CN109620957A - The mesoporous silicon oxide of load indocyanine green superscribes the preparation method of conversion nano particle - Google Patents
The mesoporous silicon oxide of load indocyanine green superscribes the preparation method of conversion nano particle Download PDFInfo
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- CN109620957A CN109620957A CN201910053358.3A CN201910053358A CN109620957A CN 109620957 A CN109620957 A CN 109620957A CN 201910053358 A CN201910053358 A CN 201910053358A CN 109620957 A CN109620957 A CN 109620957A
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- nano particle
- silicon oxide
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- mesoporous silicon
- indocyanine green
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- MOFVSTNWEDAEEK-UHFFFAOYSA-M indocyanine green Chemical compound [Na+].[O-]S(=O)(=O)CCCCN1C2=CC=C3C=CC=CC3=C2C(C)(C)C1=CC=CC=CC=CC1=[N+](CCCCS([O-])(=O)=O)C2=CC=C(C=CC=C3)C3=C2C1(C)C MOFVSTNWEDAEEK-UHFFFAOYSA-M 0.000 title claims abstract description 61
- 229960004657 indocyanine green Drugs 0.000 title claims abstract description 61
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 55
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 53
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 229910052814 silicon oxide Inorganic materials 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- 239000002245 particle Substances 0.000 claims abstract description 12
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 63
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 32
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 25
- 239000000243 solution Substances 0.000 claims description 25
- 238000003756 stirring Methods 0.000 claims description 25
- 238000000034 method Methods 0.000 claims description 23
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 21
- 239000008367 deionised water Substances 0.000 claims description 21
- 238000005119 centrifugation Methods 0.000 claims description 20
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 claims description 20
- 229910021641 deionized water Inorganic materials 0.000 claims description 18
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 18
- 235000019441 ethanol Nutrition 0.000 claims description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 14
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 13
- 238000013019 agitation Methods 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 12
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 11
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 11
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 11
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 11
- 239000005642 Oleic acid Substances 0.000 claims description 11
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 11
- 238000010792 warming Methods 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 10
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- -1 octadecylene Chemical group 0.000 claims description 9
- 239000011775 sodium fluoride Substances 0.000 claims description 9
- 235000013024 sodium fluoride Nutrition 0.000 claims description 9
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 8
- 230000001376 precipitating effect Effects 0.000 claims description 8
- 239000012153 distilled water Substances 0.000 claims description 7
- 238000005530 etching Methods 0.000 claims description 7
- DKAGJZJALZXOOV-UHFFFAOYSA-N hydrate;hydrochloride Chemical compound O.Cl DKAGJZJALZXOOV-UHFFFAOYSA-N 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 6
- JKXCZYCVHPKTPK-UHFFFAOYSA-N hydrate;trihydrochloride Chemical compound O.Cl.Cl.Cl JKXCZYCVHPKTPK-UHFFFAOYSA-N 0.000 claims description 6
- 238000009835 boiling Methods 0.000 claims description 5
- 238000000605 extraction Methods 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 4
- 239000000908 ammonium hydroxide Substances 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 239000000284 extract Substances 0.000 claims description 4
- 238000011068 loading method Methods 0.000 claims description 4
- 239000011780 sodium chloride Substances 0.000 claims description 4
- 239000004094 surface-active agent Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 240000007594 Oryza sativa Species 0.000 claims description 2
- 235000007164 Oryza sativa Nutrition 0.000 claims description 2
- 235000013339 cereals Nutrition 0.000 claims description 2
- 238000003760 magnetic stirring Methods 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 235000009566 rice Nutrition 0.000 claims description 2
- 125000005211 alkyl trimethyl ammonium group Chemical group 0.000 claims 1
- SLIYDTRIAATWQR-UHFFFAOYSA-K trichlorothulium;hydrate Chemical compound O.Cl[Tm](Cl)Cl SLIYDTRIAATWQR-UHFFFAOYSA-K 0.000 claims 1
- 230000004083 survival effect Effects 0.000 abstract description 4
- 239000000377 silicon dioxide Substances 0.000 abstract description 3
- 206010057249 Phagocytosis Diseases 0.000 abstract description 2
- 230000008782 phagocytosis Effects 0.000 abstract description 2
- 238000007334 copolymerization reaction Methods 0.000 abstract 1
- 210000004027 cell Anatomy 0.000 description 20
- 239000000047 product Substances 0.000 description 16
- 239000001963 growth medium Substances 0.000 description 8
- PITRRWWILGYENJ-UHFFFAOYSA-N 2-[2-[2-[2-[2-(4-nonylphenoxy)ethoxy]ethoxy]ethoxy]ethoxy]ethanol Chemical compound CCCCCCCCCC1=CC=C(OCCOCCOCCOCCOCCO)C=C1 PITRRWWILGYENJ-UHFFFAOYSA-N 0.000 description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 6
- 239000006144 Dulbecco’s modified Eagle's medium Substances 0.000 description 6
- 229910052681 coesite Inorganic materials 0.000 description 6
- 229910052906 cristobalite Inorganic materials 0.000 description 6
- 210000002966 serum Anatomy 0.000 description 6
- 229910052682 stishovite Inorganic materials 0.000 description 6
- 229910052905 tridymite Inorganic materials 0.000 description 6
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 4
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 3
