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A kind of preparation method of high-purity cyclohexyl peptide compound

A cyclohexyl peptide and compound technology, which is applied in the field of preparation of cyclohexyl peptide compound FR179642, can solve the problems of unsuitability for large-scale industrial production, increase of operation steps and production costs, threats to the health of operators, etc., and achieve favorable quality Control, reduce process operation and equipment requirements, improve the effect of product color and purity

Active Publication Date: 2019-04-09
CHONGQING QIANTAI BIOLOGICAL MEDICINE +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese patent CN102443050A discloses that a cyclolipopeptide compound is used as a precursor to obtain FR179642 through enzymatic hydrolysis of the side chain, and reports the separation and purification method of the precursor cyclolipopeptide compound, but does not involve the purification method of FR179642
Compared with the technical solution of the present invention, the prior art has the following disadvantages: 1) Reverse packing chromatography separation is performed after resin adsorption, which increases operation steps and production costs; 2) Reverse packing C18 is more expensive; 3) Methanol, a toxic solvent, is used in desorption, crystallization, and chromatographic separation processes, which poses a threat to the health of operators and pollutes the environment. It is not suitable for large-scale industrial production

Method used

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  • A kind of preparation method of high-purity cyclohexyl peptide compound
  • A kind of preparation method of high-purity cyclohexyl peptide compound
  • A kind of preparation method of high-purity cyclohexyl peptide compound

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Experimental program
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Effect test

Embodiment 1

[0044] Contains 22.7L of FR179642 fermentation broth, and the fermentation unit is 700μg / ml. Add 1kg diatomaceous earth to it, stir

[0045] Centrifugal separation after half an hour, obtain 18.9L filtrate (the collection of illustrative plates of HPLC sees figure 1 and Table 1). The filtrate was concentrated by flash evaporation to obtain 3.8 L of concentrated solution, the unit of which was 3642 μg / ml. The concentrated solution is introduced into XAD1600 adsorption resin (φ8*80cm), the loading volume is 1500ml, and the sample loading flow rate is 2700ml / h. The resin was washed with 12L of purified water at a flow rate of 1800ml / h, and then desorbed with 12L of 5% aqueous ethanol at a flow rate of 2700ml / h. A desorption fraction was collected every 300 ml, and the fractions with a purity above 90% were mixed to obtain 7.2 L of desorption mixture. Add 7.2 g of activated carbon for 767 needles to the desorption mixture, stir for 30 minutes and then filter to obtain a decolo...

Embodiment 2

[0050] The fermentation broth FR179642 was put into a tank of 73.6L, and the fermentation unit was 628μg / ml. Add 1.5kg diatomaceous earth therein, after stirring for half an hour, plate and frame pressure filtration obtains 62.1L filtrate (HPLC peak type and figure 1 resemblance). The filtrate was concentrated by rotary evaporation to obtain a concentrated solution of 13.3 L with a fermentation unit of 3642 μg / ml. The concentrated solution was introduced into XAD1600 adsorption resin (φ 15*100cm), the filling capacity was 3.4L, and the sample loading flow rate was 10.8L / h. The resin was washed with 80 L of purified water at a flow rate of 13.2 L / h, and then desorbed with 26 L of 5% acetone aqueous solution at a flow rate of 13.2 ml / h. A desorption component was collected every 600ml, and the components with a purity of more than 90% were mixed to obtain 22.4L of desorption mixture. Add 20 g of activated carbon for 767 needles in the desorption mixed solution, stir and decol...

Embodiment 3

[0052] The fermentation broth FR179642 was put into a tank of 4.9L, and the fermentation unit was 1350μg / ml. Add 0.2kg perlite wherein, after stirring for half an hour, suction filtration separates, obtains 4.7L filtrate (HPLC peak type and figure 1 resemblance). The filtrate was concentrated by flash evaporation to obtain 1.5 L of concentrated liquid, and the fermentation unit was 4410 μg / ml. The concentrated solution was introduced into XAD1180 adsorption resin (φ4*50cm), the filling volume was 790ml, and the sample loading flow rate was 1000ml / h. The resin was washed with 4L of purified water at a flow rate of 1000ml / h, and then desorbed with 15L of 15% aqueous ethanol at a flow rate of 800ml / h. A desorption fraction was collected every 200 ml, and the fractions with a purity above 90% were mixed to obtain 1.4 L of desorption mixture. Add 1.5 g of activated carbon for 767 needles to the desorption mixture, stir and decolorize for 25 minutes, and then filter to obtain a d...

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Abstract

The invention discloses a preparation method for preparing a cyclohexyl peptide type compound FR179642 by utilizing fermentation metabolites of coleophoma empetri. The method comprises the following steps: filtering an FR179642 fermentation solution, concentrating filtrate, adsorbing by using macro-porous adsorbent resin, desorbing, decolorizing a desorbed solution, crystalizing at a low temperature and the like to obtain a high-purity cyclohexyl peptide type compound FR179642 product. By adopting the macro-porous adsorbent resin in combination with a method of utilizing a decolorizing agent and crystallization, the preparation method disclosed by the invention has the advantages of being simple and practicable in process and suitable for industrial production.

Description

[0001] The present invention is a divisional application of a patent with the application number 201310380275.8, the application date is August 28, 2013, and the invention name is "a method for preparing high-purity cyclohexyl peptide compounds". technical field [0002] The invention belongs to the technical field of industrial microorganisms, and in particular relates to a preparation method of high-purity cyclohexyl peptide compound FR179642. Background technique [0003] Fungi are usually conditional pathogens for healthy humans. When the body's immunity is weakened and external factors are bad, it may cause local or systemic fungal infections. In recent years, with the inappropriate application of broad-spectrum antibiotics, immunosuppressants and glucocorticoids, as well as the widespread application of organ transplantation, radiotherapy and chemotherapy, and surgical intervention, the incidence of deep fungal infections has increased day by day. Fungal infection can ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07K7/56C07K1/36C07K1/34C07K1/30C07K1/16
CPCC07K7/56
Inventor 袁建栋唐恒杨久林郭明刘省伟
Owner CHONGQING QIANTAI BIOLOGICAL MEDICINE
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