CN106511299B - Ferroso-ferric oxide/gold/Nano particles of silicon dioxide preparation of a kind of core-shell structure and near infrared light Drug controlled release - Google Patents
Ferroso-ferric oxide/gold/Nano particles of silicon dioxide preparation of a kind of core-shell structure and near infrared light Drug controlled release Download PDFInfo
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- CN106511299B CN106511299B CN201610911532.XA CN201610911532A CN106511299B CN 106511299 B CN106511299 B CN 106511299B CN 201610911532 A CN201610911532 A CN 201610911532A CN 106511299 B CN106511299 B CN 106511299B
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- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 239000003814 drug Substances 0.000 title claims abstract description 58
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 229940079593 drug Drugs 0.000 title claims abstract description 42
- 229940056319 ferrosoferric oxide Drugs 0.000 title claims abstract description 39
- 239000010931 gold Substances 0.000 title claims abstract description 37
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 31
- 229910052737 gold Inorganic materials 0.000 title claims abstract description 28
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 23
- 235000012239 silicon dioxide Nutrition 0.000 title claims abstract description 22
- 239000011258 core-shell material Substances 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000013270 controlled release Methods 0.000 title claims abstract description 9
- 239000002131 composite material Substances 0.000 claims abstract description 12
- 239000000243 solution Substances 0.000 claims description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 235000019441 ethanol Nutrition 0.000 claims description 15
- 238000005406 washing Methods 0.000 claims description 13
- 239000012153 distilled water Substances 0.000 claims description 12
- VJJPUSNTGOMMGY-MRVIYFEKSA-N etoposide Chemical compound COC1=C(O)C(OC)=CC([C@@H]2C3=CC=4OCOC=4C=C3[C@@H](O[C@H]3[C@@H]([C@@H](O)[C@@H]4O[C@H](C)OC[C@H]4O3)O)[C@@H]3[C@@H]2C(OC3)=O)=C1 VJJPUSNTGOMMGY-MRVIYFEKSA-N 0.000 claims description 12
- 229960005420 etoposide Drugs 0.000 claims description 12
- 239000008055 phosphate buffer solution Substances 0.000 claims description 12
- 239000000047 product Substances 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 6
- 238000004108 freeze drying Methods 0.000 claims description 6
- 238000005259 measurement Methods 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 6
- 229910001868 water Inorganic materials 0.000 claims description 6
- 229910019142 PO4 Inorganic materials 0.000 claims description 5
- 238000013019 agitation Methods 0.000 claims description 5
- 239000006227 byproduct Substances 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 5
- 239000010452 phosphate Substances 0.000 claims description 5
- 229910004042 HAuCl4 Inorganic materials 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- YASYEJJMZJALEJ-UHFFFAOYSA-N Citric acid monohydrate Chemical compound O.OC(=O)CC(O)(C(O)=O)CC(O)=O YASYEJJMZJALEJ-UHFFFAOYSA-N 0.000 claims description 3
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 3
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 3
- 239000000908 ammonium hydroxide Substances 0.000 claims description 3
- 229960002303 citric acid monohydrate Drugs 0.000 claims description 3
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 3
- 238000010907 mechanical stirring Methods 0.000 claims description 3
- 229910000403 monosodium phosphate Inorganic materials 0.000 claims description 3
- 235000019799 monosodium phosphate Nutrition 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 3
- 239000012498 ultrapure water Substances 0.000 claims description 3
- 238000009835 boiling Methods 0.000 claims description 2
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims 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 claims 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims 1
- 239000003405 delayed action preparation Substances 0.000 claims 1
- 239000001257 hydrogen Substances 0.000 claims 1
- 229910052739 hydrogen Inorganic materials 0.000 claims 1
- 229910052742 iron Inorganic materials 0.000 claims 1
- 230000003647 oxidation Effects 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000001727 in vivo Methods 0.000 abstract 1
- 230000003902 lesion Effects 0.000 abstract 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 21
- 239000000463 material Substances 0.000 description 9
- 229910001922 gold oxide Inorganic materials 0.000 description 8
- 239000002114 nanocomposite Substances 0.000 description 7
- 206010001497 Agitation Diseases 0.000 description 4
- 230000008685 targeting Effects 0.000 description 4
- 238000009825 accumulation Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 229930182470 glycoside Natural products 0.000 description 2
- 150000002338 glycosides Chemical class 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 206010000830 Acute leukaemia Diseases 0.000 description 1
