CN102218087B - Method for preparing total flavone extracts of pagoda flower - Google Patents

Method for preparing total flavone extracts of pagoda flower Download PDF

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Publication number
CN102218087B
CN102218087B CN 201110112487 CN201110112487A CN102218087B CN 102218087 B CN102218087 B CN 102218087B CN 201110112487 CN201110112487 CN 201110112487 CN 201110112487 A CN201110112487 A CN 201110112487A CN 102218087 B CN102218087 B CN 102218087B
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ethanol
flos robiniae
robiniae pseudoacaciae
solution
extractive
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CN102218087A (en
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初正云
初明
李艳艳
翟延君
康廷国
王添敏
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Liaoning University of Traditional Chinese Medicine
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Liaoning University of Traditional Chinese Medicine
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  • Coloring Foods And Improving Nutritive Qualities (AREA)

Abstract

The invention provides a method for preparing total flavone extracts of pagoda flower. The method comprises the following process steps of: picking fresh or dry pagoda flowers, and grinding the pagoda flower to obtain coarse powder; adding 75 percent ethanol in an amount which is 10 to 20 times the weight of the coarse powder, and performing refluxing extraction for 2 to 3 times, wherein the time for each extraction is 1 to 3 hours; mixing the filtration solution, standing the solution for 12 to 24 hours, obtaining supernatant by filtration, discarding precipitates, and recovering the ethanol from the filtration solution until the filtration solution is free of alcohol smell; adding water to dilute the solution until 0.1g of pagoda flower is contained in 1 ml of solution, purifying the extraction solution by using D101 macroporous resin, washing the solution first by water and then by 75 percent ethanol, and collecting ethanol eluent to obtain total flavone eluent of pagoda flower; and discoloring and purifying the eluent by magnesium oxide, and performing ethanol recovery, condensation and drying of the obtained total flavone extraction solution of pagoda flower to obtain the total flavone extracts of pagoda flower. The method is simple, practical, low in production cost and suitable for industrialized production, and the total flavone extracts of pagoda flower prepared by the method is high in purity.

Description

A kind of method for preparing of Flos Robiniae Pseudoacaciae extractive of general flavone
Technical field
The present invention relates to a kind of extraction method for preparing of medicine material, be specifically related to the novel preparation method of Flos Robiniae Pseudoacaciae extractive of general flavone.Method of the present invention is meant through water or ethanol extraction, from Flos Robiniae Pseudoacaciae (comprising alabastrum), extracts the method for preparing its extractive of general flavone through macroporous adsorbent resin separation and purification and magnesium oxide decolouring.
Background technology
Flos Robiniae Pseudoacaciae be the leguminous plant Robinia pseudoacacia L. ( Robinia pseudoacaciaL.) dry flower and alabastrum.Beginning is stated from " Guizhou side's medicine among the people collection ", its sweet in the mouth, and property is flat, slightly poisonously goes into Liver Channel, and astringing to arrest bleeding cures mainly spitting of blood, large intestine hematochezia, metrorrhagia.All there is distribution in 24 provinces in the whole nation, and reserves are very abundant.Its flower, root, Ye Junke are used as medicine, and among the peoplely are used to treat haematemesis, spitting of blood, large intestine hematochezia and the women is red collapses.Mainly containing flavones ingredient in spending, is main with robinin, rhamnose robinin etc.Flavones ingredient has than the wide biological activity effect, as reconciling blood pressure, microcirculation improvement, resisting myocardial ischemia, infection and antitumor etc.
Summary of the invention
The object of the invention provides a kind of method for preparing the Flos Robiniae Pseudoacaciae extractive of general flavone, and this method can increase substantially the purity of the total pyrite extract of Flos Robiniae Pseudoacaciae.
The technical scheme that adopts is:
A kind of method for preparing of Flos Robiniae Pseudoacaciae extractive of general flavone comprises following processing step:
1, gets fresh or exsiccant Flos Robiniae Pseudoacaciae, be ground into coarse powder, adopt water or ethanol extraction; When adopting ethanol extraction, add raw material 10-20 and doubly measure the ethanol that concentration is 60-75%, reflux, extract, 2-3 time; The each extraction 1-3 hour filtered merging filtrate; Left standstill 12-24 hour, the leaching supernatant discards precipitate; Filtrate recycling ethanol is not equivalent to Flos Robiniae Pseudoacaciae 0.1g/ml to having the alcohol flavor, being diluted with water to, and it is subsequent use to get extracting solution;
2, the extracting solution with step 1 gained adopts the macroporous resin adsorption purification, and macroporous resin adopts D101, AB-8, HP-20, DM-301, HPD-400 or HPD-600 resin;
Eluting solvent adopts one or more in water, methanol, ethanol, aqueous methanol, the aquiferous ethanol; Select for use above-mentioned eluent to carry out certain density eluting during eluting or carry out gradient elution, eluting solvent preferred water and ethanol, promptly earlier with washing, reuse 75% alcohol is washed, and collects ethanol elution and obtains the total pyrite eluent of Flos Robiniae Pseudoacaciae;
3, with the resulting Flos Robiniae Pseudoacaciae total flavones of step 2 eluent further with the magnesium oxide purification that decolours, consumption is regulated according to the depth of actual color, the total flavones extracting solution that obtains is through reclaiming ethanol, concentrating, be drying to obtain the Flos Robiniae Pseudoacaciae extractive of general flavone.
Above-mentioned Flos Robiniae Pseudoacaciae comprises alabastrum.
Above-mentioned magnesium oxide addition is per 10 liters and adds the 500g magnesium oxide.
Above-mentioned concentration operation can adopt conventional concentrating or concentrating under reduced pressure, and drying can adopt conventional drying below 80 ℃, vacuum drying, spray drying or lyophilization.
The yield of the Flos Robiniae Pseudoacaciae extractive of general flavone that application the inventive method obtains is that content of total flavone is greater than 40% more than 2%.Content assaying method adopts spectrophotography (AlCl 3Colour developing is measured trap at 395nm, is reference with the robinin).
This extract can be applied in the medicament of various treating correlative diseases as crude drug separately or with the other medicines combination.
The inventive method is simple and practical, and production cost is low, and the Flos Robiniae Pseudoacaciae extractive of general flavone purity of production is high, is suitable for suitability for industrialized production.
The specific embodiment
A kind of method for preparing of Flos Robiniae Pseudoacaciae extractive of general flavone is to get Flos Robiniae Pseudoacaciae (comprising alabastrum) coarse powder 500g, uses 20 times respectively, 75% alcohol reflux of 15 times and 10 times amounts three times, each 2 hours; Filter merging filtrate, static 12 hours, leaching supernatant; Reclaim ethanol to there not being the alcohol flavor, be diluted with water to 5000ml, last macroporous adsorbent resin D-101 post; Wash to color very lightly, reuse 75% ethanol is washed, and the ethanol elution of gained added the magnesium oxide reflux decolour 1 hour by every liter 50 gram; Filter, filtrate recycling ethanol, concentrating under reduced pressure, spray drying get Flos Robiniae Pseudoacaciae extract 25 grams (yield 5%), and general flavone content is 52%.

