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Preparation method of high-purity cyclohexyl peptide type 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 increasing operation steps and production costs, threats to the health of operators, and being unsuitable for large-scale production, so as to facilitate quality control , improve the color and purity of the product, and facilitate large-scale synthesis

Inactive Publication Date: 2015-03-18
CHONGQING QIANTAI BIOLOGICAL MEDICINE +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese patent CN102443050A discloses a cyclolipopeptide compound as a precursor to obtain FR179642 by enzymatically hydrolyzing 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 chromatographic separation after resin adsorption increases the operation steps and production cost; 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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  • Preparation method of high-purity cyclohexyl peptide type compound
  • Preparation method of high-purity cyclohexyl peptide type compound
  • Preparation method of high-purity cyclohexyl peptide type compound

Examples

Experimental program
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Effect test

Embodiment 1

[0041] Contains 22.7L of FR179642 fermentation broth, and the fermentation unit is 700μg / ml. Add 1kg of diatomaceous earth therein, centrifuge after stirring for 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. Introduce the concentrated solution into XAD1600 adsorption resin (?8*80cm), the filling 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. Collect a desorption fraction every 300ml, and mix the fractions with a purity above 90% to obtain 7.2L 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 decolorizing solution. The decolori...

Embodiment 2

[0049] The fermentation broth FR179642 was put into a tank of 73.6L, and the fermentation unit was 628μg / ml. Add 1.5kg of 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 (?15*100cm), the loading volume was 3.4L, and the sample loading flow rate was 10.8L / h. The resin was washed with 80L of purified water at a flow rate of 13.2L / h, and then desorbed with 26L of 5% acetone aqueous solution at a flow rate of 13.2ml / h. Collect a desorption fraction every 600ml, and mix the fractions with a purity above 90% to obtain 22.4L of desorption mixture. Add 20 g of activated carbon for 767 needles to the desorption mixture, stir and decolorize for 30 minutes, and then f...

Embodiment 3

[0051] The fermentation broth FR179642 was put into a tank of 4.9L, and the fermentation unit was 1350μg / ml. Add 0.2kg perlite therein, stir and separate by suction filtration after half an hour, obtain 4.7L filtrate (HPLC peak shape 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. Introduce the concentrated solution into XAD1180 adsorption resin (?4*50cm), the filling volume is 790ml, and the sample loading flow rate is 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. Collect a desorption fraction every 200ml, and mix the fractions with a purity above 90% to obtain 1.4L 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 decolorized solution. Th...

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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

technical field [0001] 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 [0002] 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 invade internal organs and deep tissues, therefore, effective control of deep mycoses has very important clinical significance. [0003] Echinocandins are new antifungal drugs that have been listed in recent years, which can inhibit the β-1,3-D-glu...

Claims

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Application Information

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IPC IPC(8): C07K7/56C07K1/22
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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