- 229910021529 ammonia Inorganic materials 0.000 description 3
- 230000022534 cell killing Effects 0.000 description 3
- 238000001727 in vivo Methods 0.000 description 3
- 239000004530 micro-emulsion Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- ILOTUXNTERMOJL-UHFFFAOYSA-K thulium(iii) chloride Chemical compound Cl[Tm](Cl)Cl ILOTUXNTERMOJL-UHFFFAOYSA-K 0.000 description 3
- CKLHRQNQYIJFFX-UHFFFAOYSA-K ytterbium(III) chloride Chemical class [Cl-].[Cl-].[Cl-].[Yb+3] CKLHRQNQYIJFFX-UHFFFAOYSA-K 0.000 description 3
- 229910052775 Thulium Inorganic materials 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000002242 deionisation method Methods 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- DCAYPVUWAIABOU-UHFFFAOYSA-N hexadecane Chemical compound CCCCCCCCCCCCCCCC DCAYPVUWAIABOU-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002090 nanochannel Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- FRNOGLGSGLTDKL-UHFFFAOYSA-N thulium atom Chemical compound [Tm] FRNOGLGSGLTDKL-UHFFFAOYSA-N 0.000 description 2
- 230000001988 toxicity Effects 0.000 description 2
- 231100000419 toxicity Toxicity 0.000 description 2
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- AZKSAVLVSZKNRD-UHFFFAOYSA-M 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide Chemical compound [Br-].S1C(C)=C(C)N=C1[N+]1=NC(C=2C=CC=CC=2)=NN1C1=CC=CC=C1 AZKSAVLVSZKNRD-UHFFFAOYSA-M 0.000 description 1
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 238000002965 ELISA Methods 0.000 description 1
- 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 description 1
- 102000004895 Lipoproteins Human genes 0.000 description 1
- 108090001030 Lipoproteins Proteins 0.000 description 1
- 238000004497 NIR spectroscopy Methods 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 238000013096 assay test Methods 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000007541 cellular toxicity Effects 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 230000009514 concussion Effects 0.000 description 1
- 238000004624 confocal microscopy Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007850 fluorescent dye Substances 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 238000001782 photodegradation Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000000700 radioactive tracer Substances 0.000 description 1
- 239000012744 reinforcing agent Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 238000007619 statistical method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000002560 therapeutic procedure Methods 0.000 description 1
- 210000004881 tumor cell Anatomy 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
- A61K41/0052—Thermotherapy; Hyperthermia; Magnetic induction; Induction heating therapy
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K49/00—Preparations for testing in vivo
- A61K49/001—Preparation for luminescence or biological staining
- A61K49/0013—Luminescence
- A61K49/0017—Fluorescence in vivo
- A61K49/0019—Fluorescence in vivo characterised by the fluorescent group, e.g. oligomeric, polymeric or dendritic molecules
- A61K49/0021—Fluorescence in vivo characterised by the fluorescent group, e.g. oligomeric, polymeric or dendritic molecules the fluorescent group being a small organic molecule
- A61K49/0032—Methine dyes, e.g. cyanine dyes
- A61K49/0034—Indocyanine green, i.e. ICG, cardiogreen
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K49/00—Preparations for testing in vivo
- A61K49/001—Preparation for luminescence or biological staining
- A61K49/0063—Preparation for luminescence or biological staining characterised by a special physical or galenical form, e.g. emulsions, microspheres
- A61K49/0069—Preparation for luminescence or biological staining characterised by a special physical or galenical form, e.g. emulsions, microspheres the agent being in a particular physical galenical form
- A61K49/0089—Particulate, powder, adsorbate, bead, sphere
- A61K49/0091—Microparticle, microcapsule, microbubble, microsphere, microbead, i.e. having a size or diameter higher or equal to 1 micrometer
- A61K49/0093—Nanoparticle, nanocapsule, nanobubble, nanosphere, nanobead, i.e. having a size or diameter smaller than 1 micrometer, e.g. polymeric nanoparticle
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
- A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
- A61K9/51—Nanocapsules; Nanoparticles
- A61K9/5107—Excipients; Inactive ingredients
- A61K9/5115—Inorganic compounds
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P35/00—Antineoplastic agents
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- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Public Health (AREA)
- Engineering & Computer Science (AREA)
- Veterinary Medicine (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Epidemiology (AREA)
- Pharmacology & Pharmacy (AREA)
- Medicinal Chemistry (AREA)
- Biomedical Technology (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Nanotechnology (AREA)
- Optics & Photonics (AREA)
- Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Organic Chemistry (AREA)
- Luminescent Compositions (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
- Silicon Compounds (AREA)
Abstract
The mesoporous silicon oxide that the present invention provides a kind of load indocyanine green superscribes the preparation method of conversion nano particle, is converted with being situated between in empty coated with silica, increases the biological safety of particle and the load capacity of indocyanine green.The mesoporous silicon oxide of load indocyanine green prepared by the present invention superscribes the partial size of conversion nano particle between 80-400 nanometers；The mesoporous silicon oxide that load indocyanine green (ICG) is added superscribes the survival rate of cell after conversion nano particle within the scope of 85-95%；The burnt microscope of copolymerization is observed that the phagocytosis of particle in the cell；The cell mortality of particle is added in 40-75% range in laser irradiation.
