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Toad skin total alkaloid and its prepn, analysis and prepn process

A technology of toad skin and total alkaloids, applied in the direction of chemical instruments and methods, alkaloids, alkaloids, etc., can solve the problems of high content of impurities, low content of active ingredients, incomplete extraction of active ingredients, etc., and achieve the goal of a practical determination method Effect

Inactive Publication Date: 2007-08-22
周亚球 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

"A preparation method of cinobufacin freeze-dried powder injection" (patent application number 200510115451.0), in which the toad skin extract is still extracted by water and alcohol precipitation method, the extraction of active ingredients is incomplete, the yield of paste is high, and the content of impurities is large. Low in ingredients

Method used

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  • Toad skin total alkaloid and its prepn, analysis and prepn process
  • Toad skin total alkaloid and its prepn, analysis and prepn process
  • Toad skin total alkaloid and its prepn, analysis and prepn process

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preparation example Construction

[0040] For the preparation of total alkaloids of toadskin, the specific operation process is as follows:

[0041] 1. Take dry toad skin, wash it, add 6-7 times the amount of 85% methanol or ethanol or acetone to soak for 2 hours, reflux extraction for 60 minutes, let it cool, filter, add 5-6 times the amount of 85% methanol or ethanol or Extract with acetone under reflux for 50 minutes, let cool, filter, and combine the filtrates.

[0042] 2. The filtrate was concentrated under reduced pressure until there was no solvent smell. Add water equivalent to 1-3 times the amount of medicinal materials to dissolve, let stand for 24 hours, and filter.

[0043] 3. Put the filtrate on a macroporous tree adsorption resin column, first elute with 2 to 4 times the column volume of water, and then use 3 to 5 times the column volume to elute with 50% to 60% ethanol, collect the ethanol eluate and concentrate it to 60% under reduced pressure. An extract with a specific gravity of 1.10 to 1.2...

Embodiment 1

[0046] Take 1 kg of dry toad skin, wash it, add 6 times the amount of 85% ethanol to soak for 2 hours, reflux extraction for 60 minutes, let cool, filter, add 5 times the amount of 85% ethanol to the residue, reflux extraction for 50 minutes, let it cool and filter, and combine the filtrates. Concentrate the filtrate under reduced pressure until there is no alcohol smell, add 2 times the amount of water to dissolve the medicinal material, let it stand for 24 hours, and filter. Add the filtrate to the HPD-400 macroporous adsorption resin column, first elute with 3 times the column volume of water, then 4 times the column volume with 50% ethanol, collect the 50% ethanol eluate, and concentrate under reduced pressure to 60°C An extract with a specific gravity of 1.15. Add 10 times the amount of neutral alumina for chromatography, mix well, dry below 60°C, add to the packed neutral alumina column for chromatography, elute with chloroform-methanol (6:1) to collect 8 column volumes,...

Embodiment 2

[0049] Take 1 kg of dry toad skin, wash it, add 7 times the amount of 85% methanol to soak for 2 hours, reflux extraction for 60 minutes, let cool, filter, add 6 times the amount of 85% methanol to the residue, reflux extract for 50 minutes, let cool, filter, and combine the filtrates . Concentrate the filtrate under reduced pressure until it has no alcohol smell, add 1.5 times the amount of water equivalent to the medicinal materials, dissolve, let stand for 24 hours, and filter. The filtrate was added to HPD-600 macroporous adsorption resin column, first eluted with 2.5 times column volume of water, then 3.5 times column volume of 55% ethanol, collected 55% ethanol eluate, concentrated under reduced pressure to 60 °C Add 15 times the amount of basic alumina for chromatography to the extract with a specific gravity of 1.20, mix well, dry below 60°C, add to the packed basic alumina column for chromatography, and use chloroform-ethyl acetate-methanol (3 : 1: 1) for elution, co...

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Abstract

The present invention provides preparation process of toad skin total alkaloid. The toad skin total alkaloid contains indole total alkaloid 50-95 wt%, cinobufagin and lipo bufogenin 0.02-0.08 wt%, and toad thetine 20-50 wt%. The present invention provides also the method of measuring toad thetine content, and the injection, powder for injection, dripping pill, capsule, oral liquid, etc with the oad skin total alkaloid as effective component and their preparation process.

Description

1. Technical field [0001] The present invention relates to a kind of total alkaloids of toad skin, the preparation method of the extract, various Chinese medicine preparations for treating chronic hepatitis B and anti-tumor prepared by adding the total alkaloids of toad skin to pharmaceutical excipients, and related to total alkaloids of toad skin at the same time. Determination method of bufathinin in alkali and its preparations. 2. Background technology [0002] The toad skin is the dried whole skin of Bufo bufo gargarizans Cantor or Bufomelanostictus Schneider, which are Bufoidae animals. The chemical components of toad skin mainly include cinobufonitoxin, repobufagenin, bufalin, etc., and the esters formed by them with succinic acid, succinic acid, arginine, etc., such as bufafolin-3- Succinyl arginine ester, bufofabin-3-succinyl arginate, cinobufagin-3-succinyl arginine ester, cinobufagenin-3-succinyl arginate Amino acid ester etc. It also contains indole alkaloids, ...

Claims

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Application Information

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IPC IPC(8): A61K35/56A61K9/08A61K9/10A61K9/14A61K9/16A61K9/20A61K9/48A61P35/00A61P31/12A61P31/20A61P17/06A61P17/12A61P1/16C07G5/00A61K35/65
Inventor 周亚球刘金旗
Owner 周亚球
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