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Method for purifying gastrodigenin

A gastrodin aglycon and purification method technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of poor application effect and high process cost, etc., and achieve content reduction, complete extraction, and high extraction efficiency Effect

Inactive Publication Date: 2013-05-01
DAXINGANLING LINGOBERRY BOREAL BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The extraction process of gastrodin aglycone in the above patent documents is mainly refined through pretreatment, enzymatic hydrolysis, supercritical extraction, methanol recrystallization and other steps. Although the final gastrodin aglycone has a high purity, the process itself is expensive and practical The application effect is far inferior to the purification and separation effect of macroporous adsorption resin coupled with silica gel column chromatography

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Weigh 500kg Gastrodia elata, crush it into coarse powder and pass through a 40-mesh sieve, add it at a constant speed of 50kg / h from the feeding port of the elevator, and add 75% acetone aqueous solution through the liquid inlet pipe at a flow rate of 200kg / h with a pipeline pump, The frequency is set to 20Hz, the frequency of host 1 is set to 16Hz, the frequency of juicer 1 is set to 50Hz, the frequency of host 2 is set to 22Hz, the frequency of juicer 2 is set to 45Hz, and 2T of gastrodin crude extract is obtained ; The gastrodin crude extract flows automatically to the temporary storage tank and is continuously pumped to the concentration tank by the outlet pump to concentrate to obtain 200L of gastrodin crude concentrate; adjust the material pump valve so that the gastrogenin crude concentrate enters at 1L / min In the extraction tower, adjust the solvent pump valve so that ethyl acetate enters the extraction tower at 3L / min to obtain 600L of gastrodin ethyl acetate ex...

Embodiment 2

[0027] Weigh Gastrodia elata 1.4T, crush it into a coarse powder and pass through an 80-mesh sieve, add it at a constant speed of 200kg / h from the feed port of the elevator, and add 75% acetone aqueous solution through the liquid inlet pipe at a flow rate of 600kg / h with a pipeline pump, and lift The machine frequency is set to 25Hz, the host 1 frequency is set to 18Hz, the juicer 1 frequency is set to 45Hz, the host 2 frequency is set to 20Hz, the juicer 2 frequency is set to 40Hz, and the gastrodin crude extract is obtained 4.2T; the gastrodin crude extract flows to the temporary storage tank by itself and is continuously pumped to the concentration tank by the outlet pump to concentrate to obtain 400L gastrodin crude concentrate; adjust the valve of the material pump to make the gastrodin crude concentrate 0.5L / min into the extraction tower, adjust the solvent pump valve, so that ethyl acetate enters the extraction tower at 2L / min, to obtain 1.2T of gastrodin ethyl acetate ...

Embodiment 3

[0029] Weigh 800kg Gastrodia elata, crush it into a coarse powder and pass through a 60-mesh sieve, add it at a constant speed of 80kg / h from the feeding port of the elevator, and add 80% acetone aqueous solution through the liquid inlet pipe at a flow rate of 250kg / h with a pipeline pump, The frequency is set to 22Hz, the frequency of host 1 is set to 18Hz, the frequency of juicer 1 is set to 50Hz, the frequency of host 2 is set to 22Hz, the frequency of juicer 2 is set to 45Hz, and 2.5 T; the gastrogenin crude extract flows automatically to the temporary storage tank and is continuously pumped to the concentration tank by the outlet pump to concentrate to obtain 250L of the gastrodin crude concentrate; adjust the valve of the material pump to make the gastrogenin crude concentrate 0.8L / min into the extraction tower, adjust the solvent pump valve, so that ethyl acetate enters the extraction tower at 2.4L / min to obtain 750L of gastrodin ethyl acetate extract; concentrate to ob...

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PUM

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Abstract

The invention discloses a method for purifying gastrodigenin, which comprises the following steps: a raw material is put into a feed hopper after coarse grinding, a host machine of an extraction tank unit rotates to slowly push forward the material from the front end of the unit to the back end, and meanwhile, an extraction solvent enters into the extraction tank from a liquid inlet tube at the tail end of the unit, passes through the moving material from the rear-end of the tank and flows to the front end thereof. In this way, the solid material and the liquid material are contacted fully in the inverse motion, and the effective constituent in the medicinal material is extracted. The herb residue is forcibly pushed forward by a discharging conveyer to a taphole and discharged, and a special juicer extrudes the residual soup of the herb residue out of the medicinal material to reduce the content of the residual soup in the herb residue. The extraction efficiency is higher and the extraction is safer. The method disclosed by the invention selects both extraction of a continuous extraction tank unit and purification of column chromatography on silica gel, so the separation effect is better, and the finished gastrodigenin with the highest yield of 0.2% and content of greater than 95% can be obtained.

Description

Technical field: [0001] The invention belongs to the field of natural organic chemistry and relates to a method for purifying gastrodin aglycone, in particular to a method for purifying gastrodin aglycone by using macroporous adsorption resin coupled with silica gel column chromatography. Background technique: [0002] Gastrodia elata is the dry tuber of the orchid plant Gastrodia elata Bl. Also known as Chijian, Limu, Guiduyou, Shencao, Duyaozhi, Chijianzhi, Dingfengcao, Helicao, Duyao, Automatic Grass, and Water Potato. Contains gastrodin, gastrodin, vanillin, protein, amino acid, trace elements. Have anti-epileptic, anti-palpitation, anti-rheumatism; Sedative, antispasmodic, analgesic, invigorating deficiency, calming liver and calming wind. Functions and indications Calming liver, calming wind and relieving spasm. For headache dizziness, limb numbness, epileptic convulsions, tetanus. Dizziness, neurasthenia, anemofrigid-damp arthralgia, convulsions in children and ot...

Claims

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Application Information

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IPC IPC(8): C07C39/11C07C37/72C07C37/82
Inventor 姚德坤姚德利张亚红姚航黄运生吴海龙
Owner DAXINGANLING LINGOBERRY BOREAL BIOTECH CO LTD
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