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A kind of preparation method of high-purity echinocandin b mother nucleus

An echinocandin, high-purity technology, applied in the field of preparation of high-purity echinocandin B parent nucleus, can solve the problems of increasing production cost, easily polluting the environment, etc., and achieves improved filtration speed, simple process and product yield high effect

Active Publication Date: 2016-07-06
NCPC NEW DRUG RES & DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method is suitable for large-scale production, a large amount of solvent is used in the extraction process, which not only increases the production cost, but also easily pollutes the environment.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Take 2L of the transformation solution of echinocandin B mother nucleus, the conversion solution unit is 1186μg / mL, adjust the pH value to 4.5 with glacial acetic acid, add 0.1g of polyacrylamide flocculant with molecular weight of 2000KDa to the final concentration of 50ppm, flocculate for 30min, add diatom Soil 100g, stir evenly, filter to obtain the primary filtrate, the primary filtrate uses 1mol / L dipotassium hydrogen phosphate solution to adjust the pH value to 6.5, let stand for 2h, add 100g diatomaceous earth, stir well, filter to obtain the final filtrate 1.83L, put The final filtrate is decolorized through a decolorizing resin column LX-700 with a diameter-to-height ratio of 1:6. The resin loading capacity is 100mL, and the flow rate is 200mL / h. The decolorization solution is introduced into an adsorption resin column with a diameter-to-height ratio of 1:6 for adsorption. The flow rate of the upper column is 200mL / h. After the upper column is completed, first w...

Embodiment 2

[0039]Take 2L of transformation solution of echinocandin B mother nucleus, the conversion solution unit is 1244μg / mL, adjust the pH value to 4.0 with oxalic acid, add 0.1g of polyacrylamide flocculant with a molecular weight of 15000KDa to a final concentration of 50ppm, flocculate for 30min, and add 60g of perlite , stir evenly, filter to obtain the primary filtrate, the primary filtrate uses 2mol / L diammonium hydrogen phosphate solution to adjust the pH value to 6.0, let it stand for 2h, add 60g perlite, stir well, filter to obtain the final filtrate 1.90L, the final filtrate Decolorize through the decolorizing resin column D290 with a diameter-to-height ratio of 1:6, the resin load is 150mL, and the flow rate is 300mL / h. The decolorization solution is introduced into the adsorption resin column HZ818 with a diameter-to-height ratio of 1:6 for adsorption. 300mL / h, after loading the column, first wash the impurities on the adsorption resin column with purified water, then anal...

Embodiment 3

[0041] Take 2L of the transformation solution of echinocandin B mother nucleus, the conversion solution unit is 1256μg / mL, adjust the pH value to 4.3 with 1mol / L phosphoric acid, add 0.1g of polyacrylamide flocculant with a molecular weight of 10000KDa to a final concentration of 50ppm, and flocculate for 30min. Add 80g of perlite, stir evenly, and filter to obtain the primary filtrate. The primary filtrate is adjusted to a pH value of 6.3 with 0.1mol / L sodium hydroxide solution, and allowed to stand for 2 hours. Add 80g of perlite, stir well, and filter to obtain 1.85L of the final filtrate. The final filtrate is decolorized through the decolorizing resin column XDA-7 with a diameter-to-height ratio of 1:6. The resin loading capacity is 170mL and the flow rate is 340mL / h. The decolorization solution is introduced into the adsorption resin column HZ816 with a diameter-height ratio of 1:6 for adsorption. , the flow rate of the upper column is 340mL / h, after the upper column is c...

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PUM

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Abstract

The invention discloses a preparation method of a high-purity echinocandin B mother nuclide. The method comprises the following steps: regulating different pH values of an echinocandin B mother nuclide conversion solution, filtering, decolorizing with a decolorizing resin, adsorbing with a macroporous adsorbent resin, desorbing, concentrating, separating the concentrated solution through a polystyrene or divinylbenzene chromatographic resin, and freeze-drying the desorbed solution to obtain the high-purity echinocandin B mother nuclide product, of which the content is greater than 96% and the total yield is greater than 70%. The method is simple and easy to implement and suitable for industrial production, uses fewer organic solvents in the whole preparation process, and thus, is environment-friendly.

Description

technical field [0001] The invention belongs to the technical field of industrial microorganisms, and in particular relates to a preparation method of a high-purity echinocandin B mother nucleus. Background technique [0002] In recent years, due to the extensive use of immunosuppressants due to organ transplantation, the application of chemotherapy and more aggressive medical methods and other reasons, the number of immunocompromised patients has increased, and the incidence of fungal infections has increased significantly, especially deep fungal infections. Morbidity and mortality are increasing year by year, so new antifungal drugs have become a research hotspot. Echinocandins antifungal drugs target the fungal cell wall, non-competitively inhibit the synthesis of β(1,3)-D-glucan on the cell wall, arrest the cell cycle, completely destroy the cell wall, and cause cell lysis die. Mammals have no cell wall and lack this synthetase, so echinocandins have high specificity t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07K7/56C07K1/36C07K1/34C07K1/22C07K1/16
Inventor 张炜孔鹏谢新宇冷凤邓佩佩李梅倪会敏郑学丽王晶珂宋盼李敏祝仕清张雪霞
Owner NCPC NEW DRUG RES & DEV
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