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Method for extracting and purifying pleuromutilin

A technology of pleuromutilin and a purification method, which is applied in the field of pharmaceutical preparation, can solve the problems of low purity, difficult purification, impurities in the product, etc., and achieves the effects of high purification degree and high extraction rate.

Active Publication Date: 2011-05-11
山东胜利生物工程有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In these processes, butyl acetate, methanol, and ethanol are generally used to extract pleuromutilin, and methyl isobutyl ketone is also used as an extraction agent. Although these methods have high extraction rates, the resulting products contain impurities and their purity is not high. , and not easy to purify

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] 1. Extraction of Crude Pleuromutilin

[0035] 1. Add 3 times (g:ml) of methyl isobutyl ketone (MIBK) to the dry mycelia of pleuromutilin, stir and leach for 1 hour, filter after leaching, and the leaching solution is concentrated after fine filtration The mycelium was leached twice with 4 times MIBK, each time for 1 hour, and after the leaching was completed, the filter was pressed, and the obtained leaching liquid was combined into the concentrator. The equipment used for the filter press is a plate and frame filter press.

[0036] 2. The leaching solution is concentrated with a falling film concentrator until it is close to the precipitated crystals (the crystal content is about 15-20wt%), and the concentrated solution is quickly transferred to the crystallization tank. The cooling rate is to drop the temperature slowly until it drops to 0-4°C, keep warm at this temperature, and the crystals will gradually precipitate until the crystallization is complete.

[0037...

Embodiment 2

[0046] Method step is the same as embodiment 1, and difference is:

[0047] one, Pleuromutilin Crude Extraction

[0048] 1. At the beginning, add 5 times of methyl isobutyl ketone (ml) to the dry mycelium of pleuromutilin (g) for leaching, and then leaching the mycelia twice with 2 times of MIBK.

[0049] 2. Purification of crude pleuromutilin

[0050] 1. Dissolve the crude pleuromutilin in 65% by volume methanol aqueous solution, the amount of methanol aqueous solution is 10 times of the crude product (mass:volume).

[0051] 2. The amount of petroleum ether to be extracted for the first time is 50% by volume of the concentrate, and the amount of petroleum ether to be extracted for the second time is 30% by volume of the aqueous phase.

[0052] 3. When extracting with butyl acetate, the volume (ml) of butyl acetate added twice is 8 times the mass (g) of the crude pleuromutilin.

[0053] 4. The amount of diethyl ether (ml) is 8 times that of the concentrated solution (g)...

Embodiment 3

[0056] Method step is the same as embodiment 1, and difference is:

[0057] 1. Extraction of Crude Pleuromutilin

[0058] 1. At the beginning, add 5 times of methyl isobutyl ketone (ml) to the dry mycelium of pleuromutilin (g) for leaching, and then leaching the mycelia twice with 2 times of MIBK.

[0059] 2. Purification of crude pleuromutilin

[0060] 1. Dissolve the crude pleuromutilin with 70% by volume methanol aqueous solution, the amount of methanol aqueous solution is 8 times (mass:volume) of the crude product.

[0061] 2. The amount of petroleum ether to be extracted for the first time is 30% by volume of the concentrated solution, and the amount of petroleum ether to be extracted for the second time is 50% by volume of the aqueous phase.

[0062] 3. During the extraction with butyl acetate, the volume (ml) of butyl acetate added twice is 15 times the mass (g) of the crude pleuromutilin.

[0063] 4. The amount of diethyl ether (ml) is 9 times that of the concen...

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PUM

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Abstract

The invention discloses a method for extracting and purifying pleuromutilin. The method comprises the following steps: leaching pleuromutilin dry hypha with methyl isobutyl ketone to obtain a crude product; and dissolving the crude product with methanol, sequentially extracting with petroleum ether and butyl acetate, concentrating, crystallizing, washing with aether, and decoloring with activatedcarbon to obtain the finished pleuromutilin product. In the process of leaching the crude pleuromutilin product, the methyl isobutyl ketone is used instead of butyl acetate, thereby increasing the extraction yield (higher than 90%); and in the purification process, proper technical steps and extracting and washing agents are selected to remove impurities contained in the pleuromutilin, thus, the degree of purification is high, and the purity of the pleuromutilin is higher than 98%.

Description

technical field [0001] The invention relates to a method for extracting and purifying veterinary medicine, in particular to a method for extracting and purifying pleuromutilin, and belongs to the technical field of medicine preparation. Background technique [0002] Pleuromutilin is a broad-spectrum diterpene antibiotic produced by Pleurotus mutilus. It acts on the 50S subunit of bacterial ribosome to inhibit protein synthesis and lead to bacterial death. Pleuromutilins are a large family of antibiotics with good antibacterial activity. They are mainly used as feed additives for poultry and livestock. Adding such substances to feed can effectively prevent many infectious diseases, such as effectively inhibiting Gram Positive bacteria, especially staphylococcus and streptococcus are the most obvious, and it also has a therapeutic effect on mycoplasma infection. Pleuromutilin is also used as the precursor of semi-synthetic derivatives of pleuromutilin. At present, there are d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/675C07C67/58C07C67/52C07C67/48
Inventor 胡江林王斌王永恒赵硕珍
Owner 山东胜利生物工程有限公司
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