CN102863489A - Method for extracting catalpol from rehmannia stem - Google Patents
Method for extracting catalpol from rehmannia stem Download PDFInfo
- Publication number
- CN102863489A CN102863489A CN2011101848071A CN201110184807A CN102863489A CN 102863489 A CN102863489 A CN 102863489A CN 2011101848071 A CN2011101848071 A CN 2011101848071A CN 201110184807 A CN201110184807 A CN 201110184807A CN 102863489 A CN102863489 A CN 102863489A
- Authority
- CN
- China
- Prior art keywords
- catalpol
- stem
- concentrated solution
- ethanol
- radix codonopsis
- 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.)
- Pending
Links
Images
Abstract
The invention relates to a method for extracting catalpol from rehmannia stem, which belongs to the medicine technical field. The method comprises the following steps: 1) rehmannia stem and water are heated for backflow extraction, an extract is performed pressure reduction and concentration to obtain a concentrate A; 2) 95% of ethanol is added in the concentrate A, standing is carried out for overnight, a supernate is performed pressure reduction and concentration to obtain a concentrate B; 3) a concentrate B is led to a XAD-16 macroporous resin column, elution is carried out by water, then elution is carried out by ethanol, an ethanol eluate is collected, the pressure reduction and concentration are carried out to obtain a stiff paste; 4) silica gel is added in the stiff paste, dried and a silica gel column is added, elution is carried out by ethyl acetate/methanol according to ratio of 4:1, a target fraction is collected, the pressure reduction, concentration and drying processes are carried out; 5) recrystallization is carried out on a dried object, the processes of filtering and drying are carried out to obtain the catalpol pure product. Compared with the prior art, the method of the invention has the characteristics of strong industrialization operationality, high extraction efficiency, resource preservation and environmental protection.
Description
Technical field
The present invention relates to a kind of method of from the Chinese medicine stem of Radix Codonopsis lanceolatae, extracting Catalpol, belong to medical technical field.
Background technology
1962, W.H.Lunn etc. at first separated from the fresh fruit of Chinese catalpa Catalpa ovata and obtain catalposide, and then with the catalposide basic hydrolysis, hydrolysate has obtained Catalpol behind recrystallization, and this is the earliest report of Catalpol.Nineteen sixty-five, R.B.Duff etc. adopt gac, diatomite as filler, and through column chromatography repeatedly, last water recrystallization separates having obtained naturally occurring Catalpol first from the leaf of Buddleia globosa.
1971, the Beichuan merit of Japan etc. were studied the blood sugar reducing component of glutinous rehmannia, and they have obtained having remarkable hypoglycemic activity active princlple R-BP-F at separation from bosom celebrating glutinous rehmannia, and the main component in this component is separated through silica gel column chromatography, has obtained Catalpol.After this, people have found Catalpol again successively from tens kind of plant.
Studies show that, glutinous rehmannia is as ginseng section per nnial herb, generally is fresh or dried root is used as medicine.Radix Rehmanniae contains the number of chemical compositions such as iridoid glycosides, monoterpene and glycoside thereof, oligosaccharides, amino acids.Catalpol is the iridoid monoglycosides that content is the highest in the Radix Rehmanniae, is one of main active ingredient of glutinous rehmannia, has hypoglycemic and the effect of protection cranial nerve.Therefore, some are arranged about how from Rehmannia Root, extracting the report of Catalpol in the existing document, as: (1) patent 200710026330.8 adopts the Rehmannia Root extracting solution by active carbon column, macroporous resin column, cationic resin column, resin anion(R.A) post, nanofiltration membrane separation purifying Catalpol, its defective is that technique is more loaded down with trivial details, production cost is high, and practicality is not strong; (2) patent patent 200710159335.8 usefulness adopt Rehmannia Root extraction using alcohol Catalpol, concentrated solution is after sherwood oil, ethyl acetate extraction removal of impurities, by the macroporous resin separation and purification, discard 0～50% ethanol eluate, collect 80% alcohol elution, obtain the Catalpol sterling with methyl alcohol-alcohol crystal at last, its defective is that Catalpol is water-soluble better, this process using extraction using alcohol, and not only cost is high but also yield is low, collect 80% alcohol elution, be not inconsistent with the characteristic of Catalpol good water solubility; (3) patent 200910232807.7 relates to Rehmannia Root methanol extraction, n-butanol extraction, chloroform methanol eluting silica gel post, and defective is that process costs is high and complicated, and practicality is not strong; (4) related macroporous resin AB-8/ADS-7 removes impurity with 30% ethanol elution in the patent 200910264454.9 purification Catalpol techniques, collect 70-80% wash-out position and with ethyl acetate crystallization Catalpol, defective is and the Catalpol good water solubility that the characteristic that is insoluble in ethyl acetate is not inconsistent.The defective that exists in above-mentioned these patents will cause industrial practicality not strong, and the purity of perhaps extracting Catalpol is not high.
