A kind of preparation method of tetrodotoxin

A technology of tetrodotoxin and puffer fish, applied in the direction of organic chemistry, can solve the problems of inability to form high water solubility, achieve good water solubility, improve stability, and good stability

Inactive Publication Date: 2011-12-21
SHANGHAI YINIAN BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the absorption rate of nasal mucosa is affected by many factors
And the acid used in the examples of this patent is a buffering agent, and the number of moles of the acid used in the preparation shows that most of the TTX still has not formed a salt, that is, most of the TTX still cannot form a highly water-soluble solution, and cannot fundamentally solve the problem of its water solubility. question

Method used

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  • A kind of preparation method of tetrodotoxin
  • A kind of preparation method of tetrodotoxin
  • A kind of preparation method of tetrodotoxin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] [embodiment 1] preparation of crude drug tetrodotoxin

[0053] Grind 100kg of pufferfish ovaries with a meat grinder, homogenate with a homogenizer, add 100 liters of 60% ethanol containing 3% acetic acid, stir and soak for 3 times, filter and centrifuge, take the filtrate for 4 times, and then filter under reduced pressure , the filtrate was passed through the D152 type weakly acidic cationic resin column, and the column was eluted with deionized water until the eluate was colorless, and then eluted with 10% acetic acid aqueous solution (elution rate 50ml / min). Detected by HPLC, enriched with venom, combined and concentrated under reduced pressure, the concentrated solution passed through a glucose gel LH-20 column, eluted with 50% ethanol solution containing 5% acetic acid, detected by HPLC, enriched with the eluate containing TTX, Combined and concentrated under reduced pressure, the concentrate was adjusted to pH = 8.0 with ammonia water, placed at a low temperature...

Embodiment 2

[0055] [embodiment 2] the preparation of bulk drug tetrodotoxin

[0056] 100kg of puffer fish ovary is minced with a meat grinder, homogenized with a homogenizer, added 120 liters of 50% methanol containing 5% acetic acid, stirred and soaked 6 times, filtered, centrifugally filtered, and the filtrate is taken 4 times, filtered under reduced pressure, The filtrate was passed through a D152 type weakly acidic cationic resin column, and the column was eluted with deionized water until the eluate was colorless, and then eluted with 10% acetic acid solution (elution rate 50ml / min). Detected by HPLC, enriched with venom, combined, concentrated under reduced pressure, the concentrated solution passed through a glucose gel LH-20 column, eluted with 50% ethanol containing 5% acetic acid, detected by HPLC, enriched with eluate containing TTX Combined and concentrated under reduced pressure, the concentrate was adjusted to pH 9.0 with ammonia water, placed at a low temperature of 10°C fo...

Embodiment 3

[0058] [embodiment 3] preparation of crude drug tetrodotoxin

[0059] Take 100 kg of puffer fish liver, mince it with a meat grinder, homogenize it with a homogenizer, add 110 liters of 60% ethanol containing 4% acetic acid, stir and soak for 4 times, filter, centrifugal filter, take the filtrate for 4 times, and then filter under reduced pressure , the filtrate was passed through the D152 type weakly acidic cationic resin column, and the column was eluted with deionized water until the eluate was colorless, and then eluted with 10% acetic acid aqueous solution (elution rate 50ml / min). Detected by HPLC, enriched with venom, combined and concentrated under reduced pressure, the concentrated solution passed through a glucose gel LH-20 column, eluted with 50% ethanol solution containing 5% acetic acid, detected by HPLC, enriched with the eluate containing TTX, Combined and concentrated under reduced pressure, the concentrate was adjusted to pH = 8.5 with ammonia water, placed at ...

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Abstract

The invention relates to a tetrodotoxin preparation for detoxification and analgesia. The preparation includes a small dose of tetrodotoxin as the active ingredient of the medicine and a co-solvent or support agent selected from pharmaceuticals, and the co-solvent is an amino acid. In the present invention, the amino acid is selected as a co-solvent, which can not only play the role of a co-solvent, increase the solubility of tetrodotoxin in water, but also form a highly water-soluble salt solution with tetrodotoxin. The tetrodotoxin used in the present invention is prepared by the specific method of the present invention, and the prepared tetrodotoxin has a purity as high as 98% and a high yield. The tetrodotoxin and amino acid preparation prepared by the method provided by the present invention not only have good water solubility, but also good stability, safety and reliability, and stable quality. They do not need to be stored in a refrigerator at a specific temperature, and the storage period at room temperature can reach For more than 2 years, the cost of storage and transportation is greatly saved, it is convenient for medical use, and the treatment effect is remarkable, especially for physiological detoxification, and the cure rate reaches 100%.

Description

[0001] This application is a divisional application of Chinese patent application 200810127045.X. [0002] Original application date: 2008-6-18 [0003] Original application number: 200810127045.X [0004] Invention name of the original application: a tetrodotoxin preparation for detoxification and analgesia technical field [0005] The invention belongs to the field of pharmaceutical preparations, in particular to a tetrodotoxin preparation for detoxification and analgesia. Background technique [0006] Tetrodotoxin (TTX) is a low molecular weight alkaloid extracted from the viscera of puffer fish. Due to its unique chemical structure, it is a specific blocker of sodium ion channels in cells. Therefore, it has an irreplaceable position as a biological reagent in the field of biological research. The pharmacological effects of tetrodotoxin in clinical medicine have been reported as early as the 1930s for the clinical intervention of alkaloid addiction. There are also co...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D491/22
Inventor 王开业
Owner SHANGHAI YINIAN BIOTECH
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