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Extraction method of nosiheptide

An extraction method and technology of nosiheptide, which is applied in the field of preparation of crude nosiheptide, can solve the problems of dichloromethane corrosive equipment, cumbersome extraction process, and large solvent loss, so as to facilitate equipment maintenance and reduce environmental protection treatment Good strength and product quality

Inactive Publication Date: 2016-11-09
NINGXIA TAIYICIN BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this process, the extraction process is cumbersome, dichloromethane is easy to corrode equipment, easy to decompose at high temperature, and the solvent loss is large

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Take 41.4 kg of Nosiheptide mycelium powder (bulk density 0.6t / m 3 , Total 0.12×10 9 u) Extraction with 138L composite solvent (dimethylformamide (V): ethanol (V): water (V)=2.5:4.5:1.5), extraction time 4hr, extraction temperature 25℃, centrifugal separation, 137.6L of extract (titer 865 u / ml, 0.119×10 9 u), the yield is 99.21%.

[0034] The above extraction liquid is fed into the macroporous resin LSA-700 for adsorption and decolorization, the feeding temperature is 20°C, and the feeding speed is 2.0 BV / h until the feeding of the liquid is complete.

[0035] After the feed solution is finished, first wash with 90% (w / w) ethanol until it is colorless, and then wash with 50% (w / w) acetic acid. The elution speed is 1.5BV / h, and the HPLC check After the peak of nosiheptide appears, collect the eluate, and when the concentration of nosiheptide in the liquid phase is less than 30ug / ml, stop the elution to obtain 206L of the eluate (titer 560 u / ml, 0.115×10 9 u), the yield is 96....

Embodiment 2

[0038] Take 41.4 kg of Nosiheptide mycelium powder (bulk density 0.6t / m 3 , Total 0.12×10 9 u) Extraction with 172.5L composite solvent (dimethylformamide (V): ethanol (V): water (V)=3:5:2), extraction time 4.5hr, extraction temperature 30℃, centrifuge After separation, 170.8L of extract (titer 690 u / ml, 0.119×10 9 u), the yield is 98.20%.

[0039] The above leaching liquid is fed into the macroporous resin LSA-700 for adsorption and decolorization, the feeding temperature is 21°C, and the feeding speed is 3.0 BV / h, until the feeding of the liquid is complete.

[0040] After the feed solution is finished, first wash with 92% (w / w) ethanol until it is colorless, and then wash with 52% (w / w) acetic acid. The elution speed is 2.0 BV / h, and the HPLC check After the nosiheptide peak appears, collect the eluate. When the concentration of nosiheptide in the liquid phase is less than 30ug / ml, stop the elution, and obtain 256L of the eluate (titer 450u / ml, 0.115×10 9 u), the yield is 97.75%...

Embodiment 3

[0043] Take 41.4 kg of Nosiheptide mycelium powder (bulk density 0.6t / m 3 , Total 0.12×10 9 u) Extraction with 207L composite solvent (dimethylformamide (V): ethanol (V): water (V)=3.5:5.5:2.5), extraction time 5hr, extraction temperature 35℃, centrifugal separation, Obtained extract 205L (titer 580 u / ml, 0.119×10 9 u), the yield is 99.29%.

[0044] The above leaching liquid is fed into the macroporous resin LSA-700 for adsorption and decolorization, the feeding temperature is 22°C, and the feeding speed is 4.0 BV / h until the feeding of the liquid is complete.

[0045] After the feed liquid is finished, first wash with 93% (w / w) ethanol until it is colorless, and then wash with 53% (w / w) acetic acid. The elution speed is 2.5BV / h, and the HPLC check After the nosiheptide peak appears, collect the eluate, and stop the elution when the concentration of nosiheptide is less than 30ug / ml in the liquid phase, and obtain 307L of eluate (titer 375u / ml, 0.115×10 9 u), the yield is 96.82%.

[...

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PUM

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Abstract

The invention relates to an extraction method of nosiheptide. The extraction method comprises the following process steps: nosiheptide fermentation liquid atomizing and drying, composite solvent extraction and centrifugation, macroporous resin absorption, acid water hydrolysis, brine precipitation, washing, depressurization and drying. The invention provides a process for extracting the nosiheptide by utilizing composite solvent extraction and macroporous resin de-coloration and purification. According to the method provided by the invention, the extraction efficiency can be improved by 6.5 percent or more, the product purity reaches 96 percent or above, and the economic benefits are favorably improved. According to the method provided by the invention, the wastewater discharge amount is reduced, and the environmental protection treatment is facilitated. The extraction method provided by the invention has the benefits that the solvent corrosion is low, the toxicity is low, the equipment maintenance is facilitated, and the occupational health is facilitated.

Description

Technical field [0001] The invention belongs to the technical field of antibiotic extraction, and particularly relates to a method for preparing crude nosiheptide. Background technique [0002] Nosiheptide is a sulfur-containing peptide antibiotic produced by Streptomy-ces actuosus. It is a secondary metabolite and belongs to the Thiostrepton class. Because it can obviously promote the growth of livestock and poultry, improve the utilization rate of feed, at the same time, it has a low dosage, no residue in the body, little impact on the environment, and no cross-resistance, so it is called an environmentally friendly feed additive. [0003] Nosiheptide is an ester-soluble antibiotic, which mainly exists in the cells of the bacteria, and only a small amount is secreted outside the cells. [0004] Nosiheptide is a crystalline powder at room temperature. The color is light yellow to light brown. It is soluble in chloroform, pyridine, dimethylformamide, slightly soluble in methanol, et...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07K5/078C07K1/36C07K1/30C07K1/16
CPCC07K5/06139
Inventor 裴立忠王勇平
Owner NINGXIA TAIYICIN BIOTECH CO LTD
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