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Refining method of nedaplatin

A refining method, the technology of nedaplatin, applied in the electrolysis process, electrolysis components, electrolysis organic production and other directions, can solve the problem that silver ions cannot be completely removed, which is not conducive to the removal of silver ions, and achieves less associated impurities, stable quality, Good process reproducibility

Inactive Publication Date: 2014-11-05
NANJING TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Insufficient use of potassium iodide will cause silver ions to not be completely removed; excessive use of potassium iodide will introduce new impurities (iodide ions) in the final nedaplatin product; excessive potassium iodide may react with nedaplatin to produce new impurities; Excess potassium iodide will also precipitate with silver iodide to form a stable complex (AgI 2 ) - , to promote the partial dissolution of the silver iodide precipitate, which is not conducive to the removal of silver ions

Method used

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  • Refining method of nedaplatin
  • Refining method of nedaplatin
  • Refining method of nedaplatin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Take 5.0g of neda platinum with a known silver content of 83ppm, dissolve it in 200ml of hot water at 60°C, cool to room temperature, insert the anode (graphite column, Φ0.8×2.0cm) and cathode (stainless steel plate, 3.0×2.0 cm), the pole distance is 1cm, the electrolysis voltage is adjusted to 1.75 volts, the current is 10 mA, and the electrolysis is carried out for 1.5 hours until the black deposits deposited on the stainless steel plate do not increase significantly. Filtrate, concentrate the filtrate under reduced pressure, crystallize, filter, wash the filter cake with a small amount of ice water, and dry to obtain 4.2 g of nedaplatin, with a yield of 84.0%.

[0025] Detected by atomic absorption spectrometry, the content of silver in nedaplatin is 0.58ppm; determined by high performance liquid chromatography, the content of nedaplatin is 99.38%, and the related substances are less than 1.00%.

Embodiment 2

[0027] Take 10.0 g of neda platinum with a known silver content of 200 ppm, dissolve it in 350 ml of hot water at 70 ° C, cool to room temperature, insert the anode (graphite column, Φ0.8 × 4.0 cm) and cathode (stainless steel plate, 3.0 × 4.0 cm), the pole distance is 1cm, the electrolysis voltage is adjusted to 1.75 volts, the current is 20 mA, and the electrolysis is carried out for 2.0 hours until the black deposits deposited on the stainless steel plate do not increase significantly. Filtrate, concentrate the filtrate under reduced pressure, crystallize, filter, wash the filter cake with a small amount of ice water, and dry to obtain 8.7 g of nedaplatin, with a yield of 87.0%.

[0028] Detected by atomic absorption spectrometry, the content of silver in nedaplatin is 0.76ppm; determined by high performance liquid chromatography, the content of nedaplatin is 99.25%, and the related substances are less than 1.00%.

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Abstract

The invention relates to a refining method of nedaplatin. The refining method comprises the following steps of: dissolving nedaplatin in water at 30-90 DEG C, wherein the weight ratio of nedaplatin to water is 1:(10-100); then, putting the nedaplatin in an electrolytic tank composed of an anode (graphite rod) and a cathode (stainless steel); regulating electrolysis voltage and current to enable the residual silver ions in the solution to be reduced and separated out on the cathode; filtering, and concentrating the filtered solution under the reduced pressure; crystallizing; filtering, and washing the filter cake; and drying to obtain the nedaplatin with very low silver content, wherein the electrolysis voltage is 0.6-3.0V, and the current is 5-200mA. The nedaplatin prepared by the method provided by the invention has the characteristics that the silver content is less than 1.00ppm, the nedaplatin content is greater than 99.00%, the content of related substances is less than 1.00%, and the quality is stable.

Description

technical field [0001] The invention relates to a method for refining nedaplatin, which aims at reducing the silver content in nedaplatin. Background technique [0002] Nedaplatin (Nedaplatin) is another platinum-based antineoplastic drug following cisplatin and carboplatin, and its chemical structural formula is: [0003] [0004] Nedaplatin is mainly used in the treatment of head and neck tumors, small cell and non-small cell lung cancer, esophageal cancer, bladder cancer, testicular cancer, ovarian cancer, cervical cancer, etc. Nedaplatin has the characteristics of broad anti-tumor spectrum, wide range of combined chemotherapy, synergistic effect of combined radiotherapy, no cross-resistance with cisplatin, and low adverse reactions, which can provide more clinical treatment options for cancer patients. [0005] The preparation method of nedaplatin mainly contains: [0006] method 1: [0007] [0008] Method 2: [0009] [0010] Method 3: [0011] [0012...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25B3/12C25B3/04C25B3/13C25B3/25
Inventor 王浦海朱磊高鹏陈宁毛柯
Owner NANJING TECH UNIV
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