- 206010005003 Bladder cancer Diseases 0.000 description 1
- 208000006332 Choriocarcinoma Diseases 0.000 description 1
- 208000005125 Invasive Hydatidiform Mole Diseases 0.000 description 1
- 206010025323 Lymphomas Diseases 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 206010060862 Prostate cancer Diseases 0.000 description 1
- 208000000236 Prostatic Neoplasms Diseases 0.000 description 1
- 206010041067 Small cell lung cancer Diseases 0.000 description 1
- 208000005718 Stomach Neoplasms Diseases 0.000 description 1
- 208000007097 Urinary Bladder Neoplasms Diseases 0.000 description 1
- SWLVFNYSXGMGBS-UHFFFAOYSA-N ammonium bromide Chemical compound [NH4+].[Br-] SWLVFNYSXGMGBS-UHFFFAOYSA-N 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 238000002512 chemotherapy Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 230000003013 cytotoxicity Effects 0.000 description 1
- 231100000135 cytotoxicity Toxicity 0.000 description 1
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 description 1
- 230000000857 drug effect Effects 0.000 description 1
- 238000002651 drug therapy Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 206010017758 gastric cancer Diseases 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- -1 isopropyl-methyl-benzene phenol Chemical compound 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005549 size reduction Methods 0.000 description 1
- 208000000587 small cell lung carcinoma Diseases 0.000 description 1
- 201000011549 stomach cancer Diseases 0.000 description 1
- 201000005112 urinary bladder cancer Diseases 0.000 description 1
Classifications
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- 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
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/70—Carbohydrates; Sugars; Derivatives thereof
- A61K31/7042—Compounds having saccharide radicals and heterocyclic rings
- A61K31/7048—Compounds having saccharide radicals and heterocyclic rings having oxygen as a ring hetero atom, e.g. leucoglucosan, hesperidin, erythromycin, nystatin, digitoxin or digoxin
-
- 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
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/0002—Galenical forms characterised by the drug release technique; Application systems commanded by energy
- A61K9/0004—Osmotic delivery systems; Sustained release driven by osmosis, thermal energy or gas
-
- 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
- A61K9/0002—Galenical forms characterised by the drug release technique; Application systems commanded by energy
- A61K9/0009—Galenical forms characterised by the drug release technique; Application systems commanded by energy involving or responsive to electricity, magnetism or acoustic waves; Galenical aspects of sonophoresis, iontophoresis, electroporation or electroosmosis
Landscapes
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Veterinary Medicine (AREA)
- Medicinal Chemistry (AREA)
- Pharmacology & Pharmacy (AREA)
- Epidemiology (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Engineering & Computer Science (AREA)
- Molecular Biology (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Biomedical Technology (AREA)
- Nanotechnology (AREA)
- Optics & Photonics (AREA)
- Medicinal Preparation (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The present invention relates to a kind of ferroso-ferric oxide/gold/Nano particles of silicon dioxide preparation of core-shell structure and near infrared light Drug controlled release.The following steps are included: preparing ferriferrous oxide nano-particle, ferroso-ferric oxide/gold nanoparticle, ferroso-ferric oxide/gold/Nano particles of silicon dioxide controls vitro drug release near infrared light on drug loading to composite material.The beneficial effects of the present invention are: ferroso-ferric oxide/gold/Nano particles of silicon dioxide has excellent biological degradability, and lesion tissue can be targeted under the action of externally-applied magnetic field, thermal control drug slow release is converted light into under near infrared light, efficiently uses drug slow release and in vivo.
Description
Technical field
The present invention relates to a kind of ferroso-ferric oxide/gold/Nano particles of silicon dioxide preparation of core-shell structure and with close red
Outer photocontrol drug release, belongs to materials synthesis and biomedicine field.
Technical background
Medicament slow release technology comes across the eighties, and the form of the controlled release of drug can produce appropriate reaction, smaller
Side effect and longer curative effect.This adjustable drug releasing rate of administration mode reduces administration number of times, to increase
Safety, high efficiency and the reliability of drug therapy.Therefore, make that a kind of drug is efficient, predictable release, and continue longer
The curative effect of time is clinically meaningful.
