Separation and purification method of sugammadex

A technology for separation and purification of sugammadex, applied in the field of separation and purification of sugammadex, can solve the problems of large amount of solvent, cumbersome recrystallization and purification steps, many structural analogs, etc., and achieves good universality and versatility. , Good market application prospects, mild separation conditions

Active Publication Date: 2020-08-18
杭州泽邦科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Up to now, the reports on sugammadex in related periodicals and patent works at home and abroad are mostly in terms of process synthesis and clinical application, but there are few reports on its separation and purification methods, with a total of no more than 20 documents, such as CN1402737 reports a method for purifying sugammadex by dialysis, but the recovery rate of this osmosis method is only 34%, which is not conducive to industrial production
CN107892727A invented the purification of sugammadex sodium by using activated carbon, but this method is not conducive to environmental protection
CN108456264A has reported utilizing silica gel C18 to be that the chromatographic column of filler is purified, and this method column packing is comparatively loaded down with trivial details
[0007] Although a variety of methods for purifying sugammadex have been reported in the above literature, most of them are activated carbon adsorption, recrystallization purification and preparative chromatography purification. Large and the product is usually unstable. Because γ-cyclodextrin is highly polar and has many structural analogues, the structure is relatively complex and contains multiple chiral centers, there is almost no retention during the preparation of chromatography, and secondary purification cannot be achieved after the primary purification. Purification, so the cost of purification is high and the amount of solvent used is large. The above methods have certain disadvantages and limitations

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  • Separation and purification method of sugammadex
  • Separation and purification method of sugammadex
  • Separation and purification method of sugammadex

Examples

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Embodiment 1

[0076] Separation and purification of sugammadex: Take sugammadex and acetonitrile / water (v / v, 1 / 1) to prepare a solution with a concentration of 50g / 100mL. After the solution was clarified, it was filtered through a filter membrane with a pore size of 0.45 μm, and the filtrate was collected for later use. A self-assembled column is used, and the column packing model is SiliaSphere series ODS, with a particle size of 50 μm and a pore size of 0.1% trifluoroacetic acid aqueous solution was used as mobile phase A, acetonitrile was used as mobile phase B, and the flow rate was 80 mL / min. Such as figure 1 As shown, the equilibration time of the first column and the second column is about 15min, and the crude product loading is carried out by the first pump ( figure 1 ), 45min (the detector detects the target peak), sequentially switch valve 1, valve 2, valve 3 and valve 4 into figure 2 Shown (marked by solid line) is double-column internal circulation mode C. At 75min, turn ...

Embodiment 2

[0080] Separation and purification of sugammadex: Take sugammadex and acetonitrile / water (v / v, 1 / 1) to prepare a solution with a concentration of 50g / 100mL. After the solution was clarified, it was filtered through a filter membrane with a pore size of 0.45 μm, and the filtrate was collected for later use. A self-assembled column is used, and the column packing model is SiliaSphere series ODS, with a particle size of 50 μm and a pore size of 0.1% trifluoroacetic acid aqueous solution was used as mobile phase A, acetonitrile was used as mobile phase B, and the flow rate was 80 mL / min. Such as figure 1 As shown, the equilibration time of the first column and the second column is about 15min, and the crude product loading is carried out by the first pump ( figure 1 ), 35min (the detector detects the target peak) when entering into figure 2 Shown (marked by solid line) is double-column internal circulation mode C. At 55min, turn on the second pump to enter image 3 The two...

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Abstract

The invention discloses a separation and purification method of sugammadex. The method comprises the steps: firstly, dissolving a sugammadex sample with a mixed solution, and filtering out insoluble substances; then loading the filtered sample solution to an ODS column; separating by adopting a single-column internal circulation mode or a double-column internal circulation mode; and finally, carrying out gradient elution or isocratic elution on the sample by taking the mixed solvent as a mobile phase, collecting target peaks in sections, and summarizing components of which the target peaks meet the requirements to obtain a purified sample. The method provided by the invention has the advantages of mild separation conditions, high separation efficiency, high separation speed, high universality and the like, can well realize sample separation and purification, can realize enrichment in a short time, can purify and even other types of compounds by changing elution conditions and switchingvalves, and has a good application prospect.

Description

technical field [0001] The invention belongs to the field of separation and purification of medicines, and in particular relates to a method for the separation and purification of sugammadex, which uses assembled single-column or double-column internal circulation to enhance column efficiency mode circulation equipment, and adopts 0.1% trifluoroacetic acid water and methanol Or acetonitrile as the mobile phase, high-purity sugammadex can be obtained. Background technique [0002] Sugammadex is a modified derivative of gamma cyclodextrin. Its molecular structure retains gamma cyclodextrin and consists of a lipophilic core and a hydrophilic outer end to form a cylindrical cavity. The rapid combination of surgical anesthetics rocuronium bromide and vecuronium bromide can quickly reverse the high concentration of muscle relaxants in the blood and anesthetized tissues in a short period of time, and restore the neuromuscular junction to normal. selective muscle relaxant antagonis...

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 潘远江谭艳云林德转王伟黄德权
Owner 杭州泽邦科技有限公司
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