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Extraction method of echinocandin b mother nucleus

An extraction method and technology of echinocandin, which is applied in the field of extraction of echinocandin B nucleus, can solve the problems of low purity and yield, many residual pigments in the final product, and large amount of solvent

Active Publication Date: 2018-05-15
ZHEJIANG ZHENYUAN PHARMA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is to overcome the disadvantages of large amount of solvent used in the extraction of echinocandin B mother nuclei in the prior art, many pigment residues in the final product, low purity and yield, etc., and provide a kind of echinocandin B mother nucleus extraction method

Method used

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  • Extraction method of echinocandin b mother nucleus

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] (1) The preparation method of the conversion solution of echinocandin B mother nucleus is as above;

[0064] The conversion solution of the obtained echinocandin B mother nucleus was suction-filtered to obtain 2L of filtrate, and the pH of the filtrate was adjusted to be pH4, a macroporous adsorption resin column (Shanghai Huazhen Resin Co., Ltd. The company’s HZ-806), the flow rate of the upper column is 0.5%CV / min, after the upper column is adsorbed, it is eluted with 2CV of pH4 aqueous hydrochloric acid solution, and then the echinocandin B mother nucleus is concentrated with 1CV of pH4 aqueous hydrochloric acid solution containing 10% ethanol After washing down, the flow rate of elution is 1% CV / min, and the eluate is collected to obtain eluate A (i.e. the primary product of echinocandin B mother nucleus), with a yield of 90% and a purity of 88%;

[0065] (2) The eluent A obtained in step (1) (i.e. the primary product of echinocandin B mother nucleus) was concentrat...

Embodiment 2

[0077] (1) The preparation method of the conversion solution of echinocandin B mother nucleus is as above;

[0078] The conversion liquid of the echinocandin B mother nucleus that makes is suction-filtered, obtains 2.4L filtrate, adjusts filtrate pH to be pH3, upper aspect ratio 4:1, column volume 1.5L macroporous adsorption resin column (Rohm and Haas Company’s XAD-4), the upper column flow rate is 2%CV / min, and after the upper column is adsorbed, it is eluted with 2CV of sulfuric acid aqueous solution with pH 4.5, and then 1.5CV of sulfuric acid aqueous solution containing 12% ethanol is used to echinocandin B parent The nuclei are concentrated and washed down, and the flow rate of the elution is 4% CV / min, and the eluate is collected to obtain the eluate A (i.e. the primary product of the echinocandin B mother nucleus), with a yield of 85% and a purity of 87%. ;

[0079] (2) Concentrate the eluate A obtained in step (1) (i.e. the primary product of echinocandin B nucleus) ...

Embodiment 3

[0084] (1) The preparation method of the conversion solution of echinocandin B mother nucleus is as above;

[0085] The conversion liquid of the echinocandin B mother nucleus that makes is suction-filtered, obtains 2.7L filtrate, regulates filtrate pH to be pH5, upper aspect ratio 4:1, column volume 1.5L macroporous adsorption resin column (Rohm and Haas The company's XAD-18), the upper column flow rate is 1.25%CV / min, after the upper column adsorption, it is 5 sulfuric acid aqueous solution 3CV elution with pH 5, and then the echinocandin B is mixed with the sulfuric acid aqueous solution 2CV containing 14% ethanol The mother nucleus is concentrated and washed down, and the flow rate of the elution is 2.5% CV / min, and the eluate is collected to obtain the eluate A (i.e. the primary product of the echinocandin B mother nucleus), with a yield of 85% and a purity of 85%. %;

[0086] (2) Concentrate the eluent A obtained in step (1) (i.e. the primary product of echinocandin B nu...

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Abstract

The invention discloses a method for extracting echinocandin B parent nucleus, comprising the following steps: (1) removing solid matter in the transformation solution of echinocandin B parent nucleus, obtaining filtrate, and adjusting the pH of the filtrate to 3-5 , on the macroporous adsorption resin, eluted with an inorganic acid aqueous solution with pH 3-5, and then eluted with an inorganic acid aqueous solution containing fatty alcohol, and collected the eluent A; (2) Concentrate the eluent A and adjust the pH to 3 ‑5, a concentrated solution is obtained; (3) the concentrated solution is placed on an octadecyl-bonded silica gel chromatography column, an octaalkyl-bonded silica gel chromatographic column or a circular microsphere resin chromatographic column, using inorganic pH 3‑5 Elution with aqueous acid solution and then with aqueous solution of inorganic acid containing fatty alcohol to obtain eluent B; (4) Concentrate eluent B. The extraction method of the echinocandin B parent nucleus of the present invention has a pigment removal rate of more than 95%, the yield of the product is 70%, and the purity of the echinocandin B parent nucleus is more than 97%.

Description

technical field [0001] The invention relates to a method for extracting echinocandin B nucleus. Background technique [0002] Echinocandins are a new type of antifungal antibiotics listed in the 21st century. Its target is β-1,3-glucan synthase, which exists specifically in fungi, so it can inhibit fungal cell walls The synthesis of leads to lytic death of fungal cells. Anidungin, which is currently on the market, is obtained from Echinocandin B (ECB for short) through microbial transformation to obtain Echinocandin B Nucleus (ECBN for short), and then adds specific side chain groups through chemical synthesis. Group prepared. [0003] The echinocandin B core is an intermediate in the production of anidungin, and its isolation methods are rarely reported in the literature. Chinese patent CN102336817A discloses a separation method of echinocandin B mother nucleus. This separation method is also a method of using resin adsorption and then elution, but this method uses a rel...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07K7/56C07K1/22
Inventor 李继安陈舟舟史洲洋沈剑锋姚黎栋石飞燕林惠敏陈代杰周炜祥韩建栋
Owner ZHEJIANG ZHENYUAN PHARMA CO LTD
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