Nano ferriferrous oxide because its special physicochemical property and field of biomedicine potentially apply obtain extensively
Research.Nano ferriferrous oxide has the function of externally-applied magnetic field targeting positioning in medicament slow release.Gold nanoparticle has fine
Optical property, luminous energy can be converted to thermal energy.Mesoporous silicon oxide can effectively improve drug in medicament slow release
Charging ratio, and mesoporous silicon oxide has good biocompatibility and low cytotoxicity.Therefore synthesis ferroso-ferric oxide/
Gold/silicon dioxide nano composite material can carry out targeting positioning by externally-applied magnetic field, improve drug using mesoporous silicon oxide
Useful load, luminous energy is converted to thermal energy Drug controlled release under near infrared light.Etoposide is widely used in
The chemotherapy of cancer, be mainly used for treat Small Cell Lung Cancer, to acute leukemia, malignant lymphoma, orchioncus, bladder cancer,
Prostate cancer, gastric cancer, chorioepithelioma, oophoroma, chorioadenoma etc. are also effective.But since a large amount of Etoposide is to people
The normal cell of body has damage, it is therefore desirable to control damage of the burst size reduction of Etoposide to normal cell.Rely on pool
Glycosides is used for medicament slow release as matrix drug well.
Summary of the invention
The purpose of the invention is to provide a kind of ferroso-ferric oxide/gold/Nano particles of silicon dioxide of core-shell structure
It prepares and near infrared light Drug controlled release, discharges drug targeting, and maintain the drug effect of long period.
Ferroso-ferric oxide/gold/Nano particles of silicon dioxide preparation of a kind of core-shell structure of the present invention and with close red
Outer photocontrol drug release, comprising the following steps:
A, it prepares nano ferriferrous oxide: taking Fe2+With Fe3+Molar ratio is 1:2, weighs FeSO respectively4·7H2O and
FeCl3·6H2O is dissolved in 20mL distilled water and carries out mechanical stirring, leads to nitrogen protection.NH is added dropwise into solution3·H2O (3 seconds/
Drop), it round-bottomed flask is placed in stir 30 minutes in 80 DEG C of constant temperature water baths after being added dropwise cures.After reaction by sample
The separation of product externally-applied magnetic field, washing 6 times (washing 1 time, alcohol is washed 1 time, is washed 4 times).By the sample freeze-drying after washing.
B, ferroso-ferric oxide/gold nanoparticle is prepared: by ferroso-ferric oxide made from step a and two citric acid monohydrate trisodiums
It is added in 200mL ultrapure water, ultrasonic disperse 10 minutes.The solution (with condensing reflux pipe) is heated with vigorous stirring to boiling
It rises, rapidly joins HAuCl4(Fe3O4:HAuCl4=5:1) solution.Solution colour becomes brown from faint yellow immediately, eventually becomes
Red continues stirring 15 minutes.Products obtained therefrom externally-applied magnetic field is separated, washing 6 times (washing 1 time, alcohol wash 1 time, in triplicate),
Freeze-drying.
C, it prepares ferroso-ferric oxide/gold/Nano particles of silicon dioxide: weighing ferroso-ferric oxide/gold nano of step b preparation
Particle is dispersed in containing cetyl trimethylammonium bromide (0.3g), distilled water (80mL), ammonium hydroxide (1.2mL), ethyl alcohol (60mL)
Mixed solution, by mixed solution ultrasonic disperse 30 minutes.Ethyl orthosilicate (0.5mL) is added dropwise to the solution continuously stirred
In, it reacts 6 hours.Products obtained therefrom Magneto separate is collected, is washed repeatedly with ethyl alcohol and distilled water and removes non magnetic by-product.It will wash
Product after washing is dispersed in the acetone soln of 50mL, is flowed back 6 hours at 65 DEG C, and cetyl trimethylammonium bromide mould is removed
Plate.Products therefrom ethyl alcohol and distilled water are washed repeatedly, are freeze-dried.
D, ferroso-ferric oxide/gold/Nano particles of silicon dioxide is dispersed in etoposide solution, 37 DEG C of constant temperature stirrings 6
Hour, reach equilibrium state.It is separated with externally-applied magnetic field, the sample after load medicine is 12 hours dry at 60 DEG C.