Description
Technical field
The invention belongs to biotechnologys and pharmaceutical technology field, and in particular to a kind of to load the mesoporous of indocyanine green (ICG)
The preparation method of conversion nano particle on Silica-coated.
Background technique
Indocyanine green (ICG) is that one kind has stronger absorption near infrared spectral range, small toxicity, is not involved in vivo biodistribution
It converts, drain rapid fluorescent dye, be the near-infrared spectroscopy comparison of the currently the only clinical use being approved by the FDA in the United States
Reinforcing agent.ICG can also be used for optical dynamic therapy simultaneously, under near infrared light, using its high fluorescence efficiency, in relatively low-dose
When optionally kill tumor tissues.However the water unstable of ICG, photodegradation, thermal degradation and it is easy to and lipoprotein
In conjunction with the disadvantages of quickly being removed in vivo is caused, its application in PDT oncotherapy is limited.
Up-conversion nano material has good chemical stability, photostability.It can hold under the irradiation of near infrared light
Continue it is stable shine, and the light of long wavelength can be converted to the light of short wavelength, biomaterial interference is small, is preferably applied in vivo
Tracer.Mesoporous silicon dioxide nano particle (MSN) can guarantee drug molecule and enter in the form spread because of its distinctive meso-hole structure
To aperture；And it has the characteristics that drugloading rate height, surface are easily modified.Therefore, the light of effectively internal circulation for a long time is stablized in building
Power nano material becomes urgent problem.
Summary of the invention
Technical problem to be solved by the present invention lies in provide a kind of mesoporous silicon oxide packet for loading indocyanine green (ICG)
Wrap the preparation method of conversion nano particle.
In order to solve the above technical problems, the technical scheme is that
A kind of mesoporous silicon oxide loading indocyanine green (ICG) superscribes the preparation method of conversion nano particle, specifically
Steps are as follows:
(1) six chloride hydrate yttriums, six trichloride hydrate ytterbiums, six hydration trichlorines conversion nano particle in preparation: are respectively configured
Change thulium solution, liquid is added in clean three-necked flask, adjusts rotor speed, be uniformly mixed solution with smaller revolving speed, it will
Three-necked flask, which is heated to liquid in bottle, becomes stopping heating after white powder, but does not stop the rotation of magnetic agitation rotor, cools down
Oleic acid and octadecylene are added after to 50-60 DEG C, continues to heat up, color becomes yellow (about one hour) from milky, cools to first
The boiling point (6 points 7 degree) of alcohol, is added the methanol solution of containing sodium fluoride, connects gas circuit after being warming up to liquid level bubble-free, takes out true
Empty half an hour leads to nitrogen temperature and heats one hour, particle is collected by centrifugation with ethyl alcohol and hexamethylene；
(2) mesoporous silicon oxide superscribes conversion nano particle: upper conversion is added to hexamethylene with surfactant simultaneously
Alkane solution, magnetic agitation a few hours are added ammonium hydroxide and continue stirring two hours, and tetraethyl orthosilicate (TEOS) stirring is added, uses methanol
Reaction is terminated, is washed with ethyl alcohol and hexamethylene and is dispersed in water for several times, which has been added to cetyl trimethylammonium bromide
In the aqueous solution of triethylamine, tetraethyl orthosilicate is added after stirring a few hours, heating continues to stir, ethanol washing centrifugation, extraction
" etching of surface protection hot water " method is etched after removing cetyl trimethylammonium bromide；
(3) ICG is loaded to mesoporous silicon oxide to superscribe on the nano particle of conversion: by ICG and UCMSN nano particle
Solution is uniformly mixed, and is protected from light magnetic agitation 6-12 hours, is collected by centrifugation, and precipitating is resuspended with distilled water, obtains load ICG's
UCMSN nano particle.
Preferably, the mesoporous silicon oxide of above-mentioned load indocyanine green (ICG) superscribes the preparation side of conversion nano particle
Solution is configured to 1mM in the step (1), wherein six chloride hydrate yttriums, six trichloride hydrate ytterbiums, six trichloride hydrates by method
Heating temperature is 100 DEG C -120 DEG C after the ratio mixing of 700-800:100-200:10-40 by volume of thulium solution.
