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Method for preparing Gd3<+> magnetic resonance imaging contrast agent with graphene oxide serving as carrier

A magnetic resonance contrast agent, graphene technology, applied in the direction of nuclear magnetic resonance/magnetic resonance imaging contrast agent, etc., can solve the problems of inability to produce covalent bond interaction, strong electrostatic effect, poor load firmness, etc., to achieve clinical Application Potential, Firmness of Loading, Effect of Reduced Injection Dose

Inactive Publication Date: 2014-12-10
XI AN JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But this method still needs DTPA to chelate Gd 3+ , the reaction is more complex, and the electrostatic effect is greatly affected by the pH value of the environment; Li Yongyong et al. used graphene oxide modified by hydrophilic polymers as a nano-carrier to prepare a magnetic resonance contrast agent (CN102397563A), which was combined with Gd 3+ or gadolinium chelate (Gd 3+ -DTPA) cannot produce covalent bond interaction, adsorb Gd through physical interaction 3+ -DTPA, poor load firmness

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] 1) Graphene oxide prepared by Hummers oxidation method

[0038] At 0°C, take 1 part of natural flake graphite, 150 parts of concentrated sulfuric acid and 1.5 parts of sodium nitrate, mix well, and continue stirring for 20 minutes to obtain a mixed solution. 4 Slowly add dropwise to the above mixture, the temperature during the dropwise addition should not be higher than 20°C; after the dropwise addition, remove the ice bath, raise the temperature to 35°C, continue to stir and react for 0.5h, then add 280 parts of sulfuric acid with a mass concentration of 5% solution, heated up to 98°C, heated for 2 hours, cooled to 60°C, and added 6 parts of 30% H 2 o 2 , after stirring and reacting for 2h, graphene oxide was obtained;

[0039] 2) Carboxylation of graphene oxide

[0040] Under the action of ultrasonic waves, 1 part of graphene oxide was dispersed in distilled water, and after dispersing for 1 hour, the mass concentration was 2.5 mg·mL -1 Graphene oxide dispersion ...

Embodiment 2

[0046] 1) Graphene oxide was prepared by Hummers oxidation method

[0047] At 0°C, take 1 part of natural flake graphite, 150 parts of concentrated sulfuric acid and 1.5 parts of sodium nitrate, mix well, and continue to stir for 20 minutes to obtain a mixed solution. Add 3 parts of KMnO 4 Slowly add to the above mixture, and the temperature cannot be higher than 20°C during the addition process; remove the ice bath after the addition, raise the temperature to 35°C, continue stirring and reacting for 5 hours, add 280 parts of sulfuric acid solution with a mass concentration of 5%, and raise the temperature to 98°C, after heating for 2 hours, cool down to 60°C, and add 6 parts of 30% H 2 o 2 , after stirring and reacting for 2h, graphene oxide was obtained;

[0048] 2) Carboxylation of graphene oxide

[0049] Under the action of ultrasonic waves, 1 part of graphene oxide was dispersed in distilled water, and after dispersing for 1 hour, the mass concentration was 1.5 mg·mL ...

Embodiment 3

[0055] 1) Graphene oxide was prepared by Hummers oxidation method

[0056] At 0°C, take 1 part of natural flake graphite, 150 parts of concentrated sulfuric acid and 1.5 parts of sodium nitrate, mix well, and keep stirring for 20 minutes to obtain a mixed solution. 4 Slowly add to the above mixed solution, and the temperature cannot be higher than 20°C during the addition process; remove the ice bath after the addition, raise the temperature to 40°C, continue stirring and reacting for 12 hours, add 280 parts of sulfuric acid solution with a mass concentration of 5%, and heat up to 98°C, after heating for 1 hour, cool down to 60°C, and add 6 parts of 30% H 2 o 2 , after stirring and reacting for 2h, graphene oxide was obtained;

[0057] 2) Carboxylation of graphene oxide

[0058] Under the action of ultrasonic waves, 2 parts of graphene oxide were dispersed in distilled water, and after dispersing for 2 hours, a mass concentration of 0.5 mg·mL was obtained. -1 Graphene oxid...

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Abstract

The invention discloses a method for preparing a Gd3<+> magnetic resonance imaging contrast agent with graphene oxide serving as a carrier, and belongs to the technical field of preparation of medical materials. The method comprises the following steps of: 1) dispersing graphene oxide into distilled water to obtain a graphene oxide dispersing solution; 2) adding an alkaline substance and chloroacetic acid or sodium monochloroacetate to the graphene oxide dispersing solution, ultrasonically dispersing, centrifugally washing and processing, and dialyzing to obtain carboxylation graphene oxide; and 3) dispersing the carboxylation graphene oxide into the distilled water to obtain a carboxylation graphene oxide dispersing solution, adding an aqueous solution of gadolinium salt to the carboxylation graphene oxide dispersing solution, adding a DTPA (Diethylene Triamine Pentacetic Acid) aqueous solution after the stirring reaction is done, uniformly mixing to obtain a mixing solution, and dialyzing to obtain carboxylation graphene oxide with Gd3<+> loaded on the surface, thus obtaining the Gd3<+> magnetic resonance imaging contrast agent. The method is simple and feasible, and the Gd3<+> is firmly loaded; and the preparation magnetic resonance imaging contrast agent is high in water-borne dispersion stability and has high longitudinal relaxation rate.

Description

technical field [0001] The invention belongs to the technical field of medical material preparation, and relates to a preparation method of a magnetic resonance contrast agent, in particular to a Gd with graphene oxide as a carrier 3+ Preparation method of magnetic resonance contrast agent. Background technique [0002] Magnetic resonance molecular imaging technology has high resolution and can obtain anatomical and physiological information at the same time, which is beneficial to the diagnosis of diseases in vivo. Compared with iron oxide, Gd 3+ It has become a commonly used magnetic resonance contrast agent in clinical practice, mainly for the following reasons: ①Gd 3+ There is a half-full 4f layer with a large magnetic moment; ②The electron spin relaxation time is longer; ③The mechanism of action is to accelerate the relaxation of water protons to reflect positive results, which is easy to observe. [0003] However, free Gd 3+ Ions are toxic and must be used clinical...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): A61K49/08
Inventor 井新利任先艳刘丽华李瑜
Owner XI AN JIAOTONG UNIV
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