Present prior art all is that Radix Rehmanniae or Rehmannia Root root are extracted, and does not find to extract from stem of Radix Codonopsis lanceolatae the processing method of Catalpol.This mainly is that active constituent content is little can not be counted, and generally also is not used as medicinal material because the stem of Radix Codonopsis lanceolatae routine is considered to there is not pharmaceutical use, and as waste dispose (time precious traditional Chinese medical science traditional Chinese medicines, 2008,19 (1), 34-35.)。But applicant has been carried out in depth research to stem of Radix Codonopsis lanceolatae, has found a kind ofly take stem of Radix Codonopsis lanceolatae as raw material, can efficiently obtain the method for Catalpol.
Summary of the invention
The purpose of this invention is to provide a kind ofly take stem of Radix Codonopsis lanceolatae as raw material, extract the method for Catalpol.Technical problem to be solved by this invention is to adopt specific extracting method to extract highly purified Catalpol from stem of Radix Codonopsis lanceolatae.
The resulting Catalpol of method that extracts Catalpol from stem of Radix Codonopsis lanceolatae provided by the invention, purity is more than 90%.
Technical scheme of the present invention is:
The present invention extracts Catalpol from stem of Radix Codonopsis lanceolatae method is:
(1) with stem of Radix Codonopsis lanceolatae, the water heating and refluxing extraction, the extracting solution concentrating under reduced pressure gets concentrated solution A;
(2) in concentrated solution A, add 95% ethanol, standing over night, the supernatant liquor concentrating under reduced pressure gets concentrated solution B;
(3) with the upper XAD-16 macroporous resin column of concentrated solution B, wash with water first, use again ethanol elution, collect ethanol eluate, be evaporated to thick paste;
(4) thick paste is admixed silica gel, volatilize, add silicagel column, with 4: 1 wash-outs of ethyl acetate/methanol, collect object flow part, concentrating under reduced pressure, drying;
(5) dry thing recrystallization filters, and drying gets the Catalpol sterling.
Preferably, technical scheme of the present invention is:
(1) with after the stem of Radix Codonopsis lanceolatae pulverizing, water heating and refluxing extraction 2 times, each 1 hour, united extraction liquid was evaporated to relative density 1.13-1.16 (50 ℃), gets concentrated solution A;
(2) in concentrated solution A, added 90～100% ethanol in 1: 3 by volume～1: 5, standing over night, supernatant liquor is evaporated to relative density 1.07～1.13 (50 ℃), lets cool, and gets concentrated solution B;
(3) with the upper XAD-16 macroporous resin column (amount ratio 1: 4, blade diameter length ratio are 1: 5～1: 15) of concentrated solution B, use first 1～2.5BV water elution, use again 3～10% ethanol elutions of 1.5～3BV, collect 3～10% ethanol eluates, be evaporated to thick paste;
(4) thick paste is admixed 50～200 order silica gel, volatilized, add 50～200 order silicagel columns (amount ratio is 1: 5～1: 20), with 3: 1～5: 1 wash-outs of ethyl acetate/methanol, collect object flow part, concentrating under reduced pressure, drying;
(5) dry thing filters with 80～95% ethyl alcohol recrystallizations, and drying gets the Catalpol sterling.
