NL2025687B1 - Superparamagnetic iron oxide nanoclusters and preparation method and application thereof - Google Patents
Superparamagnetic iron oxide nanoclusters and preparation method and application thereof Download PDFInfo
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- WTFXARWRTYJXII-UHFFFAOYSA-N iron(2+);iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Fe+2].[Fe+3].[Fe+3] WTFXARWRTYJXII-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 57
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 43
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 42
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 19
- 239000002243 precursor Substances 0.000 claims description 16
- 238000005406 washing Methods 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- 238000007789 sealing Methods 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- 238000003860 storage Methods 0.000 claims description 8
- 238000001291 vacuum drying Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 4
- 235000017281 sodium acetate Nutrition 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 239000001632 sodium acetate Substances 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims 1
- 238000003384 imaging method Methods 0.000 abstract description 6
- 230000004044 response Effects 0.000 abstract description 6
- 238000002595 magnetic resonance imaging Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 2
- 229940044631 ferric chloride hexahydrate Drugs 0.000 abstract 2
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 abstract 2
- 239000012046 mixed solvent Substances 0.000 abstract 1
- 238000004729 solvothermal method Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 25
- 239000002245 particle Substances 0.000 description 12
- 238000001514 detection method Methods 0.000 description 7
- 206010028980 Neoplasm Diseases 0.000 description 6
- 230000002378 acidificating effect Effects 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000002086 nanomaterial Substances 0.000 description 6
- 239000002105 nanoparticle Substances 0.000 description 6
- 238000003745 diagnosis Methods 0.000 description 5
- 238000011160 research Methods 0.000 description 5
- 238000003760 magnetic stirring Methods 0.000 description 4
- 229940031182 nanoparticles iron oxide Drugs 0.000 description 4
- 238000011161 development Methods 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 210000001519 tissue Anatomy 0.000 description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 210000004027 cell Anatomy 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000000338 in vitro Methods 0.000 description 2
- 238000007885 magnetic separation Methods 0.000 description 2
- 238000013507 mapping Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000002560 therapeutic procedure Methods 0.000 description 2
- 208000010444 Acidosis Diseases 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- 230000007950 acidosis Effects 0.000 description 1
- 208000026545 acidosis disease Diseases 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000006907 apoptotic process Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 238000002512 chemotherapy Methods 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000012377 drug delivery Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000003018 immunoassay Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- -1 iron ions Chemical class 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 210000001165 lymph node Anatomy 0.000 description 1
- 230000005381 magnetic domain Effects 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000002122 magnetic nanoparticle Substances 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000006213 oxygenation reaction Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 238000004917 polyol method Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000002096 quantum dot Substances 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 210000000952 spleen Anatomy 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000017423 tissue regeneration Effects 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 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
- A61K49/00—Preparations for testing in vivo
- A61K49/06—Nuclear magnetic resonance [NMR] contrast preparations; Magnetic resonance imaging [MRI] contrast preparations
- A61K49/08—Nuclear magnetic resonance [NMR] contrast preparations; Magnetic resonance imaging [MRI] contrast preparations characterised by the carrier
- A61K49/10—Organic compounds
- A61K49/12—Macromolecular compounds
- A61K49/126—Linear polymers, e.g. dextran, inulin, PEG
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K49/00—Preparations for testing in vivo
- A61K49/06—Nuclear magnetic resonance [NMR] contrast preparations; Magnetic resonance imaging [MRI] contrast preparations
- A61K49/18—Nuclear magnetic resonance [NMR] contrast preparations; Magnetic resonance imaging [MRI] contrast preparations characterised by a special physical form, e.g. emulsions, microcapsules, liposomes
