Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

A kind of preparation method of paramagnetic gadolinium-based metal fullerenol

A metallofullerene and paramagnetic technology, applied in the direction of nuclear magnetic resonance/magnetic resonance imaging contrast agents, etc., can solve the problems of large changes in the number of hydroxyl groups and large structural differences, and achieve convenient operation, reduced difficulty, and simple synthesis process Effect

Active Publication Date: 2021-06-18
HENAN AGRICULTURAL UNIVERSITY
View PDF3 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The number of hydroxyl groups in the paramagnetic gadolinium-based metallofullerol molecules formed by the above-mentioned methods varies greatly, and there are heteroatom groups on the surface of the paramagnetic gadolinium-based metallofullerol carbon cages reported by different researchers, resulting in huge structural differences.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • A kind of preparation method of paramagnetic gadolinium-based metal fullerenol
  • A kind of preparation method of paramagnetic gadolinium-based metal fullerenol
  • A kind of preparation method of paramagnetic gadolinium-based metal fullerenol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] 11.4mg Gd@C 82 Fully dissolved in 5mL o-dichlorobenzene, 2mL 5mol / L NaOH solution, 25μL 30%H 2 o 2 and 2 μL of 40% TBAH were fed into 25ml single-port reaction flasks respectively, layered, the lye was in the upper layer, and the o-dichlorobenzene phase was in the lower layer; the reaction system N 2 Protection, continuous stirring at 45°C for 48 hours and then stop the reaction; liquid separation, rotary evaporation under reduced pressure to remove the water phase; after washing the residue with methanol, redissolve in deionized water, and use a dialysis device with a molecular weight cut-off of 500-10000 Daltons The bag was dialyzed and freeze-dried to obtain a pure solid paramagnetic metallofullerol 1 with an average molecular formula of Gd@C 82 (OH) 34 , yield 100%.

[0036] The characterization information of paramagnetic metal fullerenol 1 is as follows:

[0037] Such as figure 1 As shown, the ion peak at m / z 1142 in MALDI-TOF MS belongs to Gd@C 82Carbon ca...

Embodiment 2

[0041] 11.4mg Gd@C 82 Fully dissolved in 5mL chlorobenzene, 2mL 1mol / L NaOH solution, 25μL 30% H 2 o 2 and 2 μL of 40% TBAH were respectively fed into a 25 ml single-port reaction bottle, and the reaction was stopped after heating and stirring at 30° C. for 10 hours; other conditions were the same as in Example 1 of the present invention. The pure product paramagnetic metal fullerenol 2 in the solid state is obtained, and its average molecular formula is Gd@C 82 (OH) 16 , yield 75%.

Embodiment 3

[0043] 11.4mg Gd@C 82 Fully dissolved in 5mL o-dichlorobenzene, 2mL 10mol / L NaOH solution, 25μL 30%H 2 o 2 and 2 μL of 40% TBAH were respectively fed into a 25 ml single-port reaction bottle, and the reaction was stopped after heating and stirring at 60° C. for 72 hours; other conditions were the same as in Example 1 of the present invention. The pure product paramagnetic metal fullerenol 3 in the solid state is obtained, and its average molecular formula is Gd@C 82 (OH) 40 , yield 100%.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a method for preparing a water-soluble paramagnetic gadolinium-based metal fullerene, the preparation method comprising the following steps: (1) dissolving paramagnetic gadolinium-based metal fullerene dissolved in an organic solvent and a strong alkali aqueous solution , hydrogen peroxide, and tetrabutylammonium hydroxide used as a phase transfer catalyst are respectively fed into the reaction vessel, layered, the upper layer is an aqueous phase, and the lower layer is an organic solvent phase; (2) under the protection of inert gas, the reaction system of step (1) was continuously stirred at 30-70°C for 10-72 hours to stop the reaction; (3) liquid separation, taking the aqueous phase to remove the solvent, to obtain crude The product is then refined to obtain a pure paramagnetic metal fullerenol solid product. The preparation method provided by the invention has simple and convenient process, simple subsequent purification method, convenient operation, and easy realization of high-efficiency and large-scale production; the obtained paramagnetic gadolinium-based metal fullerenol has good paramagnetic enhancement effect.

Description

technical field [0001] The invention belongs to the field of carbon nanometer materials, and relates to a liquid-phase reaction method for preparing paramagnetic gadolinium-based metal fullerenol used as a magnetic resonance imaging (MRI) contrast agent. Background technique [0002] The cage structure of fullerene molecules contains paramagnetic metallofullerenes containing metal gadolinium inside, which is the successor to the "star molecule" C 60 Then there is another class of typical representative carbon nanomaterials. Paramagnetic gadolinium-based metallofullerenes can react with hydroxylating reagents to generate paramagnetic gadolinium-based metallofullerene polyhydric water-soluble derivatives, namely paramagnetic gadolinium-based metallofullerenes. The paramagnetic gadolinium-based metal fullerene has good biocompatibility, and can also retain the paramagnetic properties of the original gadolinium-based metal fullerene molecule. At present, it has shown attractiv...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): A61K49/08
CPCA61K49/08
Inventor 何睿刘艳杰臧振峰毋青男王合中范宜康李爽
Owner HENAN AGRICULTURAL UNIVERSITY
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com