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Preparation method of functionalized polyethyleneimine-modified multi-wall carbon nano-tube magnetic resonance imaging contrast agent

A technology of multi-walled carbon nanotubes and polyethyleneimine, which is applied in the field of preparation of multi-walled carbon nanotubes magnetic resonance imaging contrast agents, can solve problems such as long blood circulation time, improve blood pool imaging quality, and expand application range Effect

Inactive Publication Date: 2014-01-08
DONGHUA UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] However, a search of literature and patents related to magnetic resonance imaging at home and abroad shows that: using functionalized polyethyleneimine-modified MWCNTs as a carrier material, a small-molecule gadolinium ion chelator is loaded on its surface through covalent grafting to achieve longer No studies on blood circulation time have been reported

Method used

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  • Preparation method of functionalized polyethyleneimine-modified multi-wall carbon nano-tube magnetic resonance imaging contrast agent
  • Preparation method of functionalized polyethyleneimine-modified multi-wall carbon nano-tube magnetic resonance imaging contrast agent
  • Preparation method of functionalized polyethyleneimine-modified multi-wall carbon nano-tube magnetic resonance imaging contrast agent

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] MWCNTs (100mg) were dispersed in 40mL of DMSO solution, and 10mL of DMSO solution containing EDC (120mg) was added with stirring, followed by 5mL of DMSO solution containing NHS (62mg), and the reaction was stirred at room temperature for 2h. Then 100 mg PEI (10 mL DMSO) was added dropwise to the DMSO solution of the EDC / NHS-activated MWCNTs, and the reaction was stirred for 2 days. Finally, put the reaction solution into a dialysis bag (MWCO=50,000), and remove the reaction solvent DMSO, excess reactants, and reaction by-products by dialysis, and dialyze three times with PBS buffer, 2L each time, and then dialyze with distilled water 5 times, 2L each time, and finally freeze-dry the aqueous solution of the product to obtain MWCNT / PEI;

[0056] Disperse 140 mg of prepared MWCNT / PEI in 50 mL of DMSO solution, add 8 mL of 4.85 mg of FI in DMSO solution dropwise under stirring, and stir at room temperature for 12 hours to obtain unpurified MWCNT / PEI-FI in DMSO solution; t...

Embodiment 2

[0064] T measured by in vitro MR 1 Value to test the MR imaging effect of the materials MWCNT / PEI-FI-DOTA(Gd) synthesized in Example 1, MWCNT / PEI-FI-DOTA(Gd)-mPEG2K and MWCNT / PEI-FI-DOTA(Gd)-mPEG5K. Take example 1 sample MWCNT / PEI-FI-DOTA (Gd) 8.46mg and dissolve it in 4.8mL of ultrapure water to prepare a solution with a gadolinium concentration of 0.892mM, then dilute it to a gadolinium concentration of 0.713, 0.535, 0.357, 0.178, 0.089 Each 1.5mL of the solution of mM; Get example 1 sample MWCNT / PEI-FI-DOTA (Gd)-mPEG2K11.52mg to be dissolved in the ultrapure water of 4.8mL and prepare the solution that gadolinium concentration is 0.675mM, then dilute to gadolinium concentration respectively 0.540, 0.405, 0.270, 0.135, each 1.5mL of 0.068mM solution; take example 1 sample MWCNT / PEI-FI-DOTA(Gd)-mPEG5K22.83mg and dissolve in 4.8mL of ultrapure water to prepare 0.876mM gadolinium concentration The solution was then diluted to 1.5mL each with gadolinium concentrations of 0.701,...

Embodiment 3

[0066] The cytotoxicity of the prepared material was investigated by MTT assay. Collect the logarithmic phase cells and add them to the 96-well cell culture plate, add 200 μL of cell-containing RPMI1640 medium to each well to make the cell density to 10000 / well, add 200 μL of sterile PBS buffer to the edge wells; then in the cell incubator (5 %CO 2 , 37°C) for 24 hours, until the cell monolayer covered the bottom of the well, discard the medium and add 180 μL of fresh medium, then add MWCNT / PEI-FI-DOTA(Gd), MWCNT / PEI-FI -20 μL PBS buffer solution of DOTA(Gd)-mPEG2K and MWCNT / PEI-FI-DOTA(Gd)-mPEG5K (each material is set to 7 concentrations based on gadolinium ion, namely 0, 2.5, 5, 10, 20, 40, 80μM) to verify the effect of the material itself on cell growth. All experimental groups were set up with 3 wells as a parallel group; after incubation in the incubator for 24 hours, 20 μL of MTT solution was added to each well, and the culture was continued for 4 hours to allow the ce...

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Abstract

The invention relates to a preparation method of a functionalized polyethyleneimine-modified multi-wall carbon nano-tube magnetic resonance imaging contrast agent. The method comprises the steps that: (1) MWCNT / PEI is prepared; (2) a DMSO solution of MWCNT / PEI-FI is prepared, and MWCNT / PEI-FI-DOTA (Gd) is prepared; and (3) MWCNT / PEI-FI-DOTA (Gd)-mPEG2K or MWCNT / PEI-FI-DOTA (Gd)-mPEG5K is finally prepared. The preparation process is simple, and the experiment conditions are normal temperature and normal pressure, such that operation is easy. The adopted preparation process can be used for preparing other functionalized multi-wall carbon nano-tube composite materials. According to the invention, mice in-vivo MR blood vessel and major organ imaging is realized. Also, with the EPR effect of tumor tissues, tumor site MR imaging detection can be realized. Therefore, the method has wide application prospect.

Description

technical field [0001] The invention belongs to the field of medical imaging contrast agents, in particular to a preparation method of a multi-walled carbon nanotube magnetic resonance imaging contrast agent modified by functionalized polyethyleneimine. Background technique [0002] Magnetic resonance imaging (MR) is a type of tomography (M.M.Britton, Chem.Soc.Rev.2010, 39, 4036.), which uses magnetic resonance phenomena to obtain electromagnetic signals from the human body and reconstruct human body information. It can obtain tomographic images in any direction, three-dimensional volume images, and even four-dimensional images of space-spectrum distribution. However, in order to achieve high detection sensitivity and high-definition images to complete early detection of diseases, the assistance of magnetic resonance imaging contrast agents (MRICA) is needed (E.L.Que, C.J.Chang, Chem. Soc. Rev. 2010, 39, 51.). MRICA is some paramagnetic and superparamagnetic substances, wh...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61K49/12
Inventor 史向阳温诗辉赵庆华安箫
Owner DONGHUA UNIV
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