Preferably, the mesoporous silicon oxide of above-mentioned load indocyanine green (ICG) superscribes the preparation side of conversion nano particle
Method, the additional amount of oleic acid is 2-10mL in the step (1), and the additional amount of octadecylene is 10-40mL, and be added oleic acid and
Heating and temperature control is at 140 DEG C -180 DEG C after octadecylene.
Preferably, the mesoporous silicon oxide of above-mentioned load indocyanine green (ICG) superscribes the preparation side of conversion nano particle
Method, the concentration of sodium fluoride is 0.5-10M in the methanol solution of containing sodium fluoride in the step (1).
Preferably, the mesoporous silicon oxide of above-mentioned load indocyanine green (ICG) superscribes the preparation side of conversion nano particle
Method, the addition temperature after nitrogen is led in the step (1) are 260 DEG C -400 DEG C.
Preferably, the mesoporous silicon oxide of above-mentioned load indocyanine green (ICG) superscribes the preparation side of conversion nano particle
100-200 μ L ammonium hydroxide is added in upper conversion and surfactant in the step (2) in method after mixing in hexamethylene, and
And later with 200 μ L rates hourly by 100-500 μ L tetraethyl orthosilicate (TEOS) injected system, mixture is sealed and is protected
Hold stirring 20-48 hours.
Preferably, the mesoporous silicon oxide of above-mentioned load indocyanine green (ICG) superscribes the preparation side of conversion nano particle
Method, 100- is added dropwise in 100:1-10:10 in cetyl trimethylammonium bromide and triethylamine mass ratio in the step (2)
600 μ L tetraethyl orthosilicates (TEOS), and by system 80 DEG C -90 DEG C of stirrings 1-2 hours；And contain chlorine with 30mL at room temperature
Change the methanol of sodium, extracts 3-6 hours to remove template CTAB.
Preferably, the mesoporous silicon oxide of above-mentioned load indocyanine green (ICG) superscribes the preparation side of conversion nano particle
Method, the middle aqueous solution with 10-50mL PVP (0.25g, Mw=40,000) of the step (2), it is small to stir the mixture for 0.5-3
When, 95 DEG C are then heated to, after etching 3-6 hours, is then cooled to room temperature system.The UCMSN product second that will be obtained
Pure and mild water washing for several times, is finally dispersed in 10mL deionized water.
Preferably, the mesoporous silicon oxide of above-mentioned load indocyanine green (ICG) superscribes the preparation side of conversion nano particle
Method, being protected from light magnetic stirring speed in the step (3) is 400-800 revs/min, 10000-15000 rpms of centrifugation 10-15
Minute, it is collected by centrifugation, the UCMSN nanometer that load indocyanine green is obtained to 1-5 milligrams every milliliter is resuspended quantitatively with distilled water for precipitating
Particle.
Structure of the invention has the advantages that:
The mesoporous silicon oxide of above-mentioned load indocyanine green (ICG) superscribes the preparation method of conversion nano particle, preparation
The upper conversion nano particle for providing 800nm emission peak, wraps up mesoporous silicon oxide outside upper conversion, and ICG is loaded to
Intragranular portion, granular size 80-200nm, cell swallow after survival rate 80%, entered with confocal microscopy particle thin
Born of the same parents carry out pass flag to cell, and it is obvious that laser irradiation cell killing experiment effect is surveyed in thiazolyl blue reaction.
Detailed description of the invention
Fig. 1: the emissioning light spectrum changed is uploaded.
Fig. 2: mesoporous silicon oxide coats the transmission electron microscope appearance figure of upper conversion particles.
Fig. 3: result of the nano particle particle to HeLa cell toxicity of ICG is contained.
Fig. 4: the nano particle particle for containing ICG enters the total focused view of Hela cell.
Fig. 5: the nano particle of ICG is wrapped up after laser irradiation, the result of killing tumor cell.
Specific embodiment
To further illustrate the present invention, now by specific implementation example, the present invention will be described in detail.
Embodiment 1
By six chloride hydrate yttriums, six hydrous ytterbium chlorides, six hydrous thulium chloride solution, volume ratio 700:100:10 is mixed in proportion
It closes and mixes, 110 DEG C are heated 15 minutes to white powder is become, and are stopped heating and are not stopped to rotate, and flask is promoted, and drop is hot to 50 DEG C, adds
Enter 2mL oleic acid and 10mL octadecylene, be warming up to 140 DEG C, color becomes yellow (about one hour) from milky, is cooled to methanol
Boiling point (64.7 DEG C).The methanol solution for weighing 0.5M sodium fluoride, is added dropwise in there-necked flask, 110 DEG C is warming up to, to liquid level without gas
Gas circuit is connected when bubble.Lead to nitrogen after vacuumizing half an hour, is warming up to 260 DEG C, reaction terminates after one hour.Isometric ethyl alcohol from
The heart, 8000 rpms of centrifugation 10min, which are collected, to be precipitated, addition 20mL hexamethylene, 2000 rpms of centrifugation 5min, in collection
Clearly, it repeats the above steps primary, finally product is stored in 20mL vial.
