Purification method of high-load iohexol

A purification method, the technology of iohexol, applied in the separation/purification of carboxylic acid amide, organic chemistry, etc., can solve the problems such as greater influence on the yield and purity of iohexol, small adsorption amount of iohexol, unfavorable industrial scale-up, etc. , to achieve mild operating conditions, reduce production costs, and prolong life

Active Publication Date: 2020-05-05
SUNRESIN NEW MATERIALS CO LTD GAOLING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

"Separation and Purification of Iohexol by Liquid Chromatography" connected XAD1600 and XAD7HP two macroporous resins in series for the purification of iohexol, but the ratio of the two resins has a great influence on the yield and purity of iohexol. Good for industrial scale-up
Patent CN201711169561.4 uses monodisperse microspheres as chromatographic fillers, and only one-step chromatography can obtain raw materials that meet the requirements of the Pharmacopoeia, but the resin has a small amount of iohexol adsorption (the maximum sample loading per milliliter of chromatographic fillers is 0.11 g iohexol crude product), the production efficiency is lower

Method used

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  • Purification method of high-load iohexol
  • Purification method of high-load iohexol
  • Purification method of high-load iohexol

Examples

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Effect test

Embodiment 1

[0043] In a chromatographic column of 16×180 mm, 36 ml of ultra-high cross-linked macroporous styrene / divinylbenzene copolymer microspheres (LX-161 produced by Xi’an Lanxiao Technology New Materials Co., Ltd., with a resin particle size range of 50-150μm, the pore size is The specific surface area is 1000m 2 / g) as a chromatographic filler. Weigh 7g iohexol crude product in a beaker (the liquid chromatogram is as follows figure 1 As shown, 0.192g iohexol crude product was loaded per milliliter of resin), stirred and dissolved with 25ml deionized water, then filtered with a 0.45 μm filter membrane, and the filtrate was collected for use.

[0044] Control the flow rate to 3ml / min (0.83 column volume 10 / min), first equilibrate the chromatography column with deionized water for 6 column volumes. Then the filtered iohexol crude product solution is loaded into the chromatographic column, and 14 column volumes are used to elute with deionized water and the effluent (iohexol main ...

Embodiment 2

[0046] In a chromatographic column of 10 × 600 mm, 47 ml of ultra-high cross-linked macroporous styrene / divinylbenzene copolymer microspheres (LX-361 produced by Xi'an Lanxiao Technology New Materials Co., Ltd., with a resin particle size range of 75-120μm, the pore size is The specific surface area is 1100m 2 / g) as a chromatographic filler. Take by weighing 10g iohexol crude product in beaker (liquid phase chromatogram is as follows figure 1 As shown, 0.212g iohexol crude product was loaded per milliliter of resin), stirred and dissolved with 30ml deionized water, then filtered with a 0.45 μm filter membrane, and the filtrate was collected for use.

[0047] Control the flow rate to 4ml / min (0.85 column volume 10 / min), and first equilibrate the chromatography column with deionized water for 6 column volumes. Then the filtered iohexol crude product solution is loaded into the chromatographic column, and 16 column volumes are eluted with deionized water and the effluent (io...

Embodiment 3

[0049]In a chromatographic column of 35 × 600 mm, 576 ml of ultra-high cross-linked macroporous styrene / divinylbenzene copolymer microspheres (LX-22 produced by Xi'an Lanxiao Technology New Materials Co., Ltd., with a resin particle size range of 50-100μm, the pore size is The specific surface area is 1100m 2 / g) as a chromatographic filler. Take by weighing 150g iohexol crude product in beaker (liquid phase chromatogram is as follows figure 1 As shown, 0.260g iohexol crude product is loaded per milliliter of resin), stirred and dissolved with 500ml pure water, then filtered with a 0.45 μm filter membrane, and the filtrate is collected for use.

[0050] Control the flow rate to 5ml / min (0.87 column volume 10 / min), and first equilibrate the chromatography column with depurified water for 7 column volumes. Then the filtered iohexol crude product solution is loaded into the chromatographic column, and 17 column volumes are eluted with pure water and the effluent (main peak o...

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Abstract

The invention discloses a purification method of high-load iohexol. The purification method comprises the following specific operation steps: dissolving a crude iohexol product with deionized water, and filtering the iohexol solution; loading the iohexol solution into a chromatographic column filled with polymer microspheres for adsorption; performing elution by using deionized water as a mobile phase; collecting effluent in sections, carrying out liquid chromatography detection, and gathering the effluent meeting the requirements to obtain a purified iohexol solution; and after purification is finished, regenerating the chromatographic packing by using a low-toxicity reagent. The method is simple to operate and mild in condition, the resin for purification can be recycled, the iohexol loading capacity is high, the production cost is reduced, and the method is particularly suitable for large-scale production.

Description

technical field [0001] The invention belongs to the field of medicine purification, in particular to a method for purifying iohexol. Background technique [0002] Iohexol (Iohexol), the chemical name is 5-[acetyl(2,3-dihydroxypropyl)amino]-N,N'-bis(2,3-dihydroxypropyl)-2,4, 6-triiodo-1,3-benzenedicarboxamide is a water-soluble, non-ionic X-CT contrast agent. As a second-generation non-ionic monomeric contrast agent, iohexol has the advantages of low osmotic pressure, good tolerance, and clear diagnostic images. It is mainly used clinically for angiography, lumbar, thoracic, and cervical spine angiography, and enhanced CT scanning. Wait. Its structural formula is as follows: [0003] [0004] In addition to the iohexol endo- and exo-isomers with pharmacological effects, the iohexol sample also contains a small amount of ionizable acidic impurities, such as O-alkyl compounds and N-alkyl compounds. The existence of these impurities will cause the occurrence of adverse dr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/24C07C237/46
CPCC07C231/24C07C237/46
Inventor 吴丹王朝阳张赪贾晓妮李佩陶刘琼寇晓康
Owner SUNRESIN NEW MATERIALS CO LTD GAOLING
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