E, it takes 40mg to carry medicine composite material, is placed in bag filter, and bag filter is put in 30mL phosphate buffer solution
Magnetic agitation is carried out, carries out near infrared light drug release under the conditions of 37 DEG C of Yu Hengwen.Influence of the different pH to drug release
It makes further research.The pH of phosphate buffer solution is 7.4, is discharged 300 minutes.Every 30 minutes taking-up 5mL solution, measurement according to
The content of support pool glycosides, while adding 5mL phosphate buffer solution.The content of Etoposide is existed using ultraviolet specrophotometer
It is measured at 285nm, the drug release cumulative percentage of different time is calculated according to the Etoposide content of measurement.
Further, NH in step a3·H2The concentration of O is 0.1~1mol/L.
Further, acetone soln can remove in step c for isopropyl-methyl-benzene phenol or 500~600 DEG C of high-temperature calcinations
Cetyl trimethylammonium bromide template.
Further, Etoposide concentration is 0~0.3mg/mL in step d.
Further, phosphate buffer solution is formulated by disodium hydrogen phosphate and sodium dihydrogen phosphate in step e, and concentration is
0~0.2mol/L.
The beneficial effects of the present invention are: ferroso-ferric oxide/gold/silicon dioxide nano composite material of core-shell structure has magnetic
Targeting positioning, and pass through light control drug slow release.
Detailed description of the invention
This experiment is further illustrated with reference to the accompanying drawing.
Fig. 1 is the X-ray diffractogram of ferroso-ferric oxide in embodiment one.
Fig. 2 is ferroso-ferric oxide/gold X-ray diffractogram in embodiment one.
Fig. 3 is ferroso-ferric oxide/gold/silicon dioxide nano composite material X-ray diffractogram in embodiment one.
Fig. 4 is the external medicament slow release performance figure of composite material under different pH condition in embodiment two.
Fig. 5 be in embodiment three near infrared light and comparative example one unused near infrared light composite material it is external
Medicament slow release performance figure.
Specific embodiment
Presently in connection with specific embodiment, the present invention will be further described, following embodiment be intended to illustrate invention rather than
Limitation of the invention further.
Embodiment one:
Prepare ferroso-ferric oxide/gold/silicon dioxide nano composite material of core-shell structure including the following steps:
(1) FeSO is weighed respectively4·7H2O (2.4g) and FeCl3·6H2O (4.7g) is dissolved in 20mL distilled water and carries out
Mechanical stirring leads to nitrogen protection.20mL (0.5mol/L) NH is added dropwise into solution3·H2O (3 seconds/drop), will justify after being added dropwise
Bottom flask is placed in stir 30 minutes in 80 DEG C of constant temperature water baths and be cured.Sample externally-applied magnetic field is separated after reaction, is washed
It washs 6 times (washing 1 time, alcohol is washed 1 time, is washed 4 times).By the sample freeze-drying after washing, ferriferrous oxide nano-particle is obtained.
Its X-ray diffractogram is as shown in Figure 1.Shown in figure 2 θ be 18.7 °, 30.1 °, 35.5 °, 43.2 °, 53.3 °, 57.6 °,
At 62.4 ° and 74.5 ° occur diffraction maximum, correspond respectively to face-centered cubic crystal form ferriferrous oxide nano-particle (111),
(220), (311), (400), (422), (511), (440) and (533) crystal face.Illustrate that ferriferrous oxide nano-particle is good
It is synthesized.
(2) it weighs ferroso-ferric oxide (0.2315g) made from step (1) and two citric acid monohydrate trisodiums (0.0294g) adds
Enter into 200mL ultrapure water, ultrasonic disperse 10 minutes.The solution (with condensing reflux pipe) is heated with vigorous stirring extremely to boil,
Rapidly join HAuCl4(10mL, 0.01mol/L) solution.Solution colour becomes brown from faint yellow immediately, eventually becomes red,
Continue stirring 15 minutes.Products obtained therefrom externally-applied magnetic field is separated, washing 6 times (washing 1 time, alcohol wash 1 time, in triplicate), freezing
It is dry, obtain ferroso-ferric oxide/gold nanoparticle.Its X-ray diffractogram as shown in Fig. 2, shown in figure 2 θ 38.185 °,
Occur strong diffraction maximum at 44.393 °, 64.578 °, 77.549 ° and 81.724 °, correspond respectively to Au nanoparticle (111),
(200), (220), (311) and (222) crystal face, to show there is golden presence in ferroso-ferric oxide/gold nanoparticle structure.
