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Romidepsin separation and purification method

A technology for separation and purification of romidepsin, applied in peptide preparation methods, chemical instruments and methods, organic chemistry, etc., can solve the problems of complex operation, low yield, and many reagents and instruments, and achieve simple purification process, The effect of high extraction purity and high yield

Inactive Publication Date: 2015-03-25
SHANGHAI INST OF PHARMA IND +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In order to solve the problems of too many separation and purification steps in the separation and purification method of romidepsin in the prior art, complicated operation, too many reagents and instruments used in the purification process, the cost of separation and purification increases, and irreversible adsorption exists in the adsorption process. Yield is lower and can not be applicable to the defect of large-scale industrial production and provides a kind of separation and purification method of romidepsin

Method used

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  • Romidepsin separation and purification method

Examples

Experimental program
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Effect test

Embodiment 1

[0038] a. Add 3 L of Chromobacterium violaceum WB968 fermentation broth containing romidepsin to 150 g of SP825 macroporous adsorption resin, and stir for 20 min until the adsorption is complete as detected by HPLC.

[0039] b. Separate the macroporous resin adsorbed with romidepsin from the fermentation broth, put the SP825 adsorbed with romidepsin on the column, and wash with tap water until clarified. Romidepsin was eluted with 1.5L acetone to obtain eluent 1. The eluate 1 was concentrated under reduced pressure to obtain a brown-black concentrated solution 1 .

[0040] c. Load concentrated solution 1 to SP825 macroporous adsorption resin (the mass volume ratio of SP825 and concentrated solution 1 is 0.07g / mL), and use acetone and water mixed solvent 2 (the volume ratio of acetone and water is 3:7) For washing, the flow rate sv is controlled not to exceed 7, and then the mixed solvent 3 of acetone and water (the volume ratio of acetone to water is 4.5:5.5) is used for elut...

Embodiment 2

[0045] Other conditions remained unchanged relative to Example 1, and the stirring time was changed to 35 minutes. The finally obtained romidepsin was detected by HPLC with a purity of 97% and a yield of 85%.

Embodiment 3

[0047] Other conditions remained unchanged relative to Example 1, and the stirring time was changed to 60 min. The finally obtained romidepsin was detected by HPLC with a purity of 93% and a yield of 80%.

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Abstract

The invention discloses a romidepsin separation and purification method. The method comprises the following steps: 1, mixing a romidepsin-containing Chromobacterium violaceum broth with macroporous adsorption resin, and stirring until complete adsorption; 2, separating out the macroporous adsorption resin adsorbing romidepsin from the broth, adding the macroporous adsorption resin adsorbing romidepsin to a column, cleaning, eluting to obtain an eluate 1, and concentrating to obtain a concentrate 1; 3, adding the concentrate 1 into macroporous adsorption resin, loading to the column, washing, eluting, detecting by using HPLC in the eluting process, collecting a romidepsin-containing elute 2, and concentrating to obtain a concentrate 2; 4, extracting the concentrate 2 to obtain an organic layer, and concentrating to obtain a crude product; and 5, purifying the crude product to obtain romidepsin. The separation and purification method has the advantages of high extraction purity, high yield, simple purification process and low cost.

Description

technical field [0001] The present invention relates to a separation and purification method of romidepsin. Background technique [0002] Romidepsin, the English name is Romidepsin, is a natural polypeptide isolated from the fermentation broth of Chromobacterium violaceum, and its molecular formula is C 24 H 36 N 4 O 6 S 2 , the molecular weight is 540. [0003] Romidepsin is a new type of histone deacetylase (HDAC) inhibitor. HDAC is a type of zinc ion amidase. When catalyzing histone deacetylation, zinc ion chelates with the hydrate of oxygen on the acetyl group. Synthesis forms a transition state, excessive or abnormal regulation of HDAC makes histones over-deacetylated, and chromosome condensation inhibits transcription, causing the corresponding gene expression to decline, leading to the occurrence of tumor diseases. The anti-tumor mechanism of romidepsin is that after romidepsin enters cells, its disulfide bond is reduced to sulfhydryl by reduced glutathione (GSH...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07K5/103C07K1/22
Inventor 胡海峰熊磊
Owner SHANGHAI INST OF PHARMA IND
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