Claims (4)

1. the method for preparing of a Flos Robiniae Pseudoacaciae extractive of general flavone is characterized in that comprising following processing step:
(1), get fresh or exsiccant Flos Robiniae Pseudoacaciae, be ground into coarse powder, add 10-20 and doubly measure the ethanol that concentration is 60-75%, reflux, extract, 2-3 time; The each extraction 1-3 hour filtered merging filtrate; Left standstill 12-24 hour, the leaching supernatant discards precipitate; Filtrate recycling ethanol is not equivalent to Flos Robiniae Pseudoacaciae 0.1g/ml to having the alcohol flavor, being diluted with water to, and it is subsequent use to get extracting solution;
(2) extracting solution with step 1 gained adopts purification by macroporous resin, and macroporous resin adopts D101, AB-8, HP-20, DM-301, HPD-400 or HPD-600 resin;
Eluting solvent adopts water and ethanol; Earlier with washing, reuse 75% ethanol is washed during eluting, collects ethanol elution and obtains Flos Robiniae Pseudoacaciae total flavones eluent;
(3), with the resulting Flos Robiniae Pseudoacaciae total flavones of step 2 eluent further with the magnesium oxide purification that decolours, the magnesium oxide addition is 50g/L, the total flavones extracting solution that obtains is through reclaiming ethanol, concentrating, be drying to obtain the Flos Robiniae Pseudoacaciae extractive of general flavone.
2. the method for preparing of a kind of Flos Robiniae Pseudoacaciae extractive of general flavone according to claim 1 is characterized in that described Flos Robiniae Pseudoacaciae comprises alabastrum.
3. the method for preparing of a kind of Flos Robiniae Pseudoacaciae extractive of general flavone according to claim 1 is characterized in that the magnesium oxide addition is per 10 liters and adds the 500g magnesium oxide.
4. the method for preparing of a kind of Flos Robiniae Pseudoacaciae extractive of general flavone according to claim 1 is characterized in that described concentration operation adopts conventional concentrating or concentrating under reduced pressure, dry employing conventional drying below 80 ℃, vacuum drying, spray drying or lyophilization.
CN 201110112487 2011-05-03 2011-05-03 Method for preparing total flavone extracts of pagoda flower Expired - Fee Related CN102218087B (en)

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CN103040919B (en) * 2012-12-29 2015-04-15 黄家芬 Method for extracting general flavone from red bean
ES2607147B1 (en) * 2015-09-29 2018-01-17 Biopharma Research, S.A. USE OF AN ACACIA VEGETABLE EXTRACT TO PROMOTE RADICULAR GROWTH AND ACTIVITY IN PLANTS
CN105434482B (en) * 2015-12-30 2019-05-24 甘肃省医学科学研究院 A kind of enrichment method of cedar needles general flavone and its application in antitumor
CN105998154B (en) * 2016-06-16 2021-04-09 辽宁大学 Preparation method of total flavonoids in narrow-leaved vetch

Citations (4)

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Publication number Priority date Publication date Assignee Title
CN1395573A (en) * 2000-01-11 2003-02-05 比奥雷克斯健康有限公司 Extraction of flavonoids
CN1615947A (en) * 2004-09-16 2005-05-18 凌沛学 Medicine for treating oral ulcer, gastric ulcer, burn and scald and traumatic infection and preparing method
CN1994337A (en) * 2006-11-11 2007-07-11 周亚球 Total flavone extract of maniod eibish, its preparation and application
CN101385748A (en) * 2008-09-05 2009-03-18 周春晓 Maniod ebish flower extract, extraction and analysis method and extract preparation and use thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1395573A (en) * 2000-01-11 2003-02-05 比奥雷克斯健康有限公司 Extraction of flavonoids
CN1615947A (en) * 2004-09-16 2005-05-18 凌沛学 Medicine for treating oral ulcer, gastric ulcer, burn and scald and traumatic infection and preparing method
CN1994337A (en) * 2006-11-11 2007-07-11 周亚球 Total flavone extract of maniod eibish, its preparation and application
CN101385748A (en) * 2008-09-05 2009-03-18 周春晓 Maniod ebish flower extract, extraction and analysis method and extract preparation and use thereof

Non-Patent Citations (1)

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Title
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