CN101953880B - Method for preparing pueraria flavonid - Google Patents
Method for preparing pueraria flavonid Download PDFInfo
- Publication number
- CN101953880B CN101953880B CN 200910023425 CN200910023425A CN101953880B CN 101953880 B CN101953880 B CN 101953880B CN 200910023425 CN200910023425 CN 200910023425 CN 200910023425 A CN200910023425 A CN 200910023425A CN 101953880 B CN101953880 B CN 101953880B
- Authority
- CN
- China
- Prior art keywords
- water
- radix puerariae
- flavone
- extracting solution
- column chromatography
- 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.)
- Expired - Fee Related
Links
- 238000000034 method Methods 0.000 title claims abstract description 16
- BWWAFUZQSLIIIH-UHFFFAOYSA-N 2-phenyl-3H-chromen-3-id-4-one Chemical compound O1C(=[C-]C(=O)C2=CC=CC=C12)C1=CC=CC=C1 BWWAFUZQSLIIIH-UHFFFAOYSA-N 0.000 title abstract 6
- 241000219780 Pueraria Species 0.000 title abstract 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000004440 column chromatography Methods 0.000 claims abstract description 10
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- 150000004676 glycans Chemical class 0.000 claims abstract description 7
- 229920001282 polysaccharide Polymers 0.000 claims abstract description 7
- 239000005017 polysaccharide Substances 0.000 claims abstract description 7
- 229930003944 flavone Natural products 0.000 claims description 25
- 235000011949 flavones Nutrition 0.000 claims description 25
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 claims description 25
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 claims description 24
- 150000002212 flavone derivatives Chemical class 0.000 claims description 24
- 239000007788 liquid Substances 0.000 claims description 14
- 239000002994 raw material Substances 0.000 claims description 9
- 239000011347 resin Substances 0.000 claims description 9
- 229920005989 resin Polymers 0.000 claims description 9
- 239000012535 impurity Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 4
- 239000003818 cinder Substances 0.000 claims description 3
- 238000010521 absorption reaction Methods 0.000 claims description 2
- 238000011010 flushing procedure Methods 0.000 claims description 2
- 239000002904 solvent Substances 0.000 abstract description 4
- 238000001035 drying Methods 0.000 abstract description 3
- 239000003960 organic solvent Substances 0.000 abstract 2
- 241000196324 Embryophyta Species 0.000 abstract 1
- 235000010575 Pueraria lobata Nutrition 0.000 abstract 1
- 241000219781 Pueraria montana var. lobata Species 0.000 abstract 1
- 239000004480 active ingredient Substances 0.000 abstract 1
- 238000002791 soaking Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 5
- 238000009835 boiling Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229920001661 Chitosan Polymers 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000010828 elution Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000004556 brain Anatomy 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 210000004351 coronary vessel Anatomy 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 150000002213 flavones Chemical class 0.000 description 1
- 229930003935 flavonoid Natural products 0.000 description 1
- 150000002215 flavonoids Chemical class 0.000 description 1
- 235000017173 flavonoids Nutrition 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 230000004089 microcirculation Effects 0.000 description 1
- 150000002772 monosaccharides Chemical class 0.000 description 1
- 230000002107 myocardial effect Effects 0.000 description 1
- 230000036284 oxygen consumption Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002195 soluble material Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
- 238000003809 water extraction Methods 0.000 description 1
Landscapes
- Medicines Containing Plant Substances (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Saccharide Compounds (AREA)
Abstract
The invention provides a method for preparing pueraria flavonid, belongs to a method for extracting active ingredients of a plant, in particular to a method for extracting the pueraria flavonid, and provides a method for preparing the pueraria flavonid without organic solvent residue or peculiar smell and with good water solubility. The method comprises the following steps of: soaking kudzu root serving as a raw materail in water for decocting; separating decoction and dregs; performing column chromatography on extracting solution; eluting with water to receive the pueraria flavonid and polysaccharide; and concentrating and drying to obtain the pueraria flavonid. In the preparation method, the solvent is completely water, and the decoction is subjected to column chromatography and eluted with water so as to fulfill the aims of complete water solution, no organic solvent residue and no peculiar smell.
