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Graphene quantum dots and gadolinium ion chelate magnetic resonance contrast agent and preparation method thereof

A technology of graphene quantum dots and chelates, which is applied in the direction of nuclear magnetic resonance/magnetic resonance imaging contrast agents, graphene, general/multifunctional contrast agents, etc. Insufficient weighted contrast effect, high gadolinium content and other problems, to achieve excellent weighted contrast performance, easy surface modification, and uniform size

Active Publication Date: 2021-11-12
ANHUI UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantage of this method is that the cost of raw materials is expensive, the structure of the obtained composite of carbon quantum dots and gadolinium is very unclear, and the content of gadolinium and the amount used in imaging are high, which will have a great impact on the organism in the later stage
More importantly, the longitudinal relaxation rate r of the contrast agent 1 should be much smaller than the r of the contrast agent of the present invention 1 , so its T 1 The weighted contrast effect is far inferior to the patented technology of the present invention

Method used

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  • Graphene quantum dots and gadolinium ion chelate magnetic resonance contrast agent and preparation method thereof
  • Graphene quantum dots and gadolinium ion chelate magnetic resonance contrast agent and preparation method thereof
  • Graphene quantum dots and gadolinium ion chelate magnetic resonance contrast agent and preparation method thereof

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Embodiment 1

[0040] A kind of preparation method of graphene quantum dot and gadolinium ion chelate specifically comprises the following steps:

[0041] 1) Graphene oxide was prepared using the Hummers method (this method is cited from the literature: ACS Nano, 2010, 4(8), 4806–4814.);

[0042] 2) Weigh 20 mg of the above-mentioned graphene oxide, dissolve it in 60 g of deionized water, treat it with an ultrasonic power of 500 W, and then add 60 g of hydrogen peroxide to fully dissolve it;

[0043] 3) Add 1000 μL of hydrazine hydrate solution to the above solution, then transfer the above solution to a round bottom flask, and reflux in an oil bath at 100°C for 8 hours;

[0044] 4) After the reflux reaction is completed, the above solution is filtered and purified to remove large impurities, and then dried at high temperature (80°C) to obtain GQDs, which have a two-dimensional regular shape, uniform size, and a lateral size of 3- Between 6nm, thickness between 1-2nm, non-excitation light-d...

Embodiment 2

[0056] A kind of preparation method of graphene quantum dot and gadolinium ion chelate specifically comprises the following steps:

[0057] 1) using the Hummers method to prepare graphene oxide;

[0058] 2) Weigh 60 mg of the above graphene oxide, dissolve it in 60 g of deionized water, treat it with an ultrasonic power of 800 W, and then add 60 g to a concentration of 1 mol L -1 The potassium persulfate solution is fully dissolved;

[0059] 3) Add 800 μL of ammonia solution to the above solution, then transfer the above solution to a round bottom flask, and reflux in an oil bath at 70°C for 12 hours;

[0060] 4) After the reflux reaction is completed, the above solution is subjected to chromatographic purification to remove bulk impurities, and then to freeze-drying to obtain GQDs;

[0061] 5) Prepare the GQDs prepared above to a concentration of 0.2 mg mL -1 solution, then add gadolinium chloride, control gadolinium chloride solution concentration is 0.2mmol L -1 , carry...

Embodiment 3

[0064] A kind of preparation method of graphene quantum dot and gadolinium ion chelate specifically comprises the following steps:

[0065] 1) using the Hummers method to prepare graphene oxide;

[0066] 2) Weigh 60 mg of the above-mentioned graphene oxide, dissolve it in 60 g of deionized water, and process it with an ultrasonic power of 600 W, then add a mixture of 20 g of concentrated sulfuric acid and concentrated nitric acid to fully dissolve;

[0067] 3) Add 400 μL, 1mol L to the above solution -1 Sodium hydroxide solution, then transfer the above solution to a round bottom flask, and reflux in an oil bath at 80°C for 10h;

[0068] 4) After the reflux reaction is completed, the above solution is subjected to suction filtration and purification to remove bulk impurities, and then to vacuum drying to obtain GQDs;

[0069] 5) Prepare the GQDs prepared above to a concentration of 0.05 mg mL -1 solution, then add gadolinium chloride to control its solution concentration to...

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Abstract

The invention discloses graphene quantum dots and gadolinium ion chelates (Gd@GQDs), which belong to the field of nanomaterials. The graphene quantum dots and gadolinium ion chelates are nanomaterials with hydrophilic groups on the surface; their preparation The method is to use the Hummers method to prepare graphene oxide, then heat oxidation and purification to obtain pure graphene quantum dots, and finally combine with Gd 3+ Chelation forms stable Gd@GQDs. The Gd@GQDs prepared by the present invention are easily dispersed in aqueous systems such as water, phosphate buffered saline (PBS), and biological culture medium; they have good biocompatibility and low toxicity; in a 1.5T magnetic resonance test system, they exhibit Excellent T 1 weighted contrast performance, its r 1 Relaxation rate up to 72mM ‑1 the s ‑1 , compared to existing commercial T 1 r of weighted magnetic resonance contrast agent Gd‑DTPA 1 twenty times higher.

Description

technical field [0001] The invention relates to a graphene quantum dot and gadolinium ion chelate magnetic resonance contrast agent and a preparation method thereof, belonging to the technical field of new nanometer materials. Background technique [0002] Magnetic resonance imaging (MRI) is one of the most widely used diagnostic tools in clinical applications. MRI has many advantages, such as noninvasiveness, high spatial and temporal resolution, and good soft tissue contrast. Still, the intrinsic signal differences between tissues, especially between diseased and normal tissues, are not that great. Therefore, an MRI contrast agent is usually injected before the scan to improve image quality. According to the principle of action, MRI contrast agents can be divided into longitudinal relaxation contrast agents (T 1 contrast agent) and transverse relaxation contrast agent (T 2 contrast agent). Most commonly used T 1 The contrast agent is a gadolinium-based contrast agent...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): A61K49/00A61K49/08
CPCA61K49/0002A61K49/0019A61K49/085C09K11/65C01B32/15C01B32/182B82Y30/00B82Y25/00C09K11/025C01B32/198B82Y5/00B82Y20/00B82Y40/00C01P2004/04C01P2004/64C01P2004/80C01P2006/60C01P2006/82
Inventor 毕红王东
Owner ANHUI UNIVERSITY
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