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Method for extracting galangin from galangal

A technology of galangin and galangal, applied in the direction of organic chemistry, can solve the problems of difficult control and high product cost, and achieve the effects of low cost, easy industrialization and high product purity

Inactive Publication Date: 2010-09-08
NANJING ZELANG AGRI DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] As mentioned above, there are many types of organic reagents used in the extraction process of the existing process, which is difficult to control in large-scale production, and the product cost is relatively high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Take the galanga medicinal material and grind it, take 10kg, put it into a stainless steel extraction tank, add 60L saturated lime water, heat to 60°C, extract dynamically for 1 hour, extract 3 times, combine the extracted hydrochloric acid and adjust to neutral filtration, take 6L HZ816 macroporous resin After the pretreatment is completed, the extract is added to the macroporous resin column. The flow rate of the injection liquid is controlled at 12L / h. After the adsorption is completed, the impurities are eluted with 42Lph8 lime water, and then the galangin is eluted with 48L70% ethanol solution. , the elution flow rate is 6L / h, the eluent is decompressed to recover ethanol, and the concentrated solution is added with 1% hydrochloric acid solution by volume and allowed to settle for more than 10 hours. Centrifuge to obtain 280g of precipitate, wash twice with 780ml 50% ethanol solution, and wash back three times with 780ml70% ethanol solution. The washings were disso...

Embodiment 2

[0028] Take the galangal medicinal material and grind it, take 10kg, put it into a stainless steel extraction tank, add 15L saturated lime water, heat to 50°C, extract dynamically for 3 hours, extract twice, combine the extracted hydrochloric acid and adjust to neutral filtration, take 6L AB-8 large Porous resin column, pretreatment is completed, the extract is added to the macroporous resin column, the flow rate of the injection liquid is controlled at 13L / h, after the adsorption is completed, the impurities are eluted with 30Lph9 lime water, and then Gao Liang is eluted with 30L80% ethanol solution Gingerin, the elution flow rate is 12L / h, and the eluent is decompressed to recover ethanol, and the concentrated solution is added to its volume of 0.5% sulfuric acid solution and left to precipitate for more than 8 hours. Centrifuge to obtain 289g of precipitate, wash 3 times with 600ml 50% ethanol solution, and then reflux wash 2 times with 600ml 70% ethanol solution. The washi...

Embodiment 3

[0030] Take galanga medicinal material and crush it, take 10kg, put it into a stainless steel extraction tank, add 100L saturated lime water, heat to 60°C, extract dynamically for 1 hour, extract 3 times, combine the extracted hydrochloric acid and adjust to neutral filtration, take 6L ADS-11 large Porous resin column, pretreatment is completed, the extract is added to the macroporous resin column, the flow rate of the injection liquid is controlled at 16L / h, after the adsorption is completed, the impurities are eluted with 35Lph8 lime water, and then Gao Liang is eluted with 36L75% ethanol solution. Gingerin, the elution flow rate is 9L / h, and the eluent is decompressed to recover ethanol, and the concentrated solution is added to its volume of 0.5% hydrochloric acid solution and placed for precipitation for more than 10 hours. Centrifuge to obtain 291 g of precipitate, wash 3 times with 800ml 50% ethanol solution, and then reflux wash 3 times with 800ml 70% ethanol solution. ...

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Abstract

The invention relates to a method for extracting galangin from galangal. The method comprises the following steps of: crushing the galangal medicament serving as a raw material; adding saturated limestone solution in an amount which is 6 to 15 times that of the galangal into the galangal; heating the mixture at the temperature of between 40 and 60 DEG C; dynamically extracting the mixture for 1 to 3 hours for 2 to 3 times; adjusting the extract to be neutral; filtering the extract, adding a macroporous resin column into the extract for adsorption; eluting impurities of the extract with lime water of which the flow is 5 to 7 and pH is 8 to 9, and eluting the galangin with 70-80 percent ethanol solution of which the flow is 5 to 8; reclaiming ethanol from the eluent; adding hydrochloric acid or sulphuric acid in an amount which accounts for 0.5 to 1 percent of the volume of the concentrate into the concentrate for precipitating; refluxing and washing the filtered precipitate with 50 percent ethanol solution and 70 percent ethanol solution of which the amount is 2 to 3 times that of the filtered precipitate in sequence for 2 to 3 times; refluxing and dissolving the precipitate in acetone; filtering and reclaiming crystal which is one third to one sixth of the original volume so as to filter crystal; refluxing and dissolving the crystal in 99 percent ethanol for 2 to 3 times; and drying the crystal to obtain the galangin. The method for preparing the galangin has the advantages of low cost, small using amount of toxic reagent and high industrialization degree.

Description

Technical field: [0001] The invention belongs to the technical field of biological separation, in particular to an industrial method for extracting galangin. Background technique: [0002] Galangal is also called small galangal and wind ginger. Nature and flavor are pungent, hot, non-toxic. It has the effects of warming the stomach and dispelling cold, eliminating food and relieving pain. [0003] Galangal rhizome mainly contains volatile oil, diphenylheptane compounds and flavonoids. Flavonoids mainly include: galangin, quercetin, kaempferol, kaempferol, isorhamnetin, quercetin-5-methyl ether, galangin-3-methyl ether, etc. Among them, galangin is a functional ingredient. [0004] Galangin, another name: Galangin. [0005] Molecular formula: C15H10O5. [0006] Molecular weight: 270.23. [0007] Physical properties: light yellow needle crystal (ethanol), melting point 214-215° (219-221°). Still soluble in ethanol and ether. It becomes a yellow solution in aqueous alk...

Claims

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Application Information

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IPC IPC(8): C07D311/40C07D311/30
Inventor 苏刘花
Owner NANJING ZELANG AGRI DEV
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