Description
Technical field
The invention belongs to the extracting method of effective ingredients in plant, relate in particular to the extracting method of Radix Puerariae flavone.
Background content
Radix Puerariae flavone has the microcirculation of improvement, and coronary artery dilator increases brain and coronary flow, and decreased heart rate reduces the effect of myocardial oxygen consumption, is widely used in medicine, health product and food service industry.Traditional production Radix Puerariae flavone method is: Radix Puerariae alcohol extraction, extract n-butanol extraction, extract again with the acetic acid crystallization, dry to get Radix Puerariae flavone, the conventional production methods Main Problems is that n-butyl alcohol, acetic acid boiling point are high, the corresponding high temperature drying that needs of high boiling solvent, dry run produces again the gum sugar abnormal flavour, the poorly water-soluble of Radix Puerariae flavone and dissolvent residual, having limited the interior many kinds of industry can not use, and market can not get expanding.In order to solve the existing problem of conventional production methods, just the someone has proposed the extracting method without high boiling solvent, such as patent No. ZL031155383, name is called " a kind of extracting method of Radix Puerariae total flavones ", disclose a kind of employing water extraction, the chitosan remove impurity, the method of purification by macroporous resin, improve the purity of extract, but, weak point is: the method chitosan is only removed molecular weight greater than 200,000 above impurity, adsorption column adopts again pure desorbing, and the molecular weight of flavonoid only is 300-400, that is to say that molecular weight 400-20 ten thousand remains in this product with interior macromolecular substances, its water solublity is that 2% flavone aqueous solution is slightly placed and just produced that water-insoluble suspends and precipitation.
Summary of the invention
The technical problem to be solved in the present invention is: propose that a kind of organic solvent-free is residual, the preparation method of the Radix Puerariae flavone of free from extraneous odour and good water solubility.
The technical scheme of technical solution problem of the present invention is: take Radix Puerariae as raw material, Radix Puerariae is immersed in the water decoction, separates melt cinder, with the extracting solution column chromatography, wash with water, receive Radix Puerariae flavone and polysaccharide, then concentrated, the dry Radix Puerariae flavone that gets.
The present invention is said to be immersed in the water decoction with Radix Puerariae, and material-water ratio is 1 part of raw material weight, water body accumulated amount 8-15 part.
The said extracting solution column chromatography of the present invention is that extracting solution is adsorbed by resin column.
The resin that extracting solution column chromatography of the present invention adopts is resinene or non-polar resin.
The resinene that extracting solution column chromatography of the present invention adopts is that LSA-21 or non-polar resin are D101.
The present invention is said to be washed with water, and the method that receives Radix Puerariae flavone and polysaccharide is: liquid dumps under the post during the extracting solution upper prop, behind the water yield flushing impurity with post layer volume twice, receives feed liquid, and quantities received is 10 times of raw materials.
Said concentrated the referring to membrance concentration or concentrated with steam of the present invention.
The invention has the beneficial effects as follows:
The whole waters of the preparation method of the Radix Puerariae flavone of good water solubility of the present invention are as solvent, and decocting boils column chromatography on the feed liquid, washes with water again, reach solve water entirely molten, organic solvent-free is residual and the purpose of free from extraneous odour; The absorption of macromolecule slightly water-soluble material remains in and reaches centrifugation in the resin column, receive and keep polysaccharide and flavone part, therefore, it is complete molten without suspending without precipitation that the Radix Puerariae flavone that preparation method of the present invention obtains can reach 10% Radix Puerariae flavone aqueous solution, has fabulous water solublity.
The specific embodiment
Embodiment 1
1 kilogram of Radix Puerariae raw material, Radix Puerariae immersed in the 5L water decoct two times each 2 hours, separate melt cinder, during material loading under the post under the post of water and washing 2L liquid to discard the water elution liquid of (containing monosaccharide and small-molecular weight impurity) washing behind the 2L be that polysaccharide and flavone feed liquid receive 10L altogether, through concentrated flavone 94g, the general flavone content 68% of drying to get.
