CN103860626A - Method for preparing total flavonoids in eucommia ulmoides leaves - Google Patents
Method for preparing total flavonoids in eucommia ulmoides leaves Download PDFInfo
- Publication number
- CN103860626A CN103860626A CN201210541271.9A CN201210541271A CN103860626A CN 103860626 A CN103860626 A CN 103860626A CN 201210541271 A CN201210541271 A CN 201210541271A CN 103860626 A CN103860626 A CN 103860626A
- Authority
- CN
- China
- Prior art keywords
- total flavones
- membrane
- folium eucommiae
- extraction
- filtration
- 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
Links
Images
Abstract
The present invention discloses a method for preparing total flavonoids in eucommia ulmoides leaves. The method comprises steps of eucommia ulmoides leaf crushing, cellulase assisted medium-temperature water extraction, conventional filtration, impurity removing with ultra-filtration membrane, nano-filtration concentration, separation and purification with macroporous resin, concentration and drying to prepare the total flavonoid powder. According to the present invention, the method adopts the cellulase assisted medium-temperature water extraction to extract the total flavonoids in the eucommia ulmoides leaves, wherein the extraction rate can achieve 95%, the water extraction temperature is low, and the extraction time is shortened; the ultra-filtration membrane is adopted to remove impurities from the extraction solution and separate other byproducts, wherein the membrane process is simple, the membrane flux can be stable for a long time, and characteristics of easy cleaning, long service life and easy industrialization achievement are provided; the nano-filtration membrane is adopted to concentrate the impurity-removed extraction solution so as to reduce the load of the follow-up process and prolong the service life of the resin; the COD value of the nano-filtration filtrate is less than or equal to 100, such that the nano-filtration filtrate can be reused for the production process, and almost no wastewater is discharged; and the macroporous resin is adopted so as to effectively purify the total flavonoids, wherein the purity of the total flavonoids in the prepared powder is more than 70%, and the extraction rate is more than 4%.
Description
Technical field
The present invention relates to a kind of method of producing total flavones in Folium Eucommiae, particularly relate to a kind of method that adopts warm water extraction in enzyme process, membrane separation technique binding resin technique to prepare total flavones.
Background technology
Total flavones is a kind of important bioactive substance, has the multiple pharmacological effect such as hepatic cholagogic, resisting hypertension, neuroprotective cell, antiinflammatory, antitumor, antithrombotic, inhibition osteoporosis, is widely used in medical treatment, field of health care products.Total flavones is mainly present in the natural plants such as the Cortex Eucommiae, Fructus Gardeniae.The Cortex Eucommiae is the distinctive economical seeds of China, distributed areas are large, aboundresources, in Folium Eucommiae, the content of total flavones is 2～5%, it is the desirable feedstock of extracting total flavones, in domestic existing extraction process scheme, exist that extraction ratio is not high, product purity is low, energy resource consumption greatly, in a large number with an organic solvent, the problem such as wastewater flow rate is large, seriously restricted the development of Cortex Eucommiae industry.
Chinese patent: CN 200610123973.x " prepares the method for high-purity chlorogenic acid and total flavones from Folium Eucommiae ", CN 201010588425.0 " a kind of method of flavone high efficiency extraction Cortex Eucommiae ", CN " a kind of total flavones, chlorogenic acid extraction process prepared from Chinese medicine Folium Eucommiae ", the technique of preparing total flavones from Folium Eucommiae or skin is disclosed respectively, this several technique can be summarized as: after raw material pulverizing, with certain density alcoholic solution extraction, then with purification such as macroporous adsorbent resins.The method adopts ethanol for extracting solvent, have larger potential safety hazard, and expense is higher, after extracting in addition, directly with absorption with macroporous adsorbent resin, because impurity component in extracting solution is more, is unfavorable for purification.
Summary of the invention
In order to overcome above-mentioned problems of the prior art and shortcoming, the invention provides a kind of method of producing total flavones in Folium Eucommiae, the method is in the Folium Eucommiae powder after pulverizing, adopt the total flavones adding in cellulase and middle warm water extraction Folium Eucommiae, by two-stage membrane separation technique binding resin absorb-elute technique, the total flavones extracting is carried out to separation and purification again, after collecting ethanol elution concentrating under reduced pressure, vacuum drying, obtain product total flavones, efficiently solve the problem that in original total flavones production, extraction ratio is low, wastewater flow rate is large and product purity is low.
