Iopromide decoloring and purifying process

A technology of iopromide and process, applied in the separation/purification of carboxylic acid amide, organic chemistry, etc., can solve the problems of waste water environmental pollution, low yield, complex operation of iopromide decolorization and purification process, etc., and achieve large adsorption capacity , easy industrial production, high efficiency effect

Inactive Publication Date: 2014-09-17
上海华震科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In order to solve technical problems such as complex operation of iopromide decolorization and purification process in the prior art, low yield and environmental pollution of waste water, the purpose of the present invention is to provide a kind of simple process and low cost, and the product is not only high in purity, but also high in yield. A New Process for Decolorization and Purification of Iopromide

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  • Iopromide decoloring and purifying process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Sample preparation: take by weighing 40g iopromide crude product (purity 95%), join in 200ml deionized water, stir to make sample dissolve completely, after using filter paper to filter for subsequent use.

[0024] Iopromide decolorization and purification: use HZ PS 20ss resin as the chromatographic column, equilibrate the chromatographic column with twice the column volume of deionized water at a flow rate of 1 column volume per hour; 2 times the column volume flow rate continuously flows through the column to load the sample. After loading the sample, use deionized water as the mobile phase, elute with 2 times the column volume / hourly flow rate, and after elution of 1 times the column volume, measure the purity with a high-performance liquid chromatograph for every 0.5 times the column volume of elution. The eluent with purity greater than 99% merges to obtain the collected solution; most of the iopromide flows out in the collected solution of 2 times of column volum...

Embodiment 2

[0027] Sample preparation: Weigh 24g of crude iopromide (purity 96.5%), add it to 200ml deionized water, stir to dissolve the sample completely, and then filter it with filter paper for later use.

[0028] Iopromide decolorization and purification: use HZ PS 818 resin as the chromatographic column of the chromatographic filler, equilibrate the chromatographic column with twice the column volume of deionized water at a flow rate of one column volume per hour; The flow rate of 3 times the column volume continuously flows through the chromatographic column to load the sample. After the sample is loaded, use deionized water as the mobile phase and elute at a flow rate of 3 times the column volume / hour. After elution of 1 times the column volume, every elution The column volume is measured once with high-performance liquid chromatography, and the eluent with a purity greater than 99% is combined to obtain a collection solution; in this embodiment, most of the iopromide flows out in ...

Embodiment 3

[0031] Sample preparation: Weigh 64g of crude iopromide (purity 98%), add it to 400ml deionized water, stir to dissolve the sample completely, and then filter it with filter paper for later use.

[0032] Iopromide decolorization and purification: use HZ PS 20ss resin as a chromatographic column, use twice the column volume of deionized water to equilibrate the chromatographic column at a flow rate of one column volume per hour; 4 times the column volume flow rate continuously flows through the chromatographic column to load the sample. After the sample is loaded, use deionized water as the mobile phase and elute at a flow rate of 4 times the column volume / hour. After elution of 1 times the column volume, each elution The column volume measures the purity once with high performance liquid chromatography, and the eluent with a purity greater than 99% is combined to obtain the collected liquid; most of the iopromide flows out in 4 times the column volume eluent (collected liquid) ...

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Abstract

The invention relates to an iopromide decoloring and purifying process, mainly solving the technical problems of low yield, waste water environment pollution and the like and belonging to the technical field of chemical synthesis, separation and purification. The iopromide decoloring and purifying process is characterized by comprising the following steps of: weighing an iopromide crude product with the purity of 95%-98%, stirring to dissolve in deionized water until the concentration is 100-250 mg/ml, and filtering to remove impurities; then continuously flowing through a chromatographic column with macroporous polystyrene-divinylbenzene microsphere resin as a chromatographic packing at the flow velocity of 1-4 times of column volume per hour, wherein the ratio of the volume L of the macroporous polystyrene-divinylbenzene microsphere resin and the weight g of a sample is (1:10)-(1:80); eluting by using the deionized water as a mobile phase, collecting eluent with the purity of more than 99%, concentrating by using a nanofiltration membrane, and carrying out spray drying. According to the iopromide decoloring and purifying process, the chromatographic packing has the advantages of large adsorption quantity, good selectivity and the like; an iopromide product with the purity of 99% and the yield more than 90% can be obtained through one-time operation by eluting through the deionized water. The iopromide decoloring and purifying process disclosed by the invention has the advantages of simple process, high efficiency, easiness for industrialized production, less environmental pollution and the like.

Description

technical field [0001] The invention relates to a decolorization and purification process of iopromide, a medical non-ionic iodine-containing contrast agent, and belongs to the technical field of separation and purification of pharmaceutical synthetic products. Background technique [0002] Iopromide is a non-ionic iodine-containing contrast agent firstly developed by Schering, Germany, chemical name: N, N'-bis(2,3-dihydroxypropyl)-2,4,6-triiodo- 5-[(2-Methoxyacetyl)amino]-N'-methylphenyl-1,3-carboxamide, the structural formula is shown in Formula I. It has been widely used in clinical medicine as X-ray contrast agent. [0003] [0004] Formula I [0005] Iopromide is chemically synthesized. Because the synthesis will produce some impurities and color problems, in order to meet the relevant pharmacopoeia standards, in addition to improving the synthesis process, post-treatment purification is required to obtain a product with high purity and high yield. At present, the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C237/46C07C231/24
Inventor 宁方红厉留柱李大芦刘爽杨超男
Owner 上海华震科技有限公司
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