More preferably, glutinous rehmannic stem and leaf extract of the present invention prepares by the following method:
(1) with after the stem of Radix Codonopsis lanceolatae pulverizing, water heating and refluxing extraction 2 times, each 1 hour, united extraction liquid was evaporated to relative density 1.14 (50 ℃), gets concentrated solution A;
(2) in concentrated solution A, added 95% ethanol in 1: 4 by volume, standing over night, supernatant liquor is evaporated to relative density 1.08 (50 ℃), lets cool, and gets concentrated solution B;
(3) with the upper XAD-16 macroporous resin column (amount ratio 1: 4, blade diameter length ratio are 1: 10) of concentrated solution B, use first the 2BV water elution, use again 6% ethanol elution of 2.2BV, collect 6% ethanol eluate, be evaporated to thick paste;
(4) thick paste is admixed 50-100 order silica gel, volatilized, add 100-200 order silicagel column (amount ratio is 1: 15), with 4: 1 wash-outs of ethyl acetate/methanol, collect object flow part, concentrating under reduced pressure, drying;
(5) dry thing 85% ethyl alcohol recrystallization filters, and drying gets the Catalpol sterling.
The above-mentioned method of extracting Catalpol from stem of Radix Codonopsis lanceolatae in the step (1), adds the water of 12 times of volumes of stem of Radix Codonopsis lanceolatae weight.
The above-mentioned method of extracting Catalpol from stem of Radix Codonopsis lanceolatae is to adopt the TLC method to collect object flow part, and the thin-layer chromatography condition is: developping agent is chloroform: methyl alcohol: water 14: 6: 1, developer are the aubepine developer, and Heating temperature is 105 ℃.
Advantage of the present invention is more to have practicality and creativeness than prior art:
(1) the raw material choose stem of Radix Codonopsis lanceolatae has more practicality
The Rehmannia Root root easily goes rotten, and catalpol content also significantly descends after placing; And stem of Radix Codonopsis lanceolatae more easily stores, and after placing for a long time or drying, catalpol content all changes not quite, can satisfy long-term large-scale production.
(2) extracting method has more the industrialization possibility, therefore has more practicality
1. without noxious solvent
In the whole technique, organic solvent only uses ethanol, ethyl acetate/methanol, without noxious solvent.Emerge in an endless stream instantly in drug and food safety problem and environmental protection problem, noxious solvent will directly have influence on industrial applicibility.The present invention does not use noxious solvent, has brought substantial contribution for practicality of the present invention.
2. sample solution pre-treatment
Owing to containing Dihuang polysaccharide, oligosaccharides and plant pigments constituents in the stem of Radix Codonopsis lanceolatae; therefore; before adopting resin technique to separate; must carry out pre-treatment to sample solution; can remove partial impurities on the one hand; improve the resin column separating effect, then can effectively protect resin column on the other hand, prolong the work-ing life of resin.
3. silica gel column chromatography dry column-packing
Reduce solvent load, saved industrial cost.
4. the nontoxic cheapness of recrystallization solvent
The present invention has adopted 85% ethanol of nontoxic cheapness, and the primary crystallization yield reaches more than 90%, has embodied again industrial applicibility of the present invention.
5. the TLC method is collected Catalpol, makes technique more succinct
The TLC method both can be determined the stream part of collecting according to the separation case of Catalpol and impurity, can determine the wash-out terminal point again, so since, extract and the analytical procedure unification, make method more succinct, and avoided solvent to waste and the loss of Catalpol on silicagel column.
(3) extracting method of the present invention is creative
1. economize on resources, more environmental protection
Preparation method of the present invention is raw material for stem of Radix Codonopsis lanceolatae, and the conventional medicinal part of the non-glutinous rehmannia of stem of Radix Codonopsis lanceolatae is processed as refuse for a long time, take stem of Radix Codonopsis lanceolatae as raw material, has enlarged the glutinous rehmannia medicine resource, has avoided the wasting of resources, has also increased medicinal herb grower's income simultaneously.Extract Catalpol and be different from known technology fully from stem of Radix Codonopsis lanceolatae, the present invention has overcome technology prejudice, and is creative.