Embodiment 2
1 kilogram of Radix Puerariae raw material, decocting method gets water feed liquid 10L with example 1, resin per hour 1L of the upper column chromatography speed of D101 (nonpolar) 1L, liquid all discards under the front 2L post of upper water feed liquid and washing, later water elution liquid receives 10L, through membrance concentration, dry to get flavone 86g, general flavone content 68%.
The said material quantity of preparation method of the present invention and amount of liquid: raw material is the weight of unit kilogram, and liquid is the volume that unit rises, and its quantity respectively is described consumption unit than the consumption unit that relates to.
Claims (2)
1. the preparation method of a Radix Puerariae flavone is characterized in that: take Radix Puerariae as raw material, Radix Puerariae is immersed in the water decoction, separates melt cinder, with the extracting solution column chromatography, wash with water, receive Radix Puerariae flavone and polysaccharide, then use membrance concentration, the dry Radix Puerariae flavone that gets; Said extracting solution column chromatography is that extracting solution is adopted resin D101 absorption by resin column; Said washing with water, the method that receives Radix Puerariae flavone and polysaccharide be, liquid dumps under the post during the extracting solution upper prop, behind the water yield flushing impurity with post layer volume twice, receives feed liquid, and quantities received is 10 times of raw materials.
2. the preparation method of Radix Puerariae flavone according to claim 1 is characterized in that: said Radix Puerariae is immersed in the water decoction, material-water ratio is 1 part of raw material weight, water body accumulated amount 8-15 part.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200910023425 CN101953880B (en) | 2009-07-21 | 2009-07-21 | Method for preparing pueraria flavonid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200910023425 CN101953880B (en) | 2009-07-21 | 2009-07-21 | Method for preparing pueraria flavonid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101953880A CN101953880A (en) | 2011-01-26 |
| CN101953880B true CN101953880B (en) | 2013-05-01 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200910023425 Expired - Fee Related CN101953880B (en) | 2009-07-21 | 2009-07-21 | Method for preparing pueraria flavonid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101953880B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108651650A (en) * | 2018-07-17 | 2018-10-16 | 佛山推启农业研究院（普通合伙） | A kind of stomach-nourishing health tea and preparation method thereof |
| CN111528473A (en) * | 2020-04-24 | 2020-08-14 | 浙江师范大学行知学院 | Method for preparing radix puerariae aqueous extract by utilizing natural selenium-rich radix puerariae residues |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1872081A (en) * | 2005-06-03 | 2006-12-06 | 天津天士力制药股份有限公司 | Application of kudzuvine root flavone in preparing medicine for treating chronic insufficiency of blood supply for brain |
-
2009
- 2009-07-21 CN CN 200910023425 patent/CN101953880B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1872081A (en) * | 2005-06-03 | 2006-12-06 | 天津天士力制药股份有限公司 | Application of kudzuvine root flavone in preparing medicine for treating chronic insufficiency of blood supply for brain |
Non-Patent Citations (1)
| Title |
|---|
| 欧来良等.吸附树脂对葛根中葛根素的分离研究.《中草药》.2003,第34卷(第2期),134-136. * |
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| Publication number | Publication date |
|---|---|
| CN101953880A (en) | 2011-01-26 |
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| C14 | Grant of patent or utility model | ||
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Effective date of registration: 20170322 Address after: 725101 Hanyin County of Shaanxi Province River Industrial Park (Pu Xi se Food Industrial Park) Patentee after: Hanyin Huaye Plant Health Pharmaceutical Co.,Ltd. Address before: 725000 Shaanxi Ankang City, Wenchang Road, No. 2 Patentee before: ANKANG ZHILANG BIOLOGICAL RESOURCES APPLICATION Research Institute |
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| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20130501 |