CN102218087A - Method for preparing total flavone extracts of pagoda flower - Google Patents

Method for preparing total flavone extracts of pagoda flower Download PDF

Info

Publication number
CN102218087A
CN102218087A CN 201110112487 CN201110112487A CN102218087A CN 102218087 A CN102218087 A CN 102218087A CN 201110112487 CN201110112487 CN 201110112487 CN 201110112487 A CN201110112487 A CN 201110112487A CN 102218087 A CN102218087 A CN 102218087A
Authority
CN
China
Prior art keywords
ethanol
solution
flos robiniae
robiniae pseudoacaciae
total flavone
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN 201110112487
Other languages
Chinese (zh)
Other versions
CN102218087B (en
Inventor
初正云
初明
李艳艳
翟延君
康廷国
王添敏
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Liaoning University of Traditional Chinese Medicine
Original Assignee
Liaoning University of Traditional Chinese Medicine
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Liaoning University of Traditional Chinese Medicine filed Critical Liaoning University of Traditional Chinese Medicine
Priority to CN 201110112487 priority Critical patent/CN102218087B/en
Publication of CN102218087A publication Critical patent/CN102218087A/en
Application granted granted Critical
Publication of CN102218087B publication Critical patent/CN102218087B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

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 preparation method of Flos Robiniae Pseudoacaciae extractive of general flavone
Technical field
The present invention relates to a kind of extraction preparation method 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 by water or ethanol extraction, extracts the method for preparing its extractive of general flavone through macroporous adsorbent resin separation and purification and magnesium oxide decolouring from Flos Robiniae Pseudoacaciae (comprising alabastrum).
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 for the treatment of haematemesis, spitting of blood, large intestine hematochezia and the women is red collapses.Mainly contain flavones ingredient in spending, based on robinin, rhamnose robinin etc.Flavones ingredient has than the wide biological activity effect, as reconcile blood pressure, microcirculation improvement, resist myocardial ischemia, infection and antitumor etc.
Summary of the invention
Purpose of the present 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 preparation method 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 was extracted 1-3 hour at every turn, filter, merging filtrate left standstill the leaching supernatant 12-24 hour, discard 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 standby 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 wash with water earlier, and reuse 75% alcohol is washed, and collect ethanol elution and obtain 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 height of production is suitable for suitability for industrialized production.
The specific embodiment
A kind of preparation method of Flos Robiniae Pseudoacaciae extractive of general flavone is to get Flos Robiniae Pseudoacaciae (comprising alabastrum) coarse powder 500g, use 20 times respectively, 75% alcohol reflux of 15 times and 10 times amounts three times, each 2 hours, filter merging filtrate, static 12 hours, the leaching supernatant, reclaim ethanol to there not being the alcohol flavor, be diluted with water to 5000ml, last macroporous adsorbent resin D-101 post, it is very light to be washed to color, reuse 75% ethanol is washed, and the ethanol elution of gained added the magnesium oxide reflux decolour 1 hour by every liter 50 gram, filtered, filtrate recycling ethanol, concentrating under reduced pressure, spray drying gets Flos Robiniae Pseudoacaciae extract 25 grams (yield 5%), and general flavone content is 52%.

Claims (4)

1. the preparation method 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, and filtrate recycling ethanol is to there not being the alcohol flavor, be diluted with water to again and be equivalent to Flos Robiniae Pseudoacaciae 0.1g/ml, extracting solution is standby;
(2) extracting solution with step 1 gained adopts the D101 purification by macroporous resin, 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, when eluting solvent preferred water and ethanol, wash with water earlier, reuse 75% alcohol is washed, and 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, 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 pagodatree flower general flavone extract.
2. the preparation method 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 preparation method 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 preparation method 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)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 201110112487 CN102218087B (en) 2011-05-03 2011-05-03 Method for preparing total flavone extracts of pagoda flower

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN 201110112487 CN102218087B (en) 2011-05-03 2011-05-03 Method for preparing total flavone extracts of pagoda flower

Publications (2)

Publication Number Publication Date
CN102218087A true CN102218087A (en) 2011-10-19
CN102218087B CN102218087B (en) 2012-09-05

Family

ID=44774958

Family Applications (1)

Application Number Title Priority Date Filing Date
CN 201110112487 Expired - Fee Related CN102218087B (en) 2011-05-03 2011-05-03 Method for preparing total flavone extracts of pagoda flower

