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Method for purifying cetrorelix

A technology of cetrorelix and purification method, which is applied in the fields of peptide preparation methods, chemical instruments and methods, organic chemistry, etc., can solve the problem that cetrorelix has no obvious separation effect, achieve purification yield and stable, and produce The process is simple, the method is simple and effective

Active Publication Date: 2019-03-15
苏州天马医药集团天吉生物制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Using the above mobile phase [D-Arg 8 ]-cetrorelix and [beta-Ala-D-Cit 6 ]-cetrorelix had no significant separation effect (see figure 1 Medium [D-Arg 8 ]-Cetrorelix as the post-mixture, [β-Ala-D-Cit 6 ]-cetrorelix is ​​the former impurity), and these two impurities are unavoidable in the process, so it is necessary to further optimize the purification of cetrorelix

Method used

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  • Method for purifying cetrorelix
  • Method for purifying cetrorelix
  • Method for purifying cetrorelix

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Take the crude cetrorelix peptide, add 5% acetonitrile solution, dissolve, stir, and sonicate, the content of cetrorelix in the solution is 15 mg / ml. When the solution was clear, it was filtered with a filter membrane with a pore size of 0.45 μm, and the filtrate was collected for later use. A 3.0×250mm C18 / C8 reverse-phase silica gel column was used. The mobile phase A is a mixed aqueous solution of 0.5wt% sodium sulfate and 0.5% v / v trifluoroacetic acid, the mobile phase B is 100% acetonitrile solution, and the solution storing the mobile phase is put into a water bath and heated to 30-50°C. The pretreatment of the chromatographic column is to use a high-concentration organic phase to remove impurities, and then use an organic phase with a concentration lower than 25% to balance. The volume of the crude peptide sample on pump A is 20ml, and then gradient elution is performed with mobile phase A and mobile phase B, and the flow rate is controlled at 20ml / min. The elu...

Embodiment 2

[0031] Take the crude cetrorelix peptide, add 5% acetonitrile solution, dissolve, stir, and sonicate, the content of cetrorelix in the solution is 15 mg / ml. When the solution was clear, it was filtered with a filter membrane with a pore size of 0.45 μm, and the filtrate was collected for later use. A 3.0×250mm C18 silica gel column for reverse phase chromatography was used. The mobile phase A is a mixed aqueous solution of 4wt% sodium sulfate and 2% v / v trifluoroacetic acid, the mobile phase B is a 100% acetonitrile solution, and the solution storing the mobile phase is put into a water bath and heated to 30-50°C. The pretreatment of the chromatographic column is to use a high-concentration organic phase to remove impurities, and then use an organic phase with a concentration lower than 25% to balance. The volume of the crude peptide sample on pump A is 20ml, and then gradient elution is performed with mobile phase A and mobile phase B, and the flow rate is controlled at 20ml...

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Abstract

The invention discloses a method for purifying cetrorelix and belongs to the technical field of separation and purification. The method disclosed by the invention mainly comprises the following steps:dissolving, stirring and filtering crude cetrorelix peptides; loading the filtered solution into a reverse phase silica gel column filled with polyoctadecane for performing chromatography; eluting the target product by taking a mixed solution of sodium sulfate and trifluoroacetic acid as a mobile phase A and taking an organic solvent as a mobile phase B; collecting the elution solution accordingto a target peak order, analyzing and detecting various collected solutions, gathering all the collected solutions meeting requirements, and inspecting. According to the method for efficiently and rapidly separating and purifying cetrorelix disclosed by the invention, [D-Arg8]-cetrorelix and [beta-Ala-D-Cit6]-cetrorelix can be effectively separated, the single purity content can be less than 0.1%by virtue of one-step purification, the total purity is 99.9% or higher, and the purification yield reaches 80%. The production process is simple and can be applied to enlarged and large-scale production, and the production cost of enterprises is reduced.

Description

technical field [0001] The invention relates to a purification method of cetrorelix, which belongs to the technical field of separation and purification. Background technique [0002] Cetrorelix is ​​a luteinizing hormone releasing hormone (LHRH) antagonist. Can bind to membrane receptors of pituitary cells. Cetrorelix competes with endogenous LHRH for binding to these receptors, thereby controlling gonadotropin secretion. Cetrorelix can rely on the secretion of sex hormones through the hypothalamus-pituitary-gonad pathway, so as to achieve the purpose of indirectly inhibiting cancer growth or preventing, alleviating and treating other diseases. It can be used to treat hormone-sensitive prostate cancer and breast cancer and some Benign gynecological diseases. Compared with GNRH agonists, cetrorelix has the advantages of shorter course of treatment, fewer adverse reactions, and can effectively reduce the incidence of OHSS. [0003] Cetrorelix as a decapeptide [0004] Ce...

Claims

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Application Information

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IPC IPC(8): C07K7/23C07K1/20
CPCC07K7/23
Inventor 荆涛黄保胜沈杰孙锋
Owner 苏州天马医药集团天吉生物制药有限公司
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