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Preparation method of monensin crystal or sodium salt thereof

The technology of monensin and crystal is applied in the field of preparation of monensin crystal or its sodium salt, and can solve the problems of unqualified solubility of monensin sodium salt, low crystal purity, low extraction yield and the like, Achieve the effect of enhancing competitiveness, uniform crystal and simple process

Active Publication Date: 2014-07-16
宁夏泰瑞制药股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main problems of monensin crystals are ① the crystals contain some impurities, resulting in low crystal purity; ② the crystal form is incomplete, and less than 30% of the crystals have a particle size of 40um or more; ③ crystal bonding is prone to occur during the crystallization process; ④The solubility of monensin sodium salt is unqualified; ⑤The extraction yield is not high, generally around 80%

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Monensin fermentation broth 10m 3 , The chemical potency is 34627u / ml.

[0026] The temperature of the monensin fermentation broth was raised to 50°C and stirred for 20 minutes. Use 15% sodium hydroxide to adjust the pH to 8.0, and let it stand for 20 minutes; continue to use lye to adjust the pH to 10.0, and let it stand for another 20 minutes.

[0027] After the temperature of the fermentation broth dropped to 20°C, plate and frame filtration was performed to obtain a filtrate of 7.6m 3 , diluted with water to 15.2m 3 . At 40°C, a mixture of activated carbon, diatomaceous earth and potassium chloride was added. Among them, the dosage of activated carbon and diatomite is 15.2kg and potassium chloride 60.8kg respectively. Stir for 10 minutes, let stand for 30 minutes, filter after decolorization, the volume is 15m 3 , the chemical potency is 21815u / ml, and the yield is 94.5%.

[0028] Adjust the pH of the monensin filtrate to 3.0 with 30% hydrochloric acid, and l...

Embodiment 2

[0034] Monensin fermentation broth 10m 3 , The chemical potency is 35931u / ml.

[0035] The temperature of the monensin fermentation broth was raised to 52°C and stirred for 23 minutes. Use 30% ammonia water to adjust the pH to 8.2, and let it stand for 22 minutes; continue to use ammonia water to adjust the pH to 10.3, and let it stand for another 23 minutes.

[0036] After the temperature of the fermentation broth dropped to 22°C, plate and frame filtration was carried out to obtain a filtrate of 7.5m 3 , diluted with water to 16.5m 3 . At 42°C, a mixture of activated carbon, diatomaceous earth and potassium chloride was added. Among them, the dosages of activated carbon and diatomaceous earth are 24.75kg and 74.2kg of sodium chloride respectively. Stir for 11 minutes, let stand for 32 minutes, filter after decolorization, the volume is 16.3m 3 , the chemical potency is 20897u / ml, and the yield is 94.8%.

[0037] Adjust the pH of the monensin filtrate to 3.2 with 32% p...

Embodiment 3

[0043] Monensin fermentation broth 10m 3 , The chemical potency is 35054u / ml.

[0044] The temperature of the monensin fermentation broth was raised to 55°C and stirred for 25 minutes. Use 35% ammonia water to adjust the pH to 8.5, and let it stand for 25 minutes; continue to use ammonia water to adjust the pH to 10.5, and let it stand for another 25 minutes.

[0045] After the temperature of the fermentation broth dropped to 25°C, plate and frame filtration was performed to obtain a filtrate of 7.5m 3 , diluted with water to 18.8m 3. At 45°C, a mixture of activated carbon, diatomaceous earth and potassium chloride was added. Among them, the dosage of activated carbon and diatomaceous earth is 37.6kg and 94kg of sodium chloride respectively. Stir for 13 minutes, let stand for 35 minutes, filter after decolorization, the volume is 18.7m 3 , the chemical potency is 17846u / ml, and the yield is 95.2%.

[0046] Adjust the pH of the monensin filtrate to 3.5 with 35% sulfuric ...

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Abstract

The invention relates to a preparation method of a monensin crystal or sodium salt thereof. The method is characterized by pretreating, decoloring and precipitating monensin fermentation liquor, dissolving the product in an organic solvent, crystallizing and leaching the product and then directly drying the product to obtain the monensin crystal or adding alkali for salinizing the product and spray-drying the product to obtain the monensin sodium salt. The preparation method has the effects of abandoning the conventional crystallization process, achieving increase of the monensin yield and reduction of cost through the extraction, crystallization and synthesis processes and improving the crystal and finished product quality, and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of antibiotic extraction and synthesis, and in particular relates to a preparation method of monensin crystal or its sodium salt. Background technique [0002] Monensin is a broad-spectrum, high-efficiency polyether biological veterinary drug. The product has the characteristics of high efficiency, low toxicity, and is not easy to produce drug resistance. It is mainly used for bacterial infection and as a feed additive in clinical practice. As a feed additive, it can improve feed utilization efficiency, promote animal weight gain, and shorten the feeding cycle. It is a veterinary drug and feed additive approved by the European Union and approved by the United States and Japan. It has broad market prospects in the world. [0003] There are few technical data about the extraction and synthesis of monensin reported in China. The main problems of monensin crystals are ① the crystals contain some impurities, re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D493/10
CPCC07D493/10
Inventor 任勇
Owner 宁夏泰瑞制药股份有限公司
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