Paramagnetic fullerene-metal nano complex as well as preparation method and application thereof

A technology of fullerene-based nanometers and metal nanometers, which is applied in the field of carbon nanomaterials, can solve the problems of lack of synthesis methods for paramagnetic gadolinium-based metallofullerenes and their water-soluble derivatives, and achieve good water solubility and synthetic process operation Simple, efficient results

Active Publication Date: 2019-12-31
HENAN AGRICULTURAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the bottleneck in the application research of gadolinium-based metallofullerene-based MRI nanoprobes lies in the lack of economical and reasonable macro-scale preparation of paramagnetic gadolinium-based metallofullerenes and their water-soluble derivatives.

Method used

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  • Paramagnetic fullerene-metal nano complex as well as preparation method and application thereof
  • Paramagnetic fullerene-metal nano complex as well as preparation method and application thereof
  • Paramagnetic fullerene-metal nano complex as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Example 1: Preparation C 60 (NCH 2 CH 2 OCH 2 CH 2 Oh) 8 -Mn complex

[0033] 360mg C 60 with liquid N 3 CH 2 CH 2 OCH 2 CH 2 OH is sequentially fed into the three-necked reaction flask according to the stoichiometric ratio (molar ratio) 1:100, protected by nitrogen, mechanically stirred, controlled heating rate 1°C / min, slowly raised to 120°C, kept for 24 hours, stopped the reaction, and cooled the product to room temperature Dissolve in 500ml of water, filter, concentrate, dialyze with a molecular weight cut-off 500 dialysis bag, filter again, and freeze-dry to obtain solidified fullerene-based nano-ligand 1; mix 0.1544g of fullerene-based nano-ligand 1 with 0.186g of Manganese acetate hydrate was dispersed in 200ml of methanol according to the molar ratio of 1:10, isolated from the air, refluxed for 12 hours, and the reaction was terminated. After distilling off the methanol, it was redissolved in water, dialyzed in a dialysis bag with a molecular weight c...

Embodiment 2

[0039] Example 2: Preparation C 70 (NCH 2 CH 2 OCH 2 CH 2 Oh) 10 -Mn complex

[0040] With reference to embodiment 1, 420mg C 70 with liquid N 3 CH 2 CH 2 OCH 2 CH 2 OH is sequentially fed into a three-necked reaction flask according to a stoichiometric ratio (molar ratio) of 1:100, and all the other conditions are the same as in Example 1 of the present invention to obtain a pure fullerene-based nano ligand 2 solid product, and its average molecular formula is characterized by thermogravimetric analysis: C 70 (NCH 2 CH 2 OCH 2 CH 2 Oh) 10 . Further obtain fullerene-manganese nanocomplex 2 product C after the operation chelation according to embodiment 1 70 (NCH 2 CH 2 OCH 2 CH 2 Oh) 10 -Mn.

Embodiment 3

[0041] Example 3: Preparation C 60 (NCH 2 CH(OH)CH 2 Oh) 10 -Mn complex

[0042] With reference to embodiment 1, the 360mg C 60 with liquid N 3 CH 2 CH(OH)CH 2 OH is sequentially fed into a three-necked reaction flask according to a stoichiometric ratio (molar ratio) of 1:100, and the remaining conditions are the same as in Example 1 of the present invention to obtain a pure fullerene-based nano ligand 3 solid product, and its average molecular formula is characterized by thermogravimetric analysis: C 60 (NCH 2 CH(OH)CH 2 Oh) 10 . Further obtain fullerene-manganese nanocomplex 3 product C after the operation chelation according to embodiment 1 60 (NCH 2 CH(OH)CH 2 Oh) 10 -Mn.

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Abstract

The invention discloses a paramagnetic fullerene-metal nano complex as well as a preparation method and application thereof. The paramagnetic fullerene-metal nano complex is prepared from a fullerene-based nano ligand and an inorganic metal salt through a chelation reaction; the inorganic metal salt is one of manganese sulfate, manganese nitrate, manganese chloride, manganese carbonate, manganeseacetate, gadolinium sulfate, gadolinium nitrate and gadolinium chloride; the fullerene-based nano ligand is formed by linking side chains to the surfaces of carbon cages of fullerene through nitrogenbridges, and each carbon cage is averagely linked with 6-18 side chains; the side chain is selected from chains disclosed in the invention. The paramagnetic fullerene-metal nano complex is good in water solubility and excellent in paramagnetic performance, has a remarkable effect of enhancing MRI imaging contrast when being used as an MRI nano probe, and has an important application prospect in the technical field of nano diagnosis and treatment.

Description

technical field [0001] The invention belongs to the field of carbon nanomaterials, and relates to a class of water-soluble paramagnetic fullerene-metal nanocomplexes and their preparation methods and applications. The water-soluble paramagnetic fullerene-metal nanocomplexes can be used as magnetic resonance Imaging (MRI) probes. Background technique [0002] MRI relies on nanomaterials to develop high-efficiency and low-toxic paramagnetic MRI nanoprobes to realize malignant tumor diagnosis and / or early image-mediated therapy. one. Among them, among the paramagnetic carbon-based MRI nanoprobes, the most common in the scientific literature is the gadolinium-based metallofullerene MRI nanoprobe. These probes are all Gd@C 82 、Gd 3 N@C 80 、Gd 3 N@C 84 Hydroxylation, amination, and Bingel derivatives of fullerenes such as gadolinium. For example, Gd 3 N@C 80 (OH) 30 (CH 2 CH 2 COOH) 20 、Gd 3 N@C 80 (OH) x (NH 2 ) y 、Gd@C 82 (OH) x (CH 2 CH 2 COOH) y and Gd@...

Claims

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Application Information

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IPC IPC(8): C07F13/00A61K49/08A61K49/10
CPCA61K49/085A61K49/103C07F13/00
Inventor 何睿臧振锋刘艳杰毋青男王合中刘育科李玥
Owner HENAN AGRICULTURAL UNIVERSITY
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