2. catalpol content more than 90% in the finished product
The resulting catalpol content of the present invention reaches more than 90%, and its purity is very high, thereby can guarantee medicinal effect and high purity demand.The technique effect of the high purity Catalpol that the technical solution used in the present invention reaches meets the creative requirement of patent law fully.
In a word, the present invention meets the pharmacy requirement of relevant safe, efficient, the environmental protection of present country, therefore has more practicality; And any step of technique all rationally overcomes technology prejudice than the more ingenious of prior art design, and obvious technical effects has embodied creativeness of the present invention.
Description of drawings
The Catalpol TCL collection of illustrative plates of Fig. 1 embodiment of the invention 1, wherein 1, reference substance 2, sample
Fig. 2 Catalpol standard substance HPLC collection of illustrative plates
The Catalpol HPLC collection of illustrative plates of Fig. 3 embodiment 1
Experimental example
1, the selection of polymeric adsorbent
Purpose: adopt the Static Adsorption test, investigated respectively representative non-polar resin D101, XAD-16, HPD-300, low-pole resin CAD40, AB-8, HPD-750, polar resin HPD-600,7HP is to the adsorption effect of Catalpol.
Method: take by weighing approximately 50g of each resin of handling well, put in the 250ml ground Erlenmeyer flask, the accurate approximately 90ml (being equivalent to 100 gram stem of Radix Codonopsis lanceolatae) of pretreated alcohol precipitation concentrated solution that adds left standstill 24 hours, measures resin Catalpol is got adsorption rate (mg/g).Result such as following table 1:
Table 1 Static Adsorption Choice of Resin result
Cross in the post process resin to the absorb-elute effect of Catalpol in order further to investigate in reality, and the content situation of Catalpol after the separation and purification, preferred XAD-16, HPD-300, D101 carry out further dynamic adsorption test, method is as follows: get the resin 100g that handles well, pack in the glass column, loading after the water punching is real, standing adsorption.Use first purified water 150ml wash-out, collect water elution liquid, use again 300ml 7% ethanol elution, collect alcohol eluen.With alcohol eluen concentrating under reduced pressure, vacuum-drying.Measure respectively water lotion, 7% pure washing lotion, catalpol content in the dried cream.Result such as following table 2:
Table 2 dynamic adsorption Choice of Resin result
Conclusion: find by dynamic adsorption test, although these 3 kinds of resins differ the adsorption rate of Catalpol and not quite during static test, but when carrying out dynamic adsorption test, pure washing lotion Catalpol yield and dried cream content difference are apart from larger, and XAD-16 significantly is better than other resin to the separation and purification effect of Catalpol.
2, TLC collects Catalpol
A silicagel column wash-out stream part employing TLC method detects Catalpol, and the thin-layer chromatography condition: silica gel G plate, developping agent are chloroform: methyl alcohol: water 14: 6: 1, developer are the aubepine developer.Concrete operations: after getting an amount of stream part some plate, launch, dry, spray is heated to clear spot with the aubepine developer at 105 ℃.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.These embodiment are interpreted as only being used for explanation the present invention and are not used in restriction protection scope of the present invention.After the content of having read the present invention's record, those skilled in the art can make various changes or modifications the present invention, and these equivalences change and modification falls into claim limited range of the present invention equally.