- A61K49/1818—Nuclear magnetic resonance [NMR] contrast preparations; Magnetic resonance imaging [MRI] contrast preparations characterised by a special physical form, e.g. emulsions, microcapsules, liposomes particles, e.g. uncoated or non-functionalised microparticles or nanoparticles
- A61K49/1887—Agglomerates, clusters, i.e. more than one (super)(para)magnetic microparticle or nanoparticle are aggregated or entrapped in the same maxtrix
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide [Fe3O4]
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Radiology & Medical Imaging (AREA)
- Epidemiology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Organic Chemistry (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Veterinary Medicine (AREA)
- Nanotechnology (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Medicinal Chemistry (AREA)
- Medicines Containing Antibodies Or Antigens For Use As Internal Diagnostic Agents (AREA)
- Compounds Of Iron (AREA)
Abstract
The present invention discloses a superparamagnetic iron oxide nanoclusters and a preparation method and an application thereof. The superparamagnetic iron oxide nanoclusters are synthesized by an improved solvothermal method, ferric chloride hexahydrate (FeC1306H20) is used as a raw material, a cluster-shaped product Fe304 is synthesized by a hydrothermal method, and a size of the cluster-shaped product Fe304 is adjustable within a range of 60-200 nm by changing a proportion of a mixed solvent. Because of characteristics of good biocompatibility, unique magnetic characteristic, pH response and the like, the superparamagnetic iron oxide nanoclusters prepared by the present invention not only can be used as a Magnetic Resonance Imaging (MRI)-T2 weighted nanoprobe for magnetic resonance molecular imaging, but also has the characteristic of pH response.
Description
FIELD OF TECHNOLOGY The present invention belongs to the technical field of nano magnetic materials, and relates to a superparamagnetic iron oxide nanoclusters and a preparation method and an application thereof.
BACKGROUND ART In the prior art, along with rapid development of manufacturing, assembly and modification technologies, the application of nanomaterials shows a bright future in the high and new technical fields, such as high-sensitivity and high-selectivity separators and sensors, etc. The research on unique physical properties and mechanisms of the nanomaterials and the utilization on characteristics of the nanomaterials are constituted into core contents of nanoscience and nanotechnology. In recent years, owing to the development of the nanomaterials and particularly novel nanoparticles for cancer diagnosis and treatment, the nanobiotechnology has made an unprecedented progress in aspects of magnetic separation between proteins and cells, replacement of fluorescems by quantum dot, and research, development and medical diagnosis of magnetic- resonance molecular imaging probes. Superparamagnetic Iron Oxide Nanoparticles (SPIONs) are nanomaterials that are most functional and researched in biomedical application. With a high biocompatibility, a negligible toxicity to healthy tissues and excellent surface chemical properties, the SPIONs have been widely applied to Magnetic Resonance Imaging (MRI), tissue repair, immunoassay, thermal therapy, drug delivery and cell separation. As a magnetic nanoparticle, nano Fe;O, has a single magnetic domain structure and a very high coercivity; and when prepared into a magnetic recording material, it may improve a signal-to-noise ratio and improve the image quality. Because of such characteristics as a high saturated magnetization intensity, the Fe;O4 nanoparticles are often used for magnetic- resonance T2 weighed imaging, Till now, many processes for preparing the nano Fe;O, have been researched by people, including a coprecipitation method. a sol-gel method, a micro-emulsion method, a microwave synthesis method, a polyol method, a mechanical grinding method, a pyrolysis method. a hydrothermal method, etc. The SPIONSs are widely applied to the field of biomedicine, for example, as MRI-T2 weighed imaging nanomaterial, they are used in imaging of livers and spleens, lymph nodes, tumors and other tissues, and magnetic-heat treatment, magnetic separation, and tumor diagnosis and treatment. Different from normal tissues, the Tumor Microenvironment (TME) has the characteristics of non-uniform nutritional distribution, insufficient oxygenation (oxygen deprivation), acidic pH (acidosis) and high redox state, thus leads to weakly acidic environment. In case of synthesis of the Fe;0, nanoparticles that have the MRI-T2 weighed imaging characteristic and the TME response characteristic, and can be dissociated into undersized nanoparticles in a weakly acidic condition to penetrate into a deep tumor part to release iron ions, and thus accelerates apoptosis of tumor cells in combination with other therapies such as a chemotherapy, it will be of a great significance to integrated research of tumor diagnosis and treatment. However, the Fe;Oy researched and synthesized at present fails to have the TME response characteristic.
