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Separation and purification method of high-purity iodine contrast agent monomer

A technology of separation and purification, contrast agent, applied in the separation/purification of carboxylic acid amide, organic chemistry, etc., can solve the problem of low overall yield, and achieve the effect of good process stability, fast elution speed and good repeatability

Pending Publication Date: 2021-07-02
ZHEJIANG STARRY PHARMA +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method requires two recrystallizations, and the overall yield is not high

Method used

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  • Separation and purification method of high-purity iodine contrast agent monomer
  • Separation and purification method of high-purity iodine contrast agent monomer
  • Separation and purification method of high-purity iodine contrast agent monomer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Loading solution: 37.5 ml of synthetic feed solution, the content of ioversol is 40%, and the solution is filtered with a 0.22 μm microporous membrane.

[0030] Separation and purification: The sample solution is separated and purified by a column system, and all the sample solution is injected. The column system uses octadecyl bonded silica gel filler, the column size is Φ50×650mm, the particle size is 10μm, the pore size is 10nm, the filler The mass is 300g, the solvent is water / methanol, the flow rate is 0.1bv / min; 90:10, the detection wavelength is 254nm, and the fraction is taken from the target peak to the peak and the baseline is dropped, and the collection is stopped every 3 minutes during the fraction collection process. , through the liquid phase fraction analysis, and the fractions are combined, the combined fractions are concentrated and dried to obtain the ioversol product with a purity greater than 99%.

[0031] Wherein, the synthetic feed liquid refers to...

Embodiment 2

[0033] Loading solution: 375 ml of synthetic feed solution, the content of ioversol is 40%, and the solution is filtered with a 0.22 μm microporous membrane.

[0034] Separation and purification: Separation and purification of the sample solution using a column system, all of the sample solution is injected, and the column chromatography uses an octyl silica gel column with a column size of Φ80×650mm, a particle size of 30μm, and a pore size of 12nm. The mass is 1500g, the solvent is water / ethanol (95:5), the flow rate is 0.05bv / min; the detection wavelength is 254nm, and the fraction is collected from the peak of the target peak until the peak begins to fall, and the collection is stopped every 4 minutes during the fraction collection process. According to the analysis results of the liquid phase fractions, the fractions are combined, and the combined fractions are concentrated and dried to obtain the ioversol product with a purity greater than 99%.

Embodiment 3

[0036] Loading solution: 400 ml of synthetic feed solution, the content of ioversol is 60%, and the solution is filtered with a 0.22 μm microporous membrane.

[0037] Separation and purification: Separation and purification of the sample solution using a column system, all the sample solution is injected, and the column chromatography uses a methoxysilane silica gel column with a column size of Φ80×650mm, a particle size of 40μm, and a pore size of 12nm. The mass of filler is 1500g, the solvent is 100% water, the flow rate is 0.05bv / min; the detection wavelength is 254nm, the fraction is collected from the peak of the target peak to the peak and the collection is stopped. Fraction analysis results combine the fractions, concentrate and dry the combined fractions to obtain the ioversol product with a purity greater than 99%.

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Abstract

The invention discloses a separation and purification method of a high-purity iodine contrast agent monomer, which is used for separating and purifying a raw material containing an iodine contrast agent monomer by adopting a chromatographic separation method. Wherein the chromatographic separation adopts a dynamic axial pressurization chromatographic column, a bonding material modified by non-polar and low-polar silica gel surfaces is used as a stationary phase, a polar solvent or a medium-polar solvent is used as an eluent, and the purity of the iodine contrast agent monomer obtained after separation and purification is 99% or above. The method effectively solves the problem that a traditional purification method is insufficient in selectivity, and meanwhile, the method is large in sample loading amount, high in elution speed, easy to realize industrial production, good in repeatability, simple and controllable to operate, easy to realize automation and stable in process.

Description

technical field [0001] The invention relates to a method for separating and purifying iodine contrast agent monomers, in particular to a method for separating and purifying high-purity iodine contrast agent monomer raw materials containing iodine contrast agent monomers. Background technique [0002] As a typical non-ionic X-ray contrast agent, iodine contrast agent monomer has good water solubility, low osmotic pressure, relatively stable chemical properties, and can withstand high temperature sterilization. It can be widely used in blood vessels, Arachnoid, body cavity and gastrointestinal examination, etc. The invention has the advantages of small side effects, large dose of administration, good imaging effect and the like. [0003] Commonly used monomers of iodine contrast agents on the market include iohexol, ioversol, iopamidol, iopromide, and iomeprol. Their chemical structures are relatively similar, and the specific structures are as follows: [0004] [0005]...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C235/16C07C231/24
CPCC07C231/24
Inventor 沈伟艺李森钧李华军李奎永何小兵陈仕洪
Owner ZHEJIANG STARRY PHARMA
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