Embodiment 1
Get the stem of Radix Codonopsis lanceolatae meal, 20.0kg adds 12 times of water gagings, heating and refluxing extraction 2 times, each 1 hour, united extraction liquid was evaporated to relative density 1.14 (50 ℃), added 95% ethanol in 1: 4 by volume, standing over night, supernatant liquor is evaporated to relative density 1.08 (50 ℃), concentrated solution lets cool, and adds XAD-16 macroporous resin column (amount ratio 1: 4, blade diameter length ratio are 1: 10), use first the 2BV water elution, use again 6% ethanol elution of 2.2BV, collect 6% ethanol eluate, be evaporated to thick paste, admix 50-100 order silica gel, volatilize, add 100-200 order silicagel column (amount ratio is 1: 15), with 4: 1 wash-outs of ethyl acetate/methanol, collect object flow part, concentrating under reduced pressure, drying, dry thing 85% ethyl alcohol recrystallization, filter, drying gets Catalpol sterling 188.5g, records to contain Catalpol 96.3%.
A silicagel column wash-out stream part employing TLC method detects Catalpol, and the thin-layer chromatography condition: silica-gel plate is Qingdao Haiyang chemical industry G plate, and developping agent is chloroform: methyl alcohol: water, 14: 6: 1, developer was the aubepine developer.Concrete operations: after getting an amount of stream part some plate, launch, dry, spray is heated to clear spot with the aubepine developer at 105 ℃.
Embodiment 2
Get the stem of Radix Codonopsis lanceolatae meal, 20.0kg adds 12 times of water gagings, heating and refluxing extraction 2 times, each 1 hour, united extraction liquid was evaporated to relative density 1.15 (50 ℃), added 100% ethanol in 1: 3 by volume, standing over night, supernatant liquor is evaporated to relative density 1.13 (50 ℃), concentrated solution lets cool, and adds XAD-16 macroporous resin column (amount ratio 1: 4, blade diameter length ratio are 1: 7), use first the 1BV water elution, use again 3% ethanol elution of 3BV, collect 3% ethanol eluate, be evaporated to thick paste, admix 100-200 order silica gel, volatilize, add 100-200 order silicagel column (amount ratio is 1: 20), with 5: 1 wash-outs of ethyl acetate/methanol, collect object flow part, concentrating under reduced pressure, drying, dry thing 80% ethyl alcohol recrystallization, filter, drying gets Catalpol sterling 178.7g, records to contain Catalpol 94.2%.
The TLC method is collected Catalpol object flow part with embodiment 1.
Embodiment 3
Get the stem of Radix Codonopsis lanceolatae meal, 50kg adds 12 times of water gagings, heating and refluxing extraction 2 times, each 1 hour, united extraction liquid was evaporated to relative density 1.16 (50 ℃), added 90% ethanol in 1: 5 by volume, standing over night, supernatant liquor is evaporated to relative density 1.10 (50 ℃), concentrated solution lets cool, and adds XAD-16 macroporous resin column (amount ratio 1: 4, blade diameter length ratio are 1: 5), use first the 1.5BV water elution, use again 10% ethanol elution of 1.5BV, collect 10% ethanol eluate, be evaporated to thick paste, admix 50-100 order silica gel, volatilize, add 50-100 order silicagel column (amount ratio is 1: 5), with 3: 1 wash-outs of ethyl acetate/methanol, collect object flow part, concentrating under reduced pressure, drying, dry thing 95% ethyl alcohol recrystallization, filter, drying gets Catalpol sterling 504.1kg, records to contain Catalpol 92.8%.
The TLC method is collected Catalpol object flow part with embodiment 1.
Embodiment 4
Get the stem of Radix Codonopsis lanceolatae meal, 50.0kg adds 12 times of water gagings, heating and refluxing extraction 2 times, each 1 hour, united extraction liquid was evaporated to relative density 1.13 (50 ℃), added 96% ethanol in 1: 3.5 by volume, standing over night, supernatant liquor is evaporated to relative density 1.07 (50 ℃), concentrated solution lets cool, and adds XAD-16 macroporous resin column (amount ratio 1: 4, blade diameter length ratio are 1: 15), use first the 2.5BV water elution, use again 6.5% ethanol elution of 2.0BV, collect 6.5% ethanol eluate, be evaporated to thick paste, admix 50-100 order silica gel, volatilize, add 100-200 order silicagel column (amount ratio is 1: 7), with 3.5: 1 wash-outs of ethyl acetate/methanol, collect object flow part, concentrating under reduced pressure, drying, dry thing 88% ethyl alcohol recrystallization, filter, drying gets Catalpol sterling 466.7g, records to contain Catalpol 95.0%.