SUMMARY One technical problem to be solved by the present invention is to research and develop a superparamagnetic iron oxide nanoclusters and a preparation method and an application thereof for the above shortages of the prior art. Fe;Qy synthesized by the method has a controllable size, and the nanoclusters may respond to a weakly acidic TME. To achieve the above objective, the present invention researches and develops the following technical solutions: A preparation method of a superparamagnetic iron oxide nanoclusters includes the following steps: (1) weighing FeCl;+6H,0 in a container, adding an Ethylene Glycol (EG) solution and a Diethylene Glycol (DEG) solution, and magnetically stirring to dissolve the FeCl;*6H,0; (2) adding Polyacrylic Acid (PPA) to a solution, and stirring to dissolve the PPA; (3) adding sodium acetate (CH:COONa) and sodium hydroxide (NaOH), stirring, and heating to dissolve the CH;COONa and the NaOH to form a precursor; (4) transferring the above precursor to a hydrothermal reactor, sealing the hydrothermal reactor, then putting into a blast drying oven, heating to 180-280°C, and after 4-16 h of reaction, closing the blast drying oven and cooling naturally; and (5) taking out a colloidal product, adding anhydrous ethanol and water, ultrasonically washing, separating with a magnet, and washing and separating once again with a same method; and placing a separated solid into a vacuum drying oven and drying for 12-36 h at a room temperature, and sealing obtained Fe; 0, dry powder for storage. In the above solutions, a total volume of the EG and DEG solutions 1s 30 mL, and a ratio of the EG solution to the DEG solution is 30/0-10/20 by volume (v/v). Preferably, a preparation method of a superparamagnetic iron oxide nanoclusters includes the following steps:
(1) weighing FeCl;*6H,0 in a beaker, adding an EG solution and a DEG solution, and magnetically stirring for 10 min to dissolve the FeCl;*6H,0; (2) adding PPA to a solution, and stirring for 30 min to dissolve the PPA; (3) adding CH;COONa and NaOH, stirring for 40 min, and heating to dissolve the CH3COONa and the NaOH to form a precursor; (4) transferring the above precursor to a hydrothermal reactor, sealing the hydrothermal reactor, then putting into a blast drying oven, heating to 210°C, and after 10 h of reaction, closing the blast drying oven and cooling naturally: and (5) taking out a colloidal product, adding anhydrous ethanol and water, ultrasonically washing, separating with a magnet, and washing and separating once again with a same method; and placing a separated solid into a vacuum drying oven and drying for 24 h at a room temperature, and sealing obtained Fe:O, dry powder for storage.
The present invention has the following advantages:
1. The present invention is simple and easy in operation, and low in raw material cost: and synthesis reaction is carried out in an airtight environment, thereby being environment-friendly. 2. The synthesized nanoclusters has strong size controllability, and good monodispersity and biocompatibility. 3. The synthesized nanoclusters has a pH response characteristic, may be decomposed into iron oxide nanoparticles of different particle sizes in different pH conditions, and shows different T2 signal intensities and T2 relaxation rates on MR. 4. The synthesized nanoclusters have a high T2 relaxation rate, which provides new method and technology for MR diagnosis or treatment.
BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a schematic diagram of a preparation route according to the present invention.
Fig. 2 is a Scanning Electron Microscope (SEM) image of SPIONSs of different particle sizes.
Fig. 3 is a phantom in-vitro MR image of SPIONSs in different pH conditions.
Fig. 4 is a value of a T2 relaxation rate measured in different pH conditions.
