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Purifying method of sugammadex sodium

A technology of sugammadex sodium and a purification method, applied in the field of high-purity sugammadex sodium, can solve the problems of inability to provide high-purity sugammadex sodium, complex structure of sugammadex sodium and the like

Active Publication Date: 2018-08-28
JIANGSU HENGRUI MEDICINE CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Although a variety of purification ideas have been given in the above-mentioned literature, the structure of sugammadex sodium is complex and contains multiple chiral centers, especially there are many structural analogues of γ-cyclodextrin, and the above-mentioned methods are more or less flawed , cannot provide high-purity sugammadex sodium, and at the same time meet the needs of large-scale industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Example 1: Preparation of crude sugammadex sodium

[0036] 3.50kg of γ-cyclodextrin was placed in a vacuum drying oven I, and the temperature was 95°C with a vacuum degree of ≦-0.08MPa and dried for 10 to 12 hours, and then packed into a double-layer plastic bag for use.

[0037] Add 9.12kg of triphenylphosphorus and 35kg of DMF into a 100L reaction kettle, protect with nitrogen, stir to dissolve, cool down to -15°C, add dropwise the DMF solution of iodine (9.14kg is dissolved in 11kg DMF), and continue to stir for 0.5-1h after dropping , and then add dry 3.00kg γ-cyclodextrin, the process control temperature does not exceed 0 ℃, and the temperature rises and stirs the reaction. The system was cooled, and the methanol solution of sodium methoxide (2.18kg sodium methoxide dissolved in 8kg methanol) was added dropwise, stirring was completed for 0.5 to 1 hour, and the material solution was transferred to a 50L plastic bucket.

[0038] Into the 500L reactor II, pump 300kg...

Embodiment 2

[0041] Packing the preparative column: 1.2kg silica gel C18 packing (20μm particle size, ) After wetting with 2.4L isopropanol, put it into the column tube of the preparation column, adopt dynamic axial compression, make the packing pressure reach 80~100Bar, and use 5~10 times CV (column volume) of ethanol as the mobile phase to flush the preparation column for backup.

[0042] Dissolve 10 g of crude sodium gluconate in 100 ml of purified water in Example 1, filter with a 0.45 μm membrane filter, continue adding water to the system to 500 ml, and adjust the pH to be acidic.

[0043] The solution was loaded onto a preparative column, and 0.15% formic acid aqueous solution and acetonitrile were pumped to the chromatography column by pipelines A and B, respectively, for elution, keeping the acetonitrile content at 21%. The eluted main peak was divided into different fractions, and the qualified fractions were combined and concentrated to obtain 3.7 g of sodium sugammadex, the y...

Embodiment 3

[0045] Pack the preparative column according to Example 2 for use

[0046] Dissolve 10 g of crude sugammadex gluconate (purity 89.28%, impurity E content 0.60%) in 100 ml of purified water, filter with 0.45 μm filter membrane, continue adding water to the system to 500 ml, and adjust the pH to be acidic.

[0047] The solution was loaded onto a preparative column, and 0.15% formic acid aqueous solution and acetonitrile were pumped to the chromatography column by pipelines A and B, respectively, for elution, keeping the acetonitrile content at 21%. The eluted main peak was divided into different fractions, and the qualified fractions were combined and concentrated to obtain 3.6 g of sodium sugammadex, the yield was 40%, the purity was 99.01%, and the impurity E content was 0.05%.

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Abstract

The invention provides a purifying method of sugammadex sodium. The purifying method specially comprises the following steps: putting a sugammadex sodium crude product to a chromatography column usingsilica gel C18 as a filling, and performing purifying, wherein the purity of the obtained sugammadex sodium is greater than 99%. Through adoption of the purifying method disclosed by the invention, the quality of the products can be guaranteed, and the purifying method is suitable for process scaled production.

Description

technical field [0001] The invention relates to a method for purifying sodium sugammadex, in particular, using silica gel C18 as filler to separate and purify the crude product of sodium sugammadex to obtain high-purity sodium sugammadex . Background technique [0002] Sugammadex sodium is a derivative of γ-cyclodextrin, and its molecule consists of a lipophilic core and a hydrophilic outer end. It is a selective muscle relaxant antagonist, chemical name: 6-deoxy -6-All (2-carboxyethyl) thio-γ-cyclodextrin sodium salt (octa sodium salt), the structural formula is as follows: [0003] [0004] Sugammadex sodium is used to reverse the effects of the routinely used neuromuscular blocking drugs rocuronium or vecuronium, which can immediately reverse the effects of rocuronium used in adults, and routinely reverse the effects of rocuronium in children and adolescents (2 to 17 years old). ) used rocuronium bromide. Sugammadex is the first and only selective relaxation binding...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B37/16
CPCC08B37/0003C08B37/0012
Inventor 梅杰姜立志周大勇田伟伟
Owner JIANGSU HENGRUI MEDICINE CO LTD
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