The TLC method is collected Catalpol object flow part with embodiment 1.
Claims (5)
1. method of extracting Catalpol from stem of Radix Codonopsis lanceolatae is characterized in that:
(1) with stem of Radix Codonopsis lanceolatae, the water heating and refluxing extraction, the extracting solution concentrating under reduced pressure gets concentrated solution A;
(2) in concentrated solution A, add 95% ethanol, standing over night, the supernatant liquor concentrating under reduced pressure gets concentrated solution B;
(3) with the upper XAD-16 macroporous resin column of concentrated solution B, wash with water first, use again ethanol elution, collect ethanol eluate, be evaporated to thick paste;
(4) thick paste is admixed silica gel, volatilize, add silicagel column, with 4: 1 wash-outs of ethyl acetate/methanol, collect object flow part, concentrating under reduced pressure, drying;
(5) dry thing recrystallization filters, and drying gets the Catalpol sterling.
2. the method for extracting Catalpol from stem of Radix Codonopsis lanceolatae as claimed in claim 1 is characterized in that:
(1) with after the stem of Radix Codonopsis lanceolatae pulverizing, water heating and refluxing extraction 2 times, each 1 hour, united extraction liquid was evaporated to relative density (1.13-1.16) (50 ℃), gets concentrated solution A;
(2) by volume (1: 3～5) add 90～100% ethanol in concentrated solution A, standing over night, and supernatant liquor is evaporated to relative density (1.05～1.13) (50 ℃), lets cool, and gets concentrated solution B;
(3) with the upper XAD-16 macroporous resin column (amount ratio 1: 4 of concentrated solution B, blade diameter length ratio is 1: 5～1: 15), use first (1～2.5) BV water elution, use again 3～10% ethanol elutions of (1.5～3) BV, collect 3～10% ethanol eluates, be evaporated to thick paste;
(4) thick paste is admixed 50～200 order silica gel, volatilized, add (50～200) order silicagel column (amount ratio is 1: 5～1: 20), with ethyl acetate/methanol (3: 1～5: 1) wash-out, collect object flow part, concentrating under reduced pressure, drying;
(5) dry thing filters with (80～95%) ethyl alcohol recrystallization, and drying gets the Catalpol sterling.
3. the method for extracting Catalpol from stem of Radix Codonopsis lanceolatae as claimed in claim 1 is characterized in that:
(1) with after the stem of Radix Codonopsis lanceolatae pulverizing, water heating and refluxing extraction 2 times, each 1 hour, united extraction liquid was evaporated to relative density 1.14 (50 ℃), gets concentrated solution A;
(2) in concentrated solution A, added 95% ethanol in 1: 4 by volume, standing over night, supernatant liquor is evaporated to relative density 1.08 (50 ℃), lets cool, and gets concentrated solution B;
(3) with the upper XAD-16 macroporous resin column (amount ratio 1: 4, blade diameter length ratio are 1: 10) of concentrated solution B, use first the 2BV water elution, use again 6% ethanol elution of 2.2BV, collect 6% ethanol eluate, be evaporated to thick paste;
(4) thick paste is admixed 50-100 order silica gel, volatilized, add 100-200 order silicagel column (amount ratio is 1: 15), with 4: 1 wash-outs of ethyl acetate/methanol, collect object flow part, concentrating under reduced pressure, drying;
(5) dry thing 85% ethyl alcohol recrystallization filters, and drying gets the Catalpol sterling.
4. such as the method for from stem of Radix Codonopsis lanceolatae, extracting Catalpol of claim 1 or 2 or 3, it is characterized in that in the step (1), add the water of 8-12 times of volume of stem of Radix Codonopsis lanceolatae weight.