DETAILED DESCRIPTION OF THE EMBODIMENTS Embodiment | A preparation method of a superparamagnetic iron oxide nanoclusters includes the following steps: (1) 0.2162 g of FeCl;+6H,0 was weighed in a beaker, an EG solution and a DEG solution were added, and magnetic stirring was carried out for 10 min to dissolve the FeCl;*6H,0, a ratio of the
EG to the DEG being 30 mL to 0 mL by volume. (2) 0.5794 g of PPA was added to a solution, and dissolved with stirring for 30 min. (3) 2.5874 g of CH3COONa and 0.1402 g of NaOH were added and dissolved with stirring for 40 min and appropriate heating to form a precursor.
(4) The above precursor was transferred to a hydrothermal reactor; the hydrothermal reactor was sealed, put into a blast drying oven, heated to 210°C; and after 10 h of reaction, the blast drying oven was closed and cooled naturally.
(5) A colloidal product was taken out, 100 mL of anhydrous ethanol and water were added, ultrasonic washing was carried out for 5 min, a magnet was used for separating, and a same method was used for washing and separating once again; and a separated solid was placed into a vacuum drying oven and dried at a room temperature, and obtained Fe;O, dry powder was sealed for storage. Thereafter, further detection on particle size, shape and MR performance was carried out, with a specific result as shown in Fig. 2 (200 nm).
During synthesis, the PPA is used as a stabilizer, and a synthesized Fe30, particle is self- assembled under a cross-linking action of the PPA to form the nanoclusters; and as the PPA has pH response characteristic, the svnthesized nanoclusters may be decomposed into iron oxide nanoparticles of different particle sizes in different pH conditions.
By controlling different volume ratios of the EG to the DEG, the synthesized Fe30: has a controllable size.
In an acidic condition, the PPA cross-linked on a surface of the nanoclusters is dissociated, and the covered Fe;0, nanoparticles are separated into nanoparticles of a smaller size from the clusters. Therefore. the nanoclusters may respond to a weakly acidic TME.
Embodiment 2 A preparation method of a superparamagnetic iron oxide nanoclusters includes the following steps: (1) 0.2162 g of FeC:1::6H;0 was weighed in a beaker, an EG solution and a DEG solution were added, and magnetic stirring was carried out for 10 min to dissolve the FeCl;+6H,0, a ratio of the EG to the DEG being 20 mL to 10 mL by volume.
(2) 0.5794 g of PPA was added to a solution, and dissolved with stirring for 30 min.
(3) 2.5874 g of CH:COONa and 0.1402 g of NaOH were added and dissolved with stirring for 40 min and appropriate heating to form a precursor.
(4) The above precursor was transferred to a hydrothermal reactor; the hydrothermal reactor was sealed, put into a blast drying oven, heated to 210°C; and after 10 h of reaction, the blast drving oven was closed and cooled naturally.
(5) A colloidal product was taken out, 100 mL of anhydrous ethanol and water were added. ultrasonic washing was carried out for 5 min, a magnet was used for separating, and a same method was used for washing and separating once again; and a separated solid was placed into a vacuum drying oven and dried for 24 h at a room temperature, and obtained Fe:O, dry powder was sealed 5 for storage. Thereafter, further detection on particle size, shape and MR performance was carried out, Thereafter, further detection on particle size, shape and MR performance was carried out, with a specific result as shown in Fig. 2 (140 nm).
Embodiment 3 A preparation method of a superparamagnetic iron oxide nanoclusters includes the following steps: (1) 0.2162 g of FeC;:6H;0 was weighed in a beaker, an EG solution and a DEG solution were added. and magnetic stirring was carried out for 10 min to dissolve the FeCl;6H;0. a ratio of the EG to the DEG being 15 mL to 15 mL by volume.
(2) 0.5794 g of PPA was added to a solution, and dissolved with stirring for 30 min.