Country Status (1)

Country Link
CN (1) CN102218087B (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103040919A (en) * 2012-12-29 2013-04-17 黄家芬 Method for extracting general flavone from red bean
CN105434482A (en) * 2015-12-30 2016-03-30 甘肃省医学科学研究院 Enrichment method of total flavonoids in pine needles of Cedrus deodara and application of total flavonoids in pine needles of Cedrus deodara in tumor suppression
CN105998154A (en) * 2016-06-16 2016-10-12 辽宁大学 Preparation method for total flavonoids in V.amoena Fisch.var.angusta Freyn.
ES2607147A1 (en) * 2015-09-29 2017-03-29 Biopharma Research, S.A. Use of an acacia vegetable extract to foster growth and radicular activity in plants (Machine-translation by Google Translate, not legally binding)

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

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)

* Cited by examiner, † Cited by third party
Title
《江苏调味副食品》 20080531 李凤林等 天然黄酮类化合物分离纯化研究进展 第25卷, 第5期 *

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103040919A (en) * 2012-12-29 2013-04-17 黄家芬 Method for extracting general flavone from red bean
CN103040919B (en) * 2012-12-29 2015-04-15 黄家芬 Method for extracting general flavone from red bean
ES2607147A1 (en) * 2015-09-29 2017-03-29 Biopharma Research, S.A. Use of an acacia vegetable extract to foster growth and radicular activity in plants (Machine-translation by Google Translate, not legally binding)
CN105434482A (en) * 2015-12-30 2016-03-30 甘肃省医学科学研究院 Enrichment method of total flavonoids in pine needles of Cedrus deodara and application of total flavonoids in pine needles of Cedrus deodara in tumor suppression
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
CN105998154A (en) * 2016-06-16 2016-10-12 辽宁大学 Preparation method for total flavonoids in V.amoena Fisch.var.angusta Freyn.
CN105998154B (en) * 2016-06-16 2021-04-09 辽宁大学 Preparation method of total flavonoids in narrow-leaved vetch

Also Published As

Publication number Publication date
CN102218087B (en) 2012-09-05

Similar Documents

Publication Publication Date Title
CN104940246B (en) A method of extracting coprinus comatus element from coprinus comatus
CN112870236B (en) Flavone effective part of abelmoschus manihot and preparation method and application thereof
CN102218087B (en) Method for preparing total flavone extracts of pagoda flower
CN109293712A (en) The industrialized utilization method and its steviol glycoside and chlorogenic acid of a kind of STEVIA REBAUDIANA
CN102552340A (en) Preparation method of ginkgolide monomer and total ginkgo flavone-glycoide
CN101973853A (en) Method for extracting hydroxytyrosol
CN102453075A (en) Separation and purification process of glycyrrhizic acid
CN106176847A (en) A kind of have Quinoa saponin strengthening bacteriostasis and preparation method thereof
CN101838299B (en) Method for separating and purifying natural acteoside
CN101648901A (en) Method for preparing indirubin
CN101348474A (en) Method for preparing salvianolic acid B and tanshinol from Salvia miltiorrhiza stem
CN102895294B (en) Astragalus mongholicus injection and preparation method thereof
CN101108871A (en) Technique for extracting cycli phosphate adenosine from chinese date
CN107126452A (en) Gypenosides and preparation method thereof
CN105477026B (en) A kind of technique of combined extracting ginkgoic acid, flavones and terpene lactones and polysaccharide from gingko episperm
CN103665094A (en) Preparation method for extracting and purifying tanshinone monomeric compounds from red sage root
CN103408610B (en) The method of arbutin is extracted from leaf of pear tree
CN102060822A (en) Method for extracting esculetin from herba violae
CN101768201A (en) Preparation method of oleanolic acid
CN104945450B (en) A kind of method that Stibene-glucoside is extracted from the vine of multiflower knotweed
CN103059086A (en) Extraction and purification method of cordycepin from cordyceps militaris solid mediums
CN103588832B (en) Hederacoside C and the method for aglycon is separated from Rhizoma Calystegiae Hederaceae
CN103408645B (en) A kind of method prepared by polysaccharide-peptide
CN102329345A (en) Method for extracting and purifying sarmentosin in Sedum sarmentosum Bunge
CN102329350A (en) Method for extracting mulberroside A from white mulberry root-bark

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20120905

Termination date: 20150503

EXPY Termination of patent right or utility model