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Hyperin extraction method and preparation and use thereof

A technology of hyperin and extraction method, applied in the field of extracting active ingredients, can solve the problems of complicated process, unachieved, long working hours and the like

Inactive Publication Date: 2009-03-18
周春晓 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is complicated in process, high in cost, and long in working hours, and is not suitable for industrial chemical production.
[0005] Application No. 200610054268.9 discloses "Preparation method of hyperin and hypericin in Hypericum perforatum", using CTAB reverse micellar extractant to extract and separate hyperin, but the content of hyperin separated by this method is 83.6 -87.3%, this content does not meet the standard of a class of raw materials, that is, more than 90%

Method used

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  • Hyperin extraction method and preparation and use thereof
  • Hyperin extraction method and preparation and use thereof
  • Hyperin extraction method and preparation and use thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0017] Take 1 kg of hollyhock flower coarse powder, add 10000 ml of 80% ethanol aqueous solution, heat and reflux for extraction for 1 to 2 hours, extract 2 to 3 times in total, and combine the extract; The weight V / W is 1:1, filter; the filtrate is extracted 8 to 10 times with 1:1 (V / V) water-saturated n-butanol or water-saturated ethyl acetate, and the n-butanol or ethyl acetate extracts are combined , dried with anhydrous sodium sulfate, filtered, concentrated under reduced pressure at less than 80°C, and dried in vacuum to obtain the crude extract of hollyhock flowers; take 100 g of the crude product, first deesterify with 10 times the amount (W / V) of petroleum ether, and filter , after evaporating to dryness, add 1000ml ethyl acetate:ethanol=4:1~8:1 (V / V) reflux extraction 3 times, each time 1~2 hour, reclaim solvent, 80 ℃ of decompression drying obtain fine extract ( Containing hyperin 12%); complex crystallization, take 100g of fine extract, add 1000ml of 95% ethanol, h...

Embodiment 2

[0019] Take 1 kg of hollyhock flower coarse powder, add 10,000 ml of 80% ethanol aqueous solution, heat and reflux for extraction for 1-2 hours, extract 2-3 times in total, and combine the extracts; concentrate the extracts under reduced pressure to 1 / 2 5 volumes, let it stand for 12 hours and filter; the filtrate was chromatographed by HPD100 or HPD600 macroporous adsorption resin column, first washed with water for 5-8 column volumes, eluted with 10% ethanol for 1-2 column volumes, and then washed with 70% ethanol Eluted to free of AlCl 3 React, collect 70% ethanol eluate; Concentrate the eluate under reduced pressure at a temperature lower than 60°C, and dry in vacuo to obtain the crude extract of hollyhock flower; take crude product 100g, add 1000ml ethyl acetate:ethanol=4:1 -8:1 (V / V) reflux extraction 3 times, 1-2 hours each time, recover the solvent, and dry under reduced pressure at 80°C to obtain the refined extract (containing 12% hyperoside); recrystallize and extra...

Embodiment 3

[0021] Embodiment 3: hyperoside freeze-dried powder injection

[0022] Preparation of powder injection preparation (1):

[0023] Component Quantity

[0024] Hyperin 5-50g

[0025] Tween 80 120g

[0026] Activated carbon 4g

[0027] Mannitol 400g

[0028] Poloxamer 8g

[0029] Hyperin dry powder, Tween, and poloxamer are melted and put into a mortar to grind to make them fully dispersed, add fresh water for injection saturated with carbon dioxide to 3500ml, add mannitol, and place in a water bath (50-70°C) Add activated carbon for needles, stir while adding, boil for 5-10 minutes, cool to 40°C and filter with a vertical fusing filter. Dilute it with fresh water for injection to 4000ml, measure the pH and pass the content, pass through a 0.45um membrane, then pass through a 0.22um membrane, fill in 1000 vials, pre-freeze, and freeze to obtain 5-50mg hypericum per bottle Glycoside freeze-dried powder.

[0030]Preparation of powder injection preparation (2): Take 5-50 g of...

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Abstract

A method for extracting hyperin comprises the following steps: a crude product of an extracting solution of a maniod eibish flower is obtained through extracting the concentrated solution of a maniod eibish flow ethanol extracting solution by normal butanol or ethyl acetate or through the column chromatography of an HPD100 or HPD600 macroscopic absorbent resin; and then hyperin with the content of between 90 and 98 percent in weight percentage is obtained through purification and recrystallization by using a solvent. Hyperin preparations comprise freeze-dried powder injection, liquid drugs injection, transfusions, dropped pills, tablets, capsules, or soft capsules prepared by using hyperin as an active component and pharmaceutical adjuvant. The hyperin is used for preparing the medicines for treating cerebral ischemia.

Description

1. Technical field [0001] The invention relates to a method for extracting active ingredients from Chinese herbal medicines, in particular to a method for extracting hyperin and its preparation and use. 2. Background technology [0002] Hyperin (chemically called quercetin-3′-O-β-D-galactose) is an active ingredient in traditional Chinese medicine such as marshmallow flowers. Hyperin has the pharmacological effects of analgesia, liver protection and anti-hepatitis B. [0003] Application No. 02146370.0 discloses "a preparation method of hyperin and its new application in medicine". The dried hollyhock flower is crushed into a coarse powder, extracted by heating under reflux with a hydrophilic solvent or extracted by cold immersion and percolation, and the extract is concentrated to Specific gravity 1.15-1.30 (70 ℃) extract, water-soluble, filtered, polyamide carrier on the filtrate column chromatography, collecting water-alcohol eluate, concentrated, vacuum-dried to obtain ...

Claims

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Application Information

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IPC IPC(8): C07H17/07A61K31/7048A61K36/185A61P9/10
Inventor 王勤周春晓陈志武袁慧汪年生赵磊
Owner 周春晓
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