According to O/W reverse microemulsion process, 1mL Igepal CO-520 (NP-5) is dispersed in 20mL hexamethylene.It will be
The UCNP of oleic acid sealing end in cyclohexane solution (2mL, 50mM) is added in hexamethylene/NP-5 mixture, and magnetic agitation 3 hours
Afterwards, 100 μ L ammonia (30%) are added dropwise, stir 2 hours.100 μ L tetraethyl orthosilicates (TEOS) are infused with the rate of 200 μ L/h
Enter system.Mixture is sealed and is kept stirring 36 hours, methanol is added then to terminate reaction.The UCNP@SiO that will be obtained2
Product ethyl alcohol and hexamethylene wash for several times to remove excessive NP-5, and are finally dispersed in 5mL deionized water.By hexadecane
Base trimethyl amine bromide CTAB (2g) and triethylamine TEA (0.01g) is stirred 1.5 hours in 20mL deionized water.Then it is added
10mL contains UCNP@SiO2Deionized water and continue stirring 1.5 hours.100 μ L tetraethyl orthosilicates (TEOS) are added dropwise,
And system is stirred 1 hour at 80 DEG C.By the UCNP@SiO of generation2@mSiO2Product with ethanol washing for several times, and at room temperature
With the methanol solution of 30mL (1wt%) NaCl, 3 hours are extracted to remove template CTAB.Extraction carries out for several times, final UCNP@
SiO2@mSiO2Product is dispersed in 10mL deionized water.The UCNP@SiO that will be prepared in 10mL deionized water2@mSiO2It is added to
In flask containing 10mL PVP (0.25g, Mw=40,000) deionized water.It stirs the mixture for 0.5 hour, is then heated to
95℃.After etching 3 hours, then system is cooled to room temperature.For several times by obtained UCMSN product ethyl alcohol and water washing, most
After be dispersed in 10mL deionized water.
ICG is uniformly mixed with UCMSN nanoparticles solution, is protected from light magnetic agitation 8 hours, 10000 rpms of centrifugations
It collects within 10 minutes, precipitating is resuspended with distilled water, obtains the UCMSN nano particle of load ICG.
Embodiment 2
By six chloride hydrate yttriums, six hydrous ytterbium chlorides, six hydrous thulium chloride solution 800:200:40 by volume, mix
120 DEG C are heated 15 minutes to white powder is become, and are stopped heating and are not stopped to rotate, and flask is promoted, and drop is hot to 50 DEG C, and 10mL oil is added
Acid and 40mL octadecylene, are warming up to 180 DEG C, color becomes yellow (about one hour) from milky, is cooled to the boiling point of methanol
(64.7℃).The methanol for weighing 2.5mM sodium fluoride, is added dropwise in there-necked flask, is warming up to 110 DEG C, connects when liquid level bubble-free
Connect gas circuit.Lead to nitrogen after vacuumizing half an hour, is warming up to 400 DEG C, reaction terminates after one hour.Isometric ethyl alcohol centrifugation,
8000 rpms of centrifugation 10min collect precipitating, and 20mL hexamethylene is added, and 2000 rpms of centrifugation 5min collect supernatant, weight
Multiple above-mentioned steps are primary, and finally product is stored in 20mL vial.
According to O/W reverse microemulsion process, 1mL Igepal CO-520 (NP-5) is dispersed in 20mL hexamethylene.It will be
The UCNP of oleic acid sealing end in cyclohexane solution (2mL, 50mM) is added in hexamethylene/NP-5 mixture, and magnetic agitation 3 hours
Afterwards, 200 μ L ammonia (30%) are added dropwise, stir 2 hours.200 μ L tetraethyl orthosilicates (TEOS) are infused with the rate of 200 μ L/h
Enter system.Mixture is sealed and is kept stirring 36 hours, methanol is added then to terminate reaction.The UCNP@SiO that will be obtained2
Product ethyl alcohol and hexamethylene wash for several times to remove excessive NP-5, and are finally dispersed in 5mL deionized water.By CTAB
(2g) and TEA (0.02g) are stirred 1.5 hours in 20mL deionized water.10mL is then added and contains UCNP@SiO2Deionization
Water simultaneously continues stirring 1.5 hours.600 μ L tetraethyl orthosilicates (TEOS) are added dropwise, and it is small that system is stirred to 1 at 80 DEG C
When.By the UCNP@SiO of generation2@mSiO2Product with ethanol washing for several times, and at room temperature use 30mL (1wt%) NaCl methanol
Solution extracts 3 hours to remove template CTAB.Extraction carries out for several times, final UCNP@SiO2@mSiO2Product is dispersed in 10mL
In deionized water.The UCNP@SiO that will be prepared in 10mL deionized water2@mSiO2It is added to containing 50mLPVP (0.25g, Mw=
40,000) in the flask of deionized water.It stirs the mixture for 3 hours, is then heated to 95 DEG C.After etching 6 hours, then will be
System is cooled to room temperature.For several times by obtained UCMSN product ethyl alcohol and water washing, it is finally dispersed in 10mL deionized water.
