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Method for purifying platinum

A purification method, the technology of miplatin, which is applied in the field of purification of the antineoplastic drug miplatin, and can solve problems affecting product quality, etc.

Active Publication Date: 2011-10-26
KUNMING GUIYAN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] Because the second and third methods use the toxic solvent chloroform, which limits the expansion of production scale, the current synthesis of miplatin is mainly improved on the basis of the first method
However, due to the extremely fast substitution speed of this method, it is easy to wrap the reactant in the product, which affects the quality of the product

Method used

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  • Method for purifying platinum

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 10g of Pt=21.78% through high-temperature weight loss detection, HPLC analysis content of 83.2% of the rice platinum crude product is added in the mixed solution of n-butanol 60ml and absolute ethanol 140ml, dissolved in a water bath at 70°C and filtered the insolubles while hot, Add 160ml of deionized water to the filtrate under stirring in an ice-water bath, let stand for 3h after the solution is cooled, filter the precipitate, wash twice with a mixed solution of isopropanol:water (volume ratio)=1:1, no Washed once with water and ethanol, and dried to obtain 6.4g of white solid with a yield of 64%. Pt=24.85% (theoretical value 24.94%) was detected by weight loss at high temperature, and the content of platinum in HPLC analysis was 98.1%.

Embodiment 2

[0025] 10g of Pt=22.13% through high-temperature weight loss detection, HPLC analysis content of 85.5% of rice platinum crude product is added in the mixed solution of n-butanol 40ml and absolute ethanol 160ml, dissolves in a water bath at 75°C and filters the insolubles while hot, Add 170ml of deionized water to the filtrate under stirring in an ice-water bath, let the solution stand for 3h after cooling, filter the precipitate, wash twice with a mixed solution of isopropanol:water (volume ratio)=1:1, no Washed once with water and ethanol, and dried to obtain 6.7g of white solid with a yield of 67%, Pt=24.89% (theoretical value 24.94%) detected by high-temperature weight loss, and the content of platinum in HPLC analysis was 99.0%.

Embodiment 3

[0027] 10g of Pt=23.04% through high-temperature weight loss detection, HPLC analysis content of 89.9% of the rice platinum crude product was added in the mixed solution of n-butanol 45ml and absolute ethanol 155ml, dissolved in a water bath at 75°C and filtered the insolubles while hot, Add 180ml of deionized water to the filtrate under stirring in an ice-water bath, let the solution stand for 3h after cooling, filter the precipitate, wash twice with a mixed solution of isopropanol:water (volume ratio)=1:1, no Washed once with water and ethanol, and dried to obtain 6.9g of white solid with a yield of 69%. The high-temperature weight loss test showed Pt=24.91% (theoretical value 24.94%), and the content of platinum in HPLC analysis was 99.2%.

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Abstract

The invention relates to a method for purifying platinum of an antitumor drug, wherein the process comprises: platinum is dissolved in a mixed solution of n butanol and anhydrous ethyl alcohol, an insoluble substance is filtered, and a proper amount of deionized water is added in the solution for obtaining a platinum elaboration. When the purification method of the present invention is used for purifying platinum crude products with the content of 80 - 95%, the purity of platinum crude products can be raised more than 98%. The purified platinum products can be directly used for the corresponding drugs production.

Description

technical field [0001] The invention relates to a platinum antitumor drug, in particular to a purification method of the antitumor drug miplatin. Background technique [0002] Miriplatin, cis-[ditetradecanoic acid-(1R,2R)-1,2-cyclohexanediamine platinum (II)] and hydrate, English name Miriplatin, CAS 141977-79-9, is A new fat-soluble platinum-based antineoplastic drug developed by Sumitomo Corporation of Japan. This variety was approved for marketing in Japan in 2009 and is mainly used clinically for the treatment of liver cancer. Studies have shown that miplatin can be mixed with peripheral embolic agent Lipiodol to maintain stability. Miplatin / Lipiodol can not only embolize tumor blood supply arteries but also slowly release anticancer drugs, and can selectively stay in liver cancer tissues for a long time, maintaining long-term effective drugs Concentration, embolization and chemotherapy complement each other and promote each other. At the same time, it also effectively...

Claims

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Application Information

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IPC IPC(8): C07F15/00
Inventor 王庆琨普绍平朱泽兵李学杰王蒙温志寿金全黄天俊
Owner KUNMING GUIYAN PHARMA
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