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.
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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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