(3) 2.5874 g of CH;COONa and 0. 1402 g of NaOH were added and dissolved with stirring for 40 min and appropriate heating to form a precursor.
(4) The above precursor was transferred to a hydrothermal reactor; the hydrothermal reactor was sealed, put into a blast drying oven, heated to 210°C; and after 10 h of reaction, the blast drying oven was closed and cooled naturally.
(5) A colloidal product was taken out, 100 mL of anhydrous ethanol and water were added, ultrasonic washing was carried out for 5 min, a magnet was used for separating, and a same method was used for washing and separating once again; and a separated solid was placed into a vacuum drying oven and dried for 24 h at a room temperature, and obtained FeO, dry powder was sealed for storage. Thereafter, further detection on particle size, shape and MR performance was carried out. with a specific result as shown in Fig. 2 (80 nm).
Embodiment 4 A preparation method of a superparamagnetic iron oxide nanoclusters includes the following steps: (1) 0.2162 g of FeCl;+6H,0 was weighed in a beaker, an EG solution and a DEG solution were added, and magnetic stirring was carried out for 10 min to dissolve the FeCl;*6H,0, a ratio of the EG to the DEG being 10 mL to 20 mL by volume.
(2) 0.5794 g of PPA was added to a solution, and dissolved with stirring for 30 min.
(3) 2.5874 g of CH;COONa and 0. 1402 g of NaOH were added and dissolved with stirring for 40 min and appropriate heating to form a precursor.
(4) The above precursor was transferred to a hydrothermal reactor; the hydrothermal reactor was sealed, put into a blast drying oven, heated to 210°C; and after 10 h of reaction, the blast drying oven was closed and cooled naturally. (5) A colloidal product was taken out, 100 mL of anhydrous ethanol and water were added, ultrasonic washing was carried out for 5 min, a magnet was used for separating, and a same method was used for washing and separating once again; and a separated solid was placed into a vacuum drying oven and dried for 24 h at a room temperature, and obtained Fe;O, dry powder was sealed for storage. Thereafter, further detection on particle size, shape and MR performance was carried out, with a specific result as shown in Fig. 2 (60 nm).
Experimental Example | In-vitro MRI detection of superparamagnetic iron oxide nanoclusters: a superparamagnetic iron oxide nanoclusters having a particle size of 60 nm was used, and respectively prepared, in a PBS or diluted hydrochloric acid solution having a pH value of 7.4/6.5/5.5, into 200 pL of superparamagnetic iron oxide nanoclusters aqueous solution having a concentration of 50 pg Fe/mL, 25 ug Fe/mL, 12.5 pg Fe/mL, 6.25 ug Fe/mL and 3.125 pg Fe/mL; and the solution was loaded into an EP tube having a capacity of 250 uL, and a T2 image and a T2 mapping were detected by a 9.4 T MR scanner. The 9.4 T MR scanner uses the following scanning parameters: TurboRARE-T2 has repetition time=2000 ms, echo time=8 ms, FOV=60*32 mm, thickness=1 mm, matrix=256*256 and the Number of Excitation (NEX)=1; and the RARE-T2 mapping has repetition time= 2000 ms, echo time=8-64 ms, FOV=60*32 mm, thickness=1 mm, matrix=256*256 and NEX=I1. Upon the completion of test, image data was processed, and determination of a relaxation rate and contrast in T2 signal enhancement were carried out in different pH conditions. Thereafter, further detection on particle size, shape and MR performance was carried out, with a specific result as shown in Fig. 3 and Fig. 4.
The present invention is simple and easy in operation, and low in raw material cost. The synthesized nanoclusters have good monodispersity and biocompatibility. The synthesized nanoclusters may be decomposed into iron oxide nanoparticles of different particle sizes in different pH conditions, and shows different T2 signal intensities and T2 relaxation rates on MR.
The above descriptions are merely specific embodiments of the present invention, and various illustrations are not intended to limit a substantial content of the present invention.
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