(3) ferroso-ferric oxide/gold nanoparticle (0.1g) for weighing step (2) preparation is dispersed in containing cetyl front three
Base ammonium bromide (0.3g), distilled water (80mL), ammonium hydroxide (1.2mL), ethyl alcohol (60mL) mixed solution, by mixed solution ultrasonic disperse
30 minutes.Ethyl orthosilicate (0.5mL) is added dropwise in the solution continuously stirred, is reacted 6 hours.By products obtained therefrom magnetic point
From collection, is washed repeatedly with ethyl alcohol and distilled water and remove non magnetic by-product.Product after washing is dispersed in the acetone of 50mL
It in solution, flows back 6 hours at 65 DEG C, removes cetyl trimethylammonium bromide template.By products therefrom ethyl alcohol and distilled water
It washs repeatedly, is freeze-dried, obtains ferroso-ferric oxide/gold/silicon dioxide composite material.Its X-ray diffractogram as shown in figure 3,
It is silica peak that 2 θ have a very wide peak at 10~30 ° in figure.
Embodiment two:
Vitro drug release behavior under condition of different pH including the following steps:
The ferroso-ferric oxide of core-shell structure/gold/silicon dioxide nano composite material preparation process is the same as example 1
(1) phosphate buffer solution of 0.1mol/L is prepared for simulating human body environment, and the composite material for weighing 40mg is set
In bag filter, and bag filter is put into 37 DEG C of magnetic agitations of phosphate buffer solution constant temperature of 30mL.Adjust phosphate-buffered
The pH of solution is 5.4,6.4 and 7.4, is discharged 300 minutes respectively.
(2) 5mL solution was taken out from solution every 30 minutes, measures medicament contg, while it is molten to add 5mL phosphate-buffered
Liquid.The content of drug is measured at 285nm using ultraviolet specrophotometer, calculates different time according to measurement medicament contg
Drug accumulation percentage, as shown in Figure 4.It can be seen from the figure that the rate of release of drug increases with the reduction of pH value, say
The pH value of bright solution has an impact to the rate of release of drug.
Embodiment three:
Vitro drug release behavior under the conditions of near infrared light including the following steps:
The ferroso-ferric oxide of core-shell structure/gold/silicon dioxide nano composite material preparation process is the same as example 1
(1) phosphate buffer solution of 0.1mol/L is prepared for simulating human body environment, is weighed 40mg composite material and is placed in
In bag filter, and bag filter is put into 37 DEG C of magnetic agitations of phosphate buffer solution constant temperature of 30mL.It is multiple near infrared light
Condensation material discharges 300 minutes.
(2) 5mL solution was taken out from solution every 30 minutes, measures medicament contg, while it is molten to add 5mL phosphate-buffered
Liquid.The content of drug is measured at 285nm using ultraviolet specrophotometer, calculates different time according to measurement medicament contg
Drug accumulation percentage, as shown in Figure 5 a.
Comparative example one:
Vitro drug release behavior under the conditions of unused near infrared light including the following steps:
The ferroso-ferric oxide of core-shell structure/gold/silicon dioxide nano composite material preparation process is the same as example 1
(1) phosphate buffer solution of 0.1mol/L is prepared for simulating human body environment, is weighed 40mg composite material and is placed in
In bag filter, and bag filter is put into 37 DEG C of magnetic agitations of phosphate buffer solution constant temperature of 30mL.Unused near infrared light
Composite material discharges 300 minutes.
(2) 5mL solution was taken out from solution every 30 minutes, measures medicament contg, while it is molten to add 5mL phosphate-buffered
Liquid.The content of drug is measured at 285nm using ultraviolet specrophotometer, calculates different time according to measurement medicament contg
Drug accumulation percentage, as shown in Figure 5 b.It can be seen from the figure that near infrared light composite material drug release cumulant is bright
It is aobvious to be higher than non-composite material of irradiation drug release cumulant.This illustrates that near infrared light can be very good releasing for control drug
It puts.
