Preparation method and application of gadolinium sodium sulfate

A technology of gadolinium sodium sulfate and sulfuric acid is applied in chemical instruments and methods, rare earth metal sulfates, inorganic chemistry, etc., which can solve the problems of inability to use nuclear magnetic resonance contrast agents, unstable phases, and difficult to discharge, and achieve obvious contrast effects. , the preparation method is simple and easy to implement, and the cost is low.

Active Publication Date: 2017-05-31
QINGDAO UNIV OF SCI & TECH
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  • Abstract
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Problems solved by technology

[0004] At present, the research on Gd-based contrast agents is the most extensive. Researchers use various methods to incorporate Gd into different substrate materials such as: DTPA, DOPA, polyamine polycarboxylate complexes, monoclonal antibodies, polysaccharides, macromolecules Polymers, etc. to form contrast agents, but when the above materials are injected into living organisms, they are easy to accumulate in the liver, spleen and bones, and are not easy to be excreted, and have high toxicity
[0005] Sodium gadolinium sulfate has water solubility and is easily absorbed by tissues, but in the prior art, sodium gadolinium sulfate is generally obtained by separating sodium gadolinium sulfate in the form of intermediate products in rare earth ores, and the obtained sodium gadolinium sulfate is industrial-grade sodium gadolinium sulfate, with low purity and good phase Unstable and cannot be used as an MRI contrast agent

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  • Preparation method and application of gadolinium sodium sulfate
  • Preparation method and application of gadolinium sodium sulfate
  • Preparation method and application of gadolinium sodium sulfate

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[0025] The invention provides a kind of preparation method of sodium gadolinium sulfate, comprises the following steps:

[0026] Mixing gadolinium salt solution, ethylene glycol and polyvinylpyrrolidone to obtain a mixed solution;

[0027] The ethanol solution of sulfuric acid and the aqueous solution of sodium hydroxide are added into the mixed solution in sequence, and the solvothermal reaction is carried out to obtain sodium gadolinium sulfate.

[0028] The invention mixes gadolinium salt solution, ethylene glycol and polyvinyl pyrrolidone to obtain a mixed solution. In the present invention, the gadolinium salt is preferably gadolinium nitrate and / or gadolinium chloride; the concentration of the gadolinium salt solution is preferably 0.1-1 mol / L, more preferably 0.3-0.6 mol / L. In the present invention, the K value of the polyvinylpyrrolidone is preferably 30-60, more preferably 40-50. In the present invention, the mass ratio of the amount of gadolinium salt, the volume o...

Embodiment 1

[0041] Accurately weigh 2.0 mL of 1 mol / L gadolinium nitrate solution, add it to 27 mL of ethylene glycol, then add 1.0 g of polyvinylpyrrolidone (PVP, K30), stir for 10 minutes until the PVP is completely dissolved, and obtain a mixed solution;

[0042] Disperse 0.08g of concentrated sulfuric acid into 10mL of absolute ethanol to obtain an ethanol solution of sulfuric acid, add the ethanol solution of sulfuric acid dropwise to the mixed solution, after the ethanol solution of sulfuric acid has been added dropwise, oxidize the hydrogen with a concentration of 0.008g / ml Add the sodium solution dropwise into the mixed solution, stir at room temperature for 30 minutes, transfer the mixed solution to a high-pressure reactor and place it at 200°C for 18 hours; after the reaction is completed, wash the mixed solution with water and alcohol, and centrifuge at a speed of 3000r / min Three times, each centrifugation time is 5 minutes, and the centrifuged product is dried at 60° C. for 24 ...

Embodiment 2

[0047] Use the MTT method to evaluate the NaGd(SO) that embodiment 1 makes 4 ) 2 Cytotoxicity, the experimental steps are as follows:

[0048] (1) Inoculate human cervical cancer cells (HeLa cells) in a 96-well culture plate at a density of 4000-6000 cells / well, and cultivate them in a cell incubator for 24 hours (5% CO 2 , 37°C);

[0049] (2) Weigh an appropriate amount of prepared NaGd(SO 4 ) 2 After the sample was dissolved in water, it was dispersed in an appropriate amount of cell culture medium, so that NaGd(SO 4 ) 2 The mass concentration is 31.25~500μg / mL;

[0050] (3) Take the NaGd(SO 4 ) 2 Each 100 μL was injected into a 96-well culture plate, 6 wells for each concentration, and co-cultured with human cervical cancer cells for 12 hours (5% CO 2 , 37°C);

[0051] (4) Aspirate the NaGd(SO4) in the 96-well culture plate 4 ) 2 , add 20 μL tetramethylazotrilium salt (MTT) to each well, and continue culturing for 4 hours (5% CO 2 , 37°C);

[0052] (5) Termina...

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Abstract

The invention provides a preparation method of gadolinium sodium sulfate. The preparation method comprises the following steps: mixing a gadolinium salt solution, ethylene glycol and polyvinylpyrrolidone to obtain a mixed solution; adding a mixed solution of sulfuric acid and absolute ethyl alcohol and a sodium hydroxide solution into the mixed solution for solvothermal reaction to obtain the gadolinium sodium sulfate. The preparation method of the gadolinium sodium sulfate, which is provided by the invention, is simple and feasible; the raw materials are readily available and low-cost; furthermore, the obtained gadolinium sodium sulfate is high in purity, high in crystallizing degree and stable in phase; an aqueous solution of the gadolinium sodium sulfate is high in nuclear magnetic signal strength, and is suitable for being prepared into a T1 contrast agent of nuclear magnetic resonance. An experimental result shows that the purity of the gadolinium sodium sulfate prepared through the method can reach 99.9 percent.

Description

technical field [0001] The invention relates to the technical field of nuclear magnetic resonance imaging agents, in particular to a preparation method and application of sodium gadolinium sulfate. Background technique [0002] Nuclear Magnetic Resonance Imaging (MRI) refers to the principle that the nuclear magnetic resonance generated by the atomic nucleus has different relaxation speeds in different media, and the intensity of the detected signal is converted into a light-dark contrast image to distinguish different substances. Structural technology. [0003] The relaxation times of some different tissues or tumors overlap each other, which makes diagnosis difficult, and dynamic scanning and organ function measurement cannot be performed. In the prior art, contrast agents are usually used to enhance signal contrast and improve the resolution of soft tissue images. Contrast agent is an imaging-enhanced contrast agent that reduces imaging time to improve the contrast and c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F17/00A61K49/06
CPCA61K49/06C01F17/282C01P2002/72C01P2004/03C01P2004/10C01P2006/80
Inventor 王玮梁凯旋陈克正
Owner QINGDAO UNIV OF SCI & TECH
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