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Separation and purification method of cyclosporin H

A technology for the separation and purification of cyclosporine, which is applied in the field of biochemistry, can solve the problems of cumbersome purification and low yield, and achieve the effects of strong applicability, avoiding waste, and saving production costs

Active Publication Date: 2018-06-12
陈秀明
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It is still difficult to obtain large-scale production of cyclosporin H, the impurity group contained in the fermented crude product itself. Generally, the leftovers produced by cyclosporin A are enriched and purified many times, and then the content is increased. Obtained by purification, the crude product obtained by patent pat20120253007 and the synthetic conversion method reported in its references is an effective and controllable source of cyclosporin H, but the purification is too cumbersome and the yield is low

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  • Separation and purification method of cyclosporin H
  • Separation and purification method of cyclosporin H
  • Separation and purification method of cyclosporin H

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] The crude cyclosporin H in Example 1 comes from the cross-over by-product of cyclosporin A purified by silica gel column chromatography, and the content of cyclosporin H was detected to be 10%.

[0035] The separation and purification method of the present embodiment comprises the following steps:

[0036] Preparation of liquid to be separated: Dissolve cyclosporine H crude product with 10% cyclosporin H content in 10 times the weight of methanol, filter to remove solid insoluble impurities to obtain a solution containing cyclosporine H, and press the solution volume Add water to 20% for stirring and diluting to make the liquid to be separated; stir and add 20% water to make the sample liquid contain water and the sample will not precipitate.

[0037] Chromatographic column preparation: Soak phenylcarbamate β-cyclodextrin silica gel in methanol and then install the column, then equilibrate the column with methanol with a volume percentage concentration of 40%; the diame...

Embodiment 2

[0043] The crude cyclosporin H in Example 2 was obtained from the fermentation broth of Trichoderma polyporus, and the cyclosporin A obtained by purifying cyclosporin A by multiple chromatography contained cross-linked impurities of cyclosporine, wherein the content of cyclosporin H was 30%.

[0044] The separation and purification method of the present embodiment comprises the following steps:

[0045] Preparation of liquid to be separated: Dissolve cyclosporine H crude product with 30% cyclosporine H content in acetonitrile of 10 times the weight, filter to remove solid insoluble impurities to obtain a solution containing cyclosporin H, and press the solution volume Add water to 15% and stir and dilute to make the liquid to be separated; stir and add a small amount of water to make the sample liquid contain water and the sample will not precipitate.

[0046] Chromatographic column preparation: Soak phenylcarbamate β-cyclodextrin silica gel in methanol and load the column, an...

Embodiment 3

[0052] The crude cyclosporin H in Example 3 comes from cyclosporin H prepared by reacting cyclosporine A, and the content of cyclosporin H after pretreatment is 21.4%, and its HPLC figure is shown in Figure 5 , Background of the Invention The HPLC chart of the crude product containing cyclosporine H synthesized from cyclosporin A.

[0053] The separation and purification method of the present embodiment comprises the following steps:

[0054] Preparation of liquid to be separated: Dissolve cyclosporine H crude product with 50% cyclosporin H content in 8 times the weight of ethanol, filter to remove solid insoluble impurities to obtain a solution containing cyclosporine H, and press the solution volume Add water to 25% to stir and dilute to make the liquid to be separated; stir and add a small amount of water to make the sample liquid contain water and the sample will not precipitate.

[0055] Chromatographic column preparation: Soak phenylcarbamate β-cyclodextrin silica gel ...

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Abstract

The invention provides a separation and purification method of cyclosporin H. Phenyl carbamic acid esterified beta-cyclodextrin silica gel is adopted as filler of a chromatographic column to perform separation and purification of cyclosporin H, and cyclosporin A and cyclosporin H in the raw material can be effectively separated. FurthermoreMeanwhile, in separation and purification processes, a single polar solvent can be used, and the solvent can be recycled, thereby savingreducing the production cost; and in an elution process, the crossed part containing cyclosporin H can also be recovered and purified again, thereby avoiding waste. Meanwhile Furthermore, the technical scheme is suitable for various raw materials containing cyclosporin H, has high applicability, can realize mass production and can provide a lot of high-purity cyclosporin H raw materials for the medical industry.

Description

technical field [0001] The invention relates to the field of biochemistry, in particular to a method for separating and purifying cyclosporine H. Background technique [0002] Cyclosporin is a group of cyclic undecapeptide substances produced by Beauveria bassiana (formerly known as Tolypocladium inflatum) discovered in the 1970s. One of the main components, cyclosporin A (Cyclosporin A, CsA), has been widely used in organ transplantation as a highly effective immunosuppressant. The structural diagram and structural formula of cyclosporin A can be seen figure 1 . Its advent has caused a revolution in the field of organ transplantation. In addition to immunosuppressive effects, cyclosporine has a series of other biological activities, such as treating autoimmune diseases such as lupus erythematosus and psoriasis, inhibiting HIV-1 virus, and reversing multidrug resistance of tumors. [0003] Cyclosporin H (CsH) structural diagram and structural formula can be seen figure ...

Claims

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Application Information

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IPC IPC(8): C07K7/64C07K1/36C07K1/34C07K1/16
CPCC07K7/645
Inventor 陈秀明乐占线江莉
Owner 陈秀明
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