Claims (4)
1. core-shell structure ferroso-ferric oxide/gold/Nano particles of silicon dioxide that one kind can use near infrared light Drug controlled release
Preparation method, it is characterised in that: steps are as follows:
A, it prepares nano ferriferrous oxide: taking Fe2+With Fe3+Molar ratio is 1:2, weighs FeSO respectively4·7H2O and FeCl3·
6H2O is dissolved in 20mL distilled water and carries out mechanical stirring, leads to nitrogen protection；NH is added dropwise into solution with the speed of 3 seconds/drop3·
H2O, round-bottomed flask is placed in stir 30 minutes in 80 DEG C of constant temperature water baths cure after being added dropwise；After reaction by sample
The separation of product externally-applied magnetic field, is washed 1 time, alcohol is washed 1 time, then is washed 4 times；By the sample freeze-drying after washing, four oxidations three are obtained
Iron；
B, it prepares ferroso-ferric oxide/gold nanoparticle: ferroso-ferric oxide made from step a and two citric acid monohydrate trisodiums is added
Into 200mL ultrapure water, ultrasonic disperse 10 minutes；The solution is heated with vigorous stirring to boiling, and rapidly joins HAuCl4It is molten
Liquid；Solution colour becomes brown from faint yellow immediately, eventually becomes red, continues stirring 15 minutes；By the additional magnetic of products obtained therefrom
Field separation, is washed 1 time, and alcohol is washed 1 time, and in triplicate, and freeze-drying obtains ferroso-ferric oxide/gold nanoparticle；
C, it prepares ferroso-ferric oxide/gold/Nano particles of silicon dioxide: weighing ferroso-ferric oxide/gold nanoparticle of step b preparation
Be dispersed in containing 0.3g cetyl trimethylammonium bromide, 80mL distilled water, 1.2mL ammonium hydroxide, 60mL ethyl alcohol mixed solution in,
By mixed solution ultrasonic disperse 30 minutes；0.5mL ethyl orthosilicate is added dropwise in the solution continuously stirred, reaction 6 is small
When；Products obtained therefrom Magneto separate is collected, is washed repeatedly with ethyl alcohol and distilled water and removes non magnetic by-product；By the product after washing
It is dispersed in the acetone soln of 50mL, flows back 6 hours at 65 DEG C, remove cetyl trimethylammonium bromide template；Gained is produced
Object ethyl alcohol and distilled water wash repeatedly, and freeze-drying obtains ferroso-ferric oxide/gold/Nano particles of silicon dioxide；
D, ferroso-ferric oxide/gold/Nano particles of silicon dioxide being dispersed in etoposide solution, 37 DEG C of constant temperature are stirred 6 hours,
Reach equilibrium state；It is separated with externally-applied magnetic field, the sample after load medicine is 12 hours dry at 60 DEG C；
E, it takes 40mg to carry medicine composite material, is placed in bag filter, and the phosphate-buffered that bag filter is put in 30mL difference pH is molten
Magnetic agitation is carried out in liquid, carries out near infrared light drug release under the conditions of 37 DEG C of Yu Hengwen；Release 300 minutes, every 30
Minute takes out 5mL solution, measures the content of Etoposide, while adding 5mL phosphate buffer solution；The content of Etoposide makes
It is measured at 285nm with ultraviolet specrophotometer, is accumulated according to the drug release that the Etoposide content of measurement calculates different time
Percentage.
2. a kind of core-shell structure ferroso-ferric oxide/gold/bis- that can use near infrared light Drug controlled release according to claim 1
The preparation method of silicon oxide nanoparticle, it is characterized in that: NH in the step a3·H2The concentration of O is 0.1 ~ 1mol/L.
3. a kind of core-shell structure ferroso-ferric oxide/gold/bis- that can use near infrared light Drug controlled release according to claim 1
The preparation method of silicon oxide nanoparticle, it is characterized in that: Etoposide concentration is 0.3mg/mL in the step d.
4. a kind of core-shell structure ferroso-ferric oxide/gold/bis- that can use near infrared light Drug controlled release according to claim 1
The preparation method of silicon oxide nanoparticle, it is characterized in that: the phosphate buffer solution of difference pH is by phosphoric acid hydrogen two in the step e
Sodium and sodium dihydrogen phosphate are formulated, and concentration is 0.1 ~ 0.2mol/L.
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