ICG is uniformly mixed with UCMSN nanoparticles solution, is protected from light magnetic agitation 9 hours, 10000 rpms 15 points
Clock is collected by centrifugation, and precipitating is resuspended with distilled water, obtains the UCMSN nano particle of load ICG.
Embodiment 3
By six chloride hydrate yttriums, six hydrous ytterbium chlorides, six hydrous thulium chloride solution, 780:200:20 is mixed by volume
Even, 110 DEG C are heated 20 minutes to white powder is become, and are stopped heating and are not stopped to rotate, and flask is promoted, and drop is hot to 50 DEG C, and 6mL is added
Oleic acid and 15mL octadecylene are warming up to 150 DEG C, and color becomes yellow (about one hour) from milky, is cooled to the boiling point of methanol
(64.7℃).Weigh 0.168g sodium fluoride, be dissolved in 4mL methanol, be added dropwise in there-necked flask, be warming up to 110 DEG C, to liquid level without
Gas circuit is connected when bubble.Lead to nitrogen after vacuumizing half an hour, is warming up to 300 DEG C, reaction terminates after one hour.Isometric ethyl alcohol
Centrifugation, 8000 rpms of centrifugation 10min, which are collected, to be precipitated, addition 20mL hexamethylene, 2000 rpms of centrifugation 5min, in collection
Clearly, it repeats the above steps primary, finally product is stored in 20mL vial.
According to O/W reverse microemulsion process, 1mL Igepal CO-520 (NP-5) is dispersed in 20mL hexamethylene.It will be
The UCNP of oleic acid sealing end in cyclohexane solution (2mL, 50mM) is added in hexamethylene/NP-5 mixture, and magnetic agitation 3 hours
Afterwards, 140 μ L ammonia (30%) are added dropwise, stir 2 hours.200 μ L tetraethyl orthosilicates (TEOS) are infused with the rate of 200 μ L/h
Enter system.Mixture is sealed and is kept stirring 36 hours, methanol is added then to terminate reaction.The UCNP@SiO that will be obtained2
Product ethyl alcohol and hexamethylene wash for several times to remove excessive NP-5, and are finally dispersed in 5mL deionized water.By CTAB
(2g) and TEA (0.2g) are stirred 1.5 hours in 20mL deionized water.10mL is then added and contains UCNP@SiO2Deionization
Water simultaneously continues stirring 1.5 hours.300 μ L tetraethyl orthosilicates (TEOS) are added dropwise, and it is small that system is stirred to 1 at 80 DEG C
When.By the UCNP@SiO of generation2@mSiO2Product with ethanol washing for several times, and at room temperature use 30mL (1wt%) NaCl methanol
Solution extracts 3 hours to remove template CTAB.Extraction carries out for several times, final UCNP@SiO2@mSiO2Product is dispersed in 10mL
In deionized water.The UCNP@SiO that will be prepared in 10mL deionized water2@mSiO2It is added to containing 10mLPVP (0.25g, Mw=
40,000) in the flask of deionized water.It stirs the mixture for 0.5 hour, is then heated to 95 DEG C.After etching 3 hours, then will
System is cooled to room temperature.For several times by obtained UCMSN product ethyl alcohol and water washing, it is finally dispersed in 10mL deionized water.
ICG is uniformly mixed with UCMSN nanoparticles solution, is protected from light magnetic agitation 12 hours, 12000 rpms of centrifugations
It collects, precipitating is resuspended with distilled water, obtains the UCMSN nano particle of load ICG.
Embodiment 4
The upper conversion nano particle prepared in embodiment 3 is dissolved in cyclohexane solution, the penetrating quartz in four sides is added to
It in ware, is irradiated with 980nm laser, with optical fiber spectral collection signal, obtains the emissioning light spectrum of prepared upper conversion (such as
Shown in Fig. 1), it is obviously emission peak that prepared upper conversion nano particle has at 800nm as figure shows.By receiving in example 3
Rice grain is diluted, and is added dropwise and is supported to carry out morphology observation (as shown in Figure 2), particle with transmission electron microscope on film in carbon
For size than more uniform, package effect is normal.
Embodiment 5
Toxicity of the various concentration nano particle of mtt assay test preparation to HeLa cell:
(1) plantation 8000/hole of HeLa cell is to 96 well culture plates, and after 24 hours, cell reaches converging for 70%-90%
When rate, the culture medium in hole is changed to 100 microlitres of DMEM culture mediums, cell is carried out Nature enemy 6 hours.
