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Preparation method of high-purity validamycin A

A technology of Jinggangmycin and Jingganghydroxylamine, which is applied in the field of new preparation of high-quality Jinggangmycin A, can solve the problems of affecting export, Jinggangmycin A cannot reach 60%, and avoid inhibition and avoid substrate to enzyme Effects of Inhibition, Yield and Purity Improvement

Inactive Publication Date: 2015-10-28
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] However, with the increase in the number of product exports, foreign users have higher and higher quality requirements for Jinggangmycin A, and are no longer satisfied with the existing Jinggangmycin A content of 600,000. Jinggangmycin A in the product has not yet reached 60%, thus affecting exports

Method used

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  • Preparation method of high-purity validamycin A
  • Preparation method of high-purity validamycin A
  • Preparation method of high-purity validamycin A

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 200 mL of Jinggang Hydroxylamine A solution containing 0.5% g / mL to 100 mL of 001×7 strong acid cation exchange gel resin (Hangzhou Zhengguang Resin Co., Ltd.), stir well to make Jinggang Hydroxylamine A completely adsorbed, filter, and wash with 100 mL of deionized water ,spare. Add the resin that has adsorbed Jinggang Hydroxylamine A to 350mL of water, add 1.5g of cellobiose, 1.8g of Escherichia coli wet cells, control pH = 6.0, react on a shaker at 30°C and 150rpm for 24h, and use gauze Filter the resin, wash the bacteria with deionized water, pack the resin into a column, elute with 0.5mol / L ammonia solution, and collect the Jinggangmycin A component through HPLC tracking detection, at 40°C under the condition of -0.95~-0.98 atmospheric pressure Concentrate under low temperature, freeze-drying obtains product 0.85g, detects through HPLC, (detects with Japan Shimadzu 20A high performance liquid chromatography, detection condition: mobile phase is to contain 2.5% ...

Embodiment 2

[0024] Add 200L solution containing 0.8% Jinggang Hydroxylamine A (W / V) to 100L D001 strongly acidic cation exchange macroporous resin (Hangzhou Zhengguang Resin Co., Ltd.), stir fully to make Jinggang Hydroxylamine A completely adsorbed, filter, and use 100L deionized water Wash and set aside. Add the resin that has adsorbed Jinggang Hydroxylamine A to 400L of water, add 2.0kg of cellobiose, 2.0kg of Escherichia coli wet cells, control pH = 6.0, stir and react at 35°C for 24h, and use gauze on the tripod Centrifuge the resin in a centrifuge, wash the bacteria with 100L deionized water, pack the resin into a column, elute with 0.8mol / L ammonia solution, and collect the Jinggangmycin A component through HPLC tracking detection. Concentrate at -0.98 atmospheric pressure, spray dry (inlet temperature: 180° C., outlet temperature: 70° C.) to obtain 1.8 kg of product, and the purity is 96.3% as detected by HPLC.

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Abstract

The invention discloses a preparation method of high-purity validamycin A. The preparation method comprises the steps that firstly validoxylamine A is adsorbed on cationic resin, colibacteriophage serves as a glycosyl transferase catalyst, cellobiose is added into water to enable the final concentration of the cellobiose to be 0.05-1.5% g / mL, and the reaction is conducted for 12-48 h under the conditions that the reaction temperature is 25-35 DEG C, and the pH is 5.0-7.0; after the reaction is finished, filtering is conducted, a filter cake is taken to be eluted by the use of a 0.2-1.2 mol / L ammonia-water solution, a validamycin A component is traced, detected and collected through HPLC, spray drying or freeze drying is conducted after concentration to prepare and obtain the validamycin A, and the mass ratio of the validoxylamine A to the cellobiose is 1:1.5-2.5. According to the preparation method of the high-purity validamycin A, the cation exchange resin is used for adsorbing the validoxylamine A and the validamycin A, not only can the substrate be avoided inhibiting enzymes, but also the products can be avoided inhibiting the enzymes, and the prepared validamycin A is high in product purity.

Description

(1) Technical field [0001] The invention relates to a new preparation process of high-quality Jinggangmycin A. (2) Background technology [0002] Jinggangmycin is an aminoglycoside agricultural antibiotic independently developed and produced in my country. It is produced by the metabolism of Streptomyces hygroscopicus var. jinggangensis yen. It can effectively inhibit rice sheath blight. One of the antibiotics with the highest unit and one of the most important varieties of biological pesticides. [0003] Jinggangmycin is a multivariate mixture, mainly composed of components such as Jinggangmycin A, B, C, D, E, F, G and H (as shown in Table 1), wherein A component is effective against rice sheath blight The activity is the strongest, the content is the highest, C and D components are almost ineffective, and there are Jinggang hydroxylamine A, B and G, which are bicyclic ring alcohols without glucosyl. [0004] Currently, Jinggangmycin products are available in two dosage fo...

Claims

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Application Information

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IPC IPC(8): C12P19/46C12R1/19
Inventor 陈小龙范永仙陆跃乐沈寅初
Owner ZHEJIANG UNIV OF TECH
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