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Method for preparing and purifying tiopronin disulphide

A technology of tiopronin disulfide and tiopronin, which is applied in the field of preparation and purification of tiopronin disulfide reference substance, can solve problems such as difficult preparation and purification of tiopronin disulfide, and achieve reduction of organic solvent residues , easy to remove, cost-reducing effect

Inactive Publication Date: 2012-06-13
青岛市药品检验所
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the preparation and purification of tiopronin disulfide has always been a difficult problem

Method used

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  • Method for preparing and purifying tiopronin disulphide
  • Method for preparing and purifying tiopronin disulphide
  • Method for preparing and purifying tiopronin disulphide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] 1) Oxidize Thiopronin to obtain Tiopronin Disulfide:

[0021] Tiopronin 5g is dissolved in 100ml of water, 50ml of aqueous hydrogen peroxide solution with a volume concentration of 10% is added dropwise, and the reaction is continuously stirred for 24 hours. % of tiopronin disulfide.

[0022] 2) Preparative HPLC purification:

[0023] The light yellow viscous solution was dissolved with 50ml of 0.1% formic acid aqueous solution containing acetonitrile volume concentration ratio of 10% to prepare the test solution, and filtered through a 0.45 μm microporous membrane; the packing material brand of the prepared chromatographic column was Chromatorex C18 bonded phase Packing, prepared column length 10cm, diameter 7.5cm; mobile phase with 0.1% formic acid aqueous solution containing 10% acetonitrile volume concentration ratio; injection volume is 10ml, flow rate is controlled at 160ml / min; detection wavelength is 210nm; collection retention time It is the fraction of 13.5-...

Embodiment 2

[0029] 1) Oxidize Thiopronin to obtain Tiopronin Disulfide:

[0030] Tiopronin 10g is dissolved in 100ml of water, 100ml of aqueous hydrogen peroxide solution with a volume concentration of 20% is added dropwise, and the reaction is continuously stirred for 48 hours. % of tiopronin disulfide.

[0031] 2) Preparative HPLC purification:

[0032] Add 100 ml of 0.1% formic acid aqueous solution containing acetonitrile volume concentration ratio of 7% to the light yellow viscous solution to dissolve to prepare the test solution, and filter it through a 0.45 μm microporous membrane; the packing material brand of the prepared chromatographic column is Microsorb C18 bonded phase Packing, preparation column length 15cm, diameter 5cm; With the 0.1% formic acid aqueous solution that contains acetonitrile volume concentration ratio of 7% as mobile phase; Injection volume is 10ml, and flow rate is controlled at 180ml / min; Detection wavelength is 210nm; Collection retention time is 14.5-1...

Embodiment 3

[0036] 1) Oxidize Thiopronin to obtain Tiopronin Disulfide:

[0037] Tiopronin 10g is dissolved in 100ml of water, 100ml of aqueous hydrogen peroxide solution with a volume concentration of 30% is added dropwise, and the reaction is continuously stirred for 72 hours. % crude product of tiopronin disulfide.

[0038] 2) Preparative HPLC purification:

[0039] The light yellow viscous solution was dissolved in 120ml of 0.1% formic acid aqueous solution containing 5% of acetonitrile volume concentration to prepare the test solution, and filtered through a 0.45 μm microporous membrane; the packing material brand of the prepared chromatographic column was Chromatorex C18 bonded phase Packing, preparation column length 20cm, diameter 7.5cm; 0.1% formic acid aqueous solution containing acetonitrile volume concentration ratio of 5% as the eluting system; injection volume is 40ml, flow rate is controlled at 140ml / min; detection wavelength is 210nm; collection and retention Fractions w...

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Abstract

The invention relates to a method for producing and purifying tiopronin disulphide. The method comprises the following steps of: using hydrogen peroxide to oxidize tiopronin to prepare tiopronin disulphide; and using a chromatographic column with C18 as the filling material, and using 0.1% of formic acid aqueous solution which adopts 5-10% of acetonitrile by volume concentration ratio as mobile phase to purify. The tiopronin which is easy to purchase is used as material, and the hydrogen peroxide which is easy to remove is used as the oxidant in the method; the aqueous solution is only adopted in the preparation process, and 0.1% of formic acid aqueous solution which contains only 5-10% of acetonitrile, is primarily adopted in the purification process, so that the dosage of the organic solvent is a little, the environment pollution is reduced and the cost is reduced; simultaneously, residue organic solvent in the tiopronin disulphide reference substance is reduced; moreover, the whole process has simple process steps, is easy to operate with good reproduction quality.

Description

technical field [0001] The invention belongs to the technical field of medicine preparation and purification, and in particular relates to a preparation and purification method of a tiopronin disulfide reference substance, and an application of the compound. Background technique [0002] Tiopronin injection has the function of protecting liver tissue and cells. It is clinically used to improve liver function of various acute and chronic hepatitis, fatty liver, alcoholic liver, drug-induced liver injury and detoxification of heavy metals, and reduce adverse reactions of radiotherapy and chemotherapy. Prevention of peripheral leukopenia caused by radiotherapy and chemotherapy and for senile early cataract and vitreous opacity. According to the research work of our laboratory, it is found that the mercapto group in the tiopronin molecule is easily oxidized into tiopronin disulfide in the air, and the tiopronin disulfide is the main impurity existing in the tiopronin bulk drug a...

Claims

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Application Information

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IPC IPC(8): C07C323/52C07C319/24C07C319/28
Inventor 张燕杨钊李新荣楚敏赵鲁青曹志胜
Owner 青岛市药品检验所
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