oxide TMB positive ion groups, parent TMB and TMB diimine, and the charge-transfer complex has strong absorbance at 652 nm. Fig. 4 illustrates that the honeysuckle prepared in this embodiment has the catalytic property of nano-enzyme, and can utilize the nano-enzyme property to perform antibacterial study under the action of low-concentration hydrogen peroxide.
The honeysuckle prepared in the embodiment is subjected to photo-thermal effect test under the condition of laser irradiation, and the preparation process of the test solution sample is as follows:
respectively placing 1mL of 50ppm flos Lonicerae solution and pure water in cuvette, and placing in 808nm near infrared laser (power density of 0.45W/cm) 2 ) The temperature of the solution was recorded every 30s by irradiating for 15 min.
Fig. 5 is a photo-thermal effect diagram of the honeysuckle prepared in example 1. In the figure, the abscissa indicates the laser irradiation time of 808nm, and the ordinate indicates the temperature of the irradiated material under laser irradiation. It can be seen from the graph that the temperature of pure water hardly increases under laser irradiation, and the temperature increases by about 1 ℃ at 900 s; the temperature of the honeysuckle material rises rapidly along with the irradiation time, and the temperature can reach 38.6 ℃ at 900 s. Fig. 5 illustrates that the honeysuckle prepared in this embodiment has a good photo-thermal effect and can be used for near infrared photo-thermal antibacterial research.
The honeysuckle prepared by the embodiment has good water solubility and good physical and chemical stability. The product prepared in this example was stored under sealed conditions at room temperature for 3 months without agglomeration and precipitation.
Based on the photo-thermal effect and the enzyme catalysis test result, the honeysuckle provided by the embodiment can be applied to preparing photo-thermal anti-tumor products, photo-thermal antibacterial products, photo-thermal sensing products, drug carrier products or nano-enzyme products.
Comparative example 1
Taking 50 mu L of 1.0wt% polylysine solution, stirring for 2min at room temperature in a glass reaction bottle containing 10mL of ultrapure water, adding 75 mu L of 1wt% chloroauric acid solution, continuously stirring for 2min, adding 30 mu L of 6mmol/L silver nitrate solution, adding 40 mu L of 0.1mol/L ascorbic acid solution in 45s, observing that the solution is rapidly changed from colorless to blue-green, and stopping stirring after the reaction is continued for 10min, thus obtaining the product prepared in the comparative example.
The honeysuckle prepared in the comparative example is subjected to ultraviolet-visible light-near infrared absorption spectrum test, and the preparation process of an absorption spectrum test solution sample is as follows:
the 96-well plate containing 200 mu L of the honeysuckle solution prepared in the comparative example is placed in a multifunctional enzyme-labeled instrument, the wavelength range is set to 300-900 nm, the bandwidth is 3.5nm, and then ultraviolet absorption spectrum test is carried out.
FIG. 6 is an ultraviolet-visible-near infrared absorption spectrum of the product prepared in comparative example 1. As is clear from FIG. 6, the maximum absorption peak of the product prepared in this comparative example was 587nm, and the maximum absorption peak was blue-shifted and the absorption intensity was decreased as compared with example 1. The product prepared in this comparative example had poor ability to absorb near infrared light, indicating that its particle size was smaller and the photothermal effect was also correspondingly poor. The reason is that the concentration of the polylysine is increased due to the crystal face sealing effect, so that the polylysine can better prevent the product nanoflower from further growing, and the particle size of the product is kept in a smaller range.
The product prepared in the comparative example is stored for 3 months under the condition of room temperature in a sealing way, and no agglomeration and precipitation phenomenon occur.
Comparative example 2
Taking 50 mu L of 0.01wt% polylysine solution, stirring for 2min at room temperature in a glass reaction bottle containing 10mL of ultrapure water, adding 75 mu L of 1wt% chloroauric acid solution, continuously stirring for 2min, adding 30 mu L of 6mmol/L silver nitrate solution, adding 40 mu L of 0.1mol/L ascorbic acid solution in 45s, observing that the solution is rapidly changed from colorless to light blue, and stopping stirring after the reaction is continued for 10min, thus obtaining the product prepared in the comparative example.
And (3) hermetically storing the product prepared in the comparative example for 24 hours at room temperature, and observing the agglomeration and layering phenomena of the original homogeneous phase solution, wherein the product is agglomerated at the bottom of the solution. This demonstrates that the product prepared in this comparative example has a larger particle size and is unstable and agglomerated due to gravity. The reason is that when the dosage of polylysine is small, the polylysine cannot provide sufficient surface hydrophilic groups for the honeysuckle particles, and the honeysuckle particles further grow to reduce the specific surface area in order to maintain stability, so that the product has poor monodispersity and even precipitates.
Comparative example 3
Taking 50 mu L of 0.1wt% polylysine solution, stirring for 2min at room temperature, adding 75 mu L of 1wt% chloroauric acid solution, continuously stirring for 2min, adding 30 mu L of 6mmol/L silver nitrate solution, stirring for 5min, adding 40 mu L of 0.1mol/L ascorbic acid solution, observing that the solution turns from colorless to purple, continuously reacting for 10min, starting to turn the solution into reddish color, and finally turning the reaction into purplish red, thus obtaining the product prepared in the comparative example.
FIG. 7 is a scanning image of the product of comparative example 3 by transmission electron microscopy. From fig. 7, it is clear that the morphology of the product obtained under this condition is not nanoflower. The possible reason is that the formation of nanoflower is determined by the combination of electrical substitution and ascorbic acid reduction, and in this comparative example, the silver nitrate solution and the ascorbic acid solution are added separately and sequentially at intervals of 5 minutes, so that the chloroauric acid solution firstly reacts with the silver nitrate solution and finally reacts with the ascorbic acid solution, and uniform spherical nanoflower particles cannot be generated.
The foregoing examples are illustrative of the present invention and are not intended to be limiting, and other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principles of the invention are intended to be equivalent in scope.
Claims (6)
1. The utility model provides a honeysuckle, its characterized in that: the honeysuckle is a gold and silver nano material coated by polylysine;
the preparation method of the honeysuckle nanometer flower comprises the following steps:
mixing polylysine with a gold source and a silver source, and then mixing the mixture with a reducing agent for reaction within 45 seconds to obtain the honeysuckle;
the mass ratio of the polylysine to the gold source is (0.05-0.08): 1, a step of;
the molar ratio of the silver source to the gold source is 1: (9-15);
the reaction temperature is 20-30 ℃.
2. The honeysuckle flower according to claim 1, wherein: the particle size of the honeysuckle is 80nm-250nm.
3. The honeysuckle flower according to claim 1, wherein: the silver source comprises at least one of silver nitrate, silver fluoride, silver sulfate and silver acetate.
4. The honeysuckle flower according to claim 1, wherein: the gold source comprises at least one of chloroauric acid, potassium chloroaurate, sodium chloroaurate and ammonium chloroaurate.
5. The honeysuckle flower according to claim 1, wherein: the reducing agent comprises at least one of citric acid, ascorbic acid, tartaric acid and hydrazine sulfate.
6. Use of the honeysuckle flower according to any one of claims 1-5 in the photo-thermal and/or biomedical fields.
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