(2) by particle with the DMEM culture medium containing serum be diluted to 0.025 milligram every milliliter, 0.0125 milligram every milliliter,
0.00625 milligram every milliliter, 0.003125 milligram every milliliter and 0.00625 milligram every milliliter five concentration, to replace in adding hole
Generation former not serum-containing media.At 37 DEG C, 5%CO2After being incubated for 24 hours under incubator environment, 10 microlitres are added into each hole
MTT solution is drawn every hole culture medium, is added into every hole 100 micro- after continuing to put back under incubator environment and continuing to be incubated for 4 hours
Rise DMSO, room temperature shaker concussion reaction 10 minutes.Every hole sample is examined to inhale in 570 nanometer wave strong points using enzyme-linked immunosorbent assay instrument
Light value calculates cell survival rate by following formula, and every group sets 8 in parallel, calculates its average value.
(3) cell survival rate (%)=experimental group absorbance of cells (A2)/blank group absorbance of cells (A1) * 100% is (such as
Shown in Fig. 3).
Embodiment 6
8000/hole of HeLa cell is planted to being copolymerized burnt capsule, after 24 hours, what cell reached 70%-90% converges rate
When, the culture medium in hole is changed to 200 microlitres of DMEM culture mediums, cell is carried out Nature enemy 4 hours.It will be in embodiment 3
The nano particle of preparation is diluted to 0.0100 milligram every milliliter with the DMEM culture medium containing serum, is free of in adding hole with substituting original
Blood serum medium.At 37 DEG C, 5%CO2After being incubated for 4 hours under incubator environment, it is fixed and with Hochest dyestuff by nuclei dyeing
Color, in fluorescence inverted microscope, (nano particle that 560 nanochannels observe ICG element label is shown in red, 405 nanochannels
Observation Hochest dyestuff is shown as blue) nano particle of observation preparation is to the phagocytosis situation (as shown in Figure 4) of cell.
The evaluation of the cellkilling capacity of nano particle of the present invention is as follows:
(1) for plantation HeLa cell to 24 well culture plates, 10000/hole of cell density reaches 70%-90%'s to cell
When converging rate, the culture medium in hole is sucked out, 200 μ L DMEM culture mediums are changed to, cell is carried out Nature enemy 6-8 hours.
(2) nano particle that the mesoporous silicon oxide for loading ICG is superscribed to conversion is dilute with the DMEM culture medium containing serum
It releases to 0.00625-0.0500 milligrams every milliliter, with the former not serum-containing media of substitution in adding hole.
Laser irradiation cell is used after (3) 4 hours.
(4) at 37 DEG C, 5%CO2After being incubated for 24 hours under incubator environment, ten to one diluted MTT and serum-free is added
Culture medium was incubated for after four hours, and the dimethyl for going supernatant to be added 100 microlitres is sub-, was existed with each cavity of microplate reader detection
Absorption intensity under 570nm wavelength light, and carry out statistical analysis cell killing efficiency such as Fig. 5.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (9)
1. the preparation method that a kind of mesoporous silicon oxide for loading indocyanine green superscribes conversion nano particle, it is characterised in that:
Specific step is as follows:
(1) six chloride hydrate yttriums, six trichloride hydrate ytterbiums, six trichloride hydrate thuliums conversion nano particle in preparation: are respectively configured
Solution liquid is added in clean three-necked flask, adjusts rotor speed, is uniformly mixed solution with smaller revolving speed, Jiang Sankou
Flask, which is heated to liquid in bottle, becomes stopping heating after white powder, but does not stop the rotation of magnetic agitation rotor, cools to 50-
Oleic acid and octadecylene are added after 60 DEG C, continues to heat up, color becomes yellow from milky, cools to the boiling point of methanol, and addition contains
The methanol solution of sodium fluoride connects gas circuit after being warming up to liquid level bubble-free, vacuumizes half an hour, and it is small to lead to nitrogen temperature heating one
When, particle is collected by centrifugation with ethyl alcohol and hexamethylene；
(2) mesoporous silicon oxide superscribes conversion nano particle: it is molten that upper conversion is added to surfactant hexamethylene simultaneously
Liquid, magnetic agitation a few hours are added ammonium hydroxide and continue stirring two hours, and tetraethyl orthosilicate stirring is added, is terminated and is reacted with methanol,
It is washed with ethyl alcohol and hexamethylene and is dispersed in water for several times, which is added to cetyl trimethylammonium bromide and triethylamine
In aqueous solution, tetraethyl orthosilicate is added after stirring a few hours, heating continues to stir, and ethanol washing centrifugation, extraction removes 16
" etching of surface protection hot water " method is etched after alkyl trimethyl ammonium bromide；
(3) ICG is loaded to mesoporous silicon oxide to superscribe on the nano particle of conversion: by ICG and UCMSN nanoparticles solution
It is uniformly mixed, is protected from light magnetic agitation 6-12 hours, is collected by centrifugation, precipitating is resuspended with distilled water, and the UCMSN for obtaining load ICG receives
Rice grain.