5. such as the method for from stem of Radix Codonopsis lanceolatae, extracting Catalpol of claim 1 or 2 or 3, it is characterized in that adopting the TLC method to collect object flow part, the thin-layer chromatography condition is: developping agent is chloroform: methyl alcohol: water 14: 6: 1, developer are the aubepine developer, and Heating temperature is 105 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101848071A CN102863489A (en) | 2011-07-04 | 2011-07-04 | Method for extracting catalpol from rehmannia stem |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101848071A CN102863489A (en) | 2011-07-04 | 2011-07-04 | Method for extracting catalpol from rehmannia stem |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102863489A true CN102863489A (en) | 2013-01-09 |
Family
ID=47442646
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011101848071A Pending CN102863489A (en) | 2011-07-04 | 2011-07-04 | Method for extracting catalpol from rehmannia stem |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102863489A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106220695A (en) * | 2016-07-21 | 2016-12-14 | 西安岳达生物科技股份有限公司 | A kind of industrial production process of catalpol |
| CN109651461A (en) * | 2019-01-14 | 2019-04-19 | 武汉轻工大学 | One kind preparing rehmannioside, Catalpol, stachyose and arginic method simultaneously from glutinous rehmannia |
| CN113480581A (en) * | 2021-07-21 | 2021-10-08 | 湖南朗林生物资源股份有限公司 | Method for extracting iridoid glycoside from rehmannia |
| CN115919949A (en) * | 2022-12-09 | 2023-04-07 | 河南省纳普生物技术有限公司 | Rehmannia functional factor extract and application thereof in preparation of anti-oxidation and/or hypoglycemic drugs |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1715285A (en) * | 2004-07-02 | 2006-01-04 | 罗何生 | Process for extracting glutinous rehmannic stem and leaf total heteroside extract |
| WO2006129964A1 (en) * | 2005-05-30 | 2006-12-07 | Korea Research Institute Of Bioscience And Biotechnology | Pharmaceutical composition comprising an extract of pseudolysimachion longifolium and the catalpol derivatives isolated therefrom having antiinflammatory, antiallergic and antiasthmatic activity |
| CN101003551A (en) * | 2007-01-16 | 2007-07-25 | 广东太阳神集团有限公司 | Method for producing stabhyose, and method for producing stabhyose and catalpol by using rehmannia root |
| CN101220063A (en) * | 2007-12-29 | 2008-07-16 | 大连理工大学 | Novel method for preparing catalpol medicament composition containing the same and uses thereof |
| CN101265282A (en) * | 2008-05-05 | 2008-09-17 | 山东大学 | Method for separating catalpol from fresh rehmanniae root |
| CN101817855A (en) * | 2009-12-23 | 2010-09-01 | 南京泽朗医药科技有限公司 | Method for preparing catalpol and polysaccharide of rehmannia glutinosa libosch from fresh rehmannia glutinosa libosch |
| CN102058712A (en) * | 2009-11-13 | 2011-05-18 | 上海玉森新药开发有限公司 | Rehmannia stem and leaf extract and preparation method and application thereof |
-
2011
- 2011-07-04 CN CN2011101848071A patent/CN102863489A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1715285A (en) * | 2004-07-02 | 2006-01-04 | 罗何生 | Process for extracting glutinous rehmannic stem and leaf total heteroside extract |
| WO2006129964A1 (en) * | 2005-05-30 | 2006-12-07 | Korea Research Institute Of Bioscience And Biotechnology | Pharmaceutical composition comprising an extract of pseudolysimachion longifolium and the catalpol derivatives isolated therefrom having antiinflammatory, antiallergic and antiasthmatic activity |
| CN101003551A (en) * | 2007-01-16 | 2007-07-25 | 广东太阳神集团有限公司 | Method for producing stabhyose, and method for producing stabhyose and catalpol by using rehmannia root |
| CN101220063A (en) * | 2007-12-29 | 2008-07-16 | 大连理工大学 | Novel method for preparing catalpol medicament composition containing the same and uses thereof |
