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
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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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