2. the preparation side that the mesoporous silicon oxide of load indocyanine green according to claim 1 superscribes conversion nano particle
Method, it is characterised in that: solution is configured to 1mM in the step (1), wherein six chloride hydrate yttriums, six trichloride hydrate ytterbiums,
Six trichloride hydrate thulium solution by volume 700-800:100-200:10-40 ratio mix after heating temperature be 100 DEG C-
120℃。
3. the preparation side that the mesoporous silicon oxide of load indocyanine green according to claim 1 superscribes conversion nano particle
Method, it is characterised in that: the additional amount of oleic acid is 2-10mL in the step (1), and the additional amount of octadecylene is 10-40mL, and
Heating and temperature control is at 140 DEG C -180 DEG C after oleic acid and octadecylene is added.
4. the preparation side that the mesoporous silicon oxide of load indocyanine green according to claim 1 superscribes conversion nano particle
Method, it is characterised in that: the concentration of sodium fluoride is 0.5-2.5M in the methanol solution of containing sodium fluoride in the step (1).
5. the preparation side that the mesoporous silicon oxide of load indocyanine green according to claim 1 superscribes conversion nano particle
Method, it is characterised in that: the addition temperature after leading to nitrogen in the step (1) is 260 DEG C -400 DEG C.
6. the preparation side that the mesoporous silicon oxide of load indocyanine green according to claim 1 superscribes conversion nano particle
Method, it is characterised in that: 100- is added after mixing in hexamethylene in upper conversion and surfactant in the step (2)
200 μ L ammonium hydroxide, and later with 200 μ L rates hourly by 100-500 μ L tetraethyl orthosilicate (TEOS) injected system, it mixes
Object is closed to seal and be kept stirring 20-48 hours.
7. the preparation side that the mesoporous silicon oxide of load indocyanine green according to claim 1 superscribes conversion nano particle
Method, it is characterised in that: in the step (2) cetyl trimethylammonium bromide and triethylamine mass ratio in 100:1-10:10, by
Be added dropwise to 100-600 μ L tetraethyl orthosilicate (TEOS), and by system 80 DEG C -90 DEG C of stirrings 1-2 hours；And it uses at room temperature
30mL contains the methanol of sodium chloride, extracts 3-6 hours to remove template CTAB.
8. the preparation side that the mesoporous silicon oxide of load indocyanine green according to claim 1 superscribes conversion nano particle
Method, it is characterised in that: with the aqueous solution of 10-50mL PVP (0.25g, Mw=40,000) in the step (2), mixture is stirred
It mixes 0.5-3 hours, is then heated to 95 DEG C, after etching 3-6 hours, be then cooled to room temperature system.The UCMSN that will be obtained
Product ethyl alcohol and water washing for several times, are finally dispersed in 10mL deionized water.
9. the preparation side that the mesoporous silicon oxide of load indocyanine green according to claim 1 superscribes conversion nano particle
Method, it is characterised in that: being protected from light magnetic stirring speed in the step (3) is 400-800 revs/min, 10000-15000 revolutions per minute
It Zhongli's heart 10-15 minutes, is collected by centrifugation, precipitating is resuspended quantitatively with distilled water to 1-5 milligrams every milliliter, obtains load indocyanine green
UCMSN nano particle.
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| CN113281321A (en) * | 2021-06-08 | 2021-08-20 | 江苏大学 | Based on Fe3+Rapid detection method for staphylococcus aureus capable of quenching up-conversion fluorescence |
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| CN110179973A (en) * | 2019-06-11 | 2019-08-30 | 扬州大学 | A kind of hybridized nanometer vaccine of photothermal response and preparation method thereof |
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| CN110507632A (en) * | 2019-08-19 | 2019-11-29 | 天津大学 | A kind of preparation method of composite membrane package mesoporous silica nano-particle |
| CN110478483A (en) * | 2019-08-22 | 2019-11-22 | 青岛大学 | Conversion nano probe and preparation method and application on a kind of polychrome |
| CN113281321A (en) * | 2021-06-08 | 2021-08-20 | 江苏大学 | Based on Fe3+Rapid detection method for staphylococcus aureus capable of quenching up-conversion fluorescence |
| CN113281321B (en) * | 2021-06-08 | 2022-08-26 | 江苏大学 | Based on Fe 3+ Staphylococcus aureus rapid detection method capable of quenching up-conversion fluorescence |
| CN113813449A (en) * | 2021-08-30 | 2021-12-21 | 孟繁宇 | Preparation method of nanoparticle rapamycin drug-loaded coating balloon |
| CN115381968A (en) * | 2022-08-23 | 2022-11-25 | 中山大学 | Rare earth-organic composite optical nano probe and preparation method and application thereof |
| CN115381968B (en) * | 2022-08-23 | 2023-09-26 | 中山大学 | Rare earth-organic composite optical nano probe and preparation method and application thereof |
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