| CN101265282A (en) * | 2008-05-05 | 2008-09-17 | 山东大学 | Method for separating catalpol from fresh rehmanniae root |
| CN102058712A (en) * | 2009-11-13 | 2011-05-18 | 上海玉森新药开发有限公司 | Rehmannia stem and leaf extract and preparation method and application thereof |
| CN101817855A (en) * | 2009-12-23 | 2010-09-01 | 南京泽朗医药科技有限公司 | Method for preparing catalpol and polysaccharide of rehmannia glutinosa libosch from fresh rehmannia glutinosa libosch |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106220695A (en) * | 2016-07-21 | 2016-12-14 | 西安岳达生物科技股份有限公司 | A kind of industrial production process of catalpol |
| CN109651461A (en) * | 2019-01-14 | 2019-04-19 | 武汉轻工大学 | One kind preparing rehmannioside, Catalpol, stachyose and arginic method simultaneously from glutinous rehmannia |
| CN109651461B (en) * | 2019-01-14 | 2022-02-18 | 武汉轻工大学 | Method for simultaneously preparing digitonin, catalpol, stachyose and arginine from rehmannia |
| CN113480581A (en) * | 2021-07-21 | 2021-10-08 | 湖南朗林生物资源股份有限公司 | Method for extracting iridoid glycoside from rehmannia |
| CN113480581B (en) * | 2021-07-21 | 2022-05-24 | 湖南朗林生物资源股份有限公司 | Method for extracting iridoid glycoside from rehmannia |
| CN115919949A (en) * | 2022-12-09 | 2023-04-07 | 河南省纳普生物技术有限公司 | Rehmannia functional factor extract and application thereof in preparation of anti-oxidation and/or hypoglycemic drugs |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100503626C (en) | Producing raw material containing benzyl carbinol glycosides from Cistanche deserticola by using membrane separation technique and preparation method thereof | |
| CN102451235A (en) | Preparation method of olive leaf extract | |
| CN100484948C (en) | Method for separating derivative of vitexin | |
| CN105294628A (en) | Method for preparing flavonoid component by separating wild chrysanthemum flower | |
| CN102863489A (en) | Method for extracting catalpol from rehmannia stem | |
| CN101348474A (en) | Method for preparing salvianolic acid B and tanshinol from Salvia miltiorrhiza stem | |
| CN102078341B (en) | High-purity ginkgo flavone and composition thereof | |
| CN104211690B (en) | Method for separating and purifying mangiferin from aquilaria sinensis leaves | |
| CN101234147B (en) | Method of preparing total flavones of tropaeolum for injections | |
| CN102924467B (en) | Preparation method for extracting and purifying bruceine D form brucea javanica | |
| CN102731592A (en) | Method for extracting cleupin and amentoflavone from olive leaf | |
| CN101757058B (en) | General flavone extract of hollyhock flower, preparation thereof and application | |
| CN105367424B (en) | The method that high-purity chlorogenic acid is prepared with Eupatorium adenophorum | |
| CN104610401A (en) | Method for simultaneously extracting baicalin, baicalein and wogonin from scutellaria baicalensis | |
| CN105175426B (en) | A kind of method of the extraction purification Bergenin from treebine stem | |
| CN102040500B (en) | Method for extracting and separating xanthohumol and flavone compounds | |
| CN101703554B (en) | Preparation and use of semen cuscutae flavonoids | |
| CN103232515A (en) | Cyclocarya paliurus glucoside I preparation method | |
| CN103172601A (en) | Method for separating and extracting salvianolic acid B | |
| CN105646464A (en) | Method for extracting high-purity mangiferin from bombax ceiba leaves | |
| CN106045960A (en) | Method of extracting diphenyl heptane substance from galangal | |
| CN102250183B (en) | Method for preparing high-purity ginsenoside Re by using ginseng flower buds as raw materials | |
| CN101991628B (en) | Process for preparing non-toxic extractive from asarum heterotropoides | |
| CN105273015A (en) | Preparation method of high-purity paeoniflorin and albiflorin | |
| CN111620917A (en) | Isovitexin-2' -O-beta-D-glucopyranoside, and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20130109 |