Process for refining Nedaplatin
A technology of nedaplatin and alkyl alcohol, which is applied in the field of refining nedaplatin, and can solve the problems of low purity and low yield in HPLC analysis
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example 1
[0018] Dissolve 10 g of nedaplatin containing 150 ppm of silver in 800 ml of hot water at 60°C, add about 1.5 mg of KI, stir for 10 min, and filter with a 0.22 μm filter membrane. After stirring, add 1200ml of ethanol next time, cool to -18°C and crystallize for 15 hours, filter the precipitated solid, and vacuum dry at 50°C for 6 hours to obtain the refined product of Nida Platinum 8.2, yield: 82%; no flame atomic absorption spectrometry analysis, silver The content is less than 5ppm, and the high performance liquid chromatography analysis shows that the content is up to 99%.
example 2
[0020] Dissolve 10 g of nedaplatin containing 150 ppm of silver in 500 ml of hot water at 70°C, add about 1.5 mg of KI, stir for 10 min, and filter with a 0.22 μm filter membrane. After stirring, add 1000ml of ethanol next time, cool to -18°C to crystallize for 15 hours, filter the precipitated solid, and dry it in vacuum at 50°C for 6 hours to obtain the refined product of Nida Platinum 8.6, yield: 86%; no flame atomic absorption spectrometry analysis, silver The content is less than 5ppm, and the high performance liquid chromatography analysis shows that the content is greater than 99%.
example 3
[0022] Dissolve 10 g of nedaplatin containing 150 ppm of silver in 500 ml of hot water at 45°C, add about 1.5 mg of KI, stir for 10 min, and filter with a 0.22 μm filter membrane. After stirring, add 1000ml of ethanol next time, cool to -18°C for crystallization for 15 hours, filter the precipitated solid, and vacuum dry at 50°C for 6 hours to obtain the refined product of Nida Platinum 8.3, yield: 83%; no flame atomic absorption spectrometry analysis, silver The content is less than 5ppm, and the high performance liquid chromatography analysis shows that the content is greater than 99%.
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