The technical solution adopted for the present invention to solve the technical problems is: in the Folium Eucommiae powder after pulverizing, adopt the total flavones adding in a certain amount of cellulase and middle warm water extraction Folium Eucommiae, by two-stage membrane separation technique binding resin absorb-elute technique, the total flavones extracting is carried out to separation and purification, after collection ethanol elution concentrating under reduced pressure, vacuum drying, obtain product total flavones powder.
The present invention produces the method for total flavones in Folium Eucommiae and comprises the following steps.
1, the pulverizing of raw material leaf: dry Folium Eucommiae, its water content≤14%, crosses 80 mesh sieves after pulverizing by conventional method.
2, the auxiliary middle warm water extraction of enzyme process: will add a certain amount of water in the raw material leaf of pulverizing, regulating pH is 4.5, and constant temperature to 50 DEG C～60 DEG C, add appropriate cellulase to extract under the following conditions: cellulase addition is concentration of substrate 0.2%, every kg feed material leaf need consume cellulase, the Folium Eucommiae of 0.002 kilogram: the mass ratio=1:12 of water, extract 2 times, each 60～80min.
3, filter: merge after extracted twice liquid, remove the impurity such as float by conventional filtration method.
4, ultrafilter membrane remove impurity: it is the ultrafiltration membrane treatment Folium Eucommiae water extraction liquid of 0.02～0.0.06 μ m that the present invention adopts pore size filter, this film can be held back the impurity such as most macro-molecular protein and polysaccharide, and total flavones molecular weight is can to see through completely about 400Dal, the operating condition of this film is: P=0.2～0.6Mpa, T=30～50 DEG C, PH=4～5, Q=60～70L/min.
5, nanofiltration is concentrated: the present invention adopts the NF membrane that interception molecular weight is 200～400Dal to concentrate one-level membrane filtration liquid, and can be partially desalted.This grade of membrance concentration multiple can reach more than 15 times, and inorganic ion clearance can reach 60%.The operating condition of this film is: P=1.0～1.5Mpa, T=30～60 DEG C, PH=4～5, Q=20 L/min.
6, the separation and purification of macroporous resin: NF membrane concentrated solution carries out absorb-elute by macroporous resin, first washes away impurity with the pure water of 2 times of resin column volumes, is then 65% ethanol elution with the concentration of volume percent of 2.5 times of resin column volumes, collects ethanol elution.
7, concentrated and dry: the ethanol elution of collection can be obtained to total flavones powder after by conventional concentrating under reduced pressure and vacuum drying.
In above-mentioned steps 2, the extraction ratio of Flavonoids from Eucommia ulmoides Leaves can reach 95%.
In above-mentioned steps 4,5, two-stage membrance concentration all can concentrate material more than 10 times, and NF membrane salt rejection rate can reach 60%, and its liquor C OD value can be reduced to below 100.
In above-mentioned steps 6, macroporous resin is ADS-17 type resin.
Concentrating under reduced pressure in above-mentioned steps 7 and vacuum drying temperature be not all higher than 60 DEG C.
the present invention has following beneficial effect.
1, the total flavones in warm water extraction Folium Eucommiae in enzyme process, adding of cellulase contributes to break leaf wall, the total flavones in release cells, extraction ratio can reach 95%, and water extraction temperature is lower, extraction time shortening, energy efficient.
2, adopt ultrafilter membrane to carry out separation and purification to extracting solution, can effectively separate other by-products, membrane operations process is simple, and membrane flux can be stablized for a long time, is easy to cleaning, long service life, is easy to realize industrialization.
3, adopt the extracting solution of NF membrane after to remove impurity to concentrate, salt rejection rate can reach 60%, can alleviate the load of subsequent technique, extends service life and the energy efficient of resin, and nanofiltration liquor C OD value≤100 can reuse production process, substantially non-wastewater discharge.
4, adopt effectively purification total flavones of macroporous adsorbent resin, the selected resin of this technique is polar macroporous adsorption resin, and its, good separating effect large to total flavones adsorbance, only concentrate eluting Fractional Collections with a small amount of solvent, just can make higher degree total flavones.In the powder making through this technique, general flavone content is greater than 70%, and extraction ratio is greater than 4%.
Brief description of the drawings
Fig. 1 is technological process route schematic diagram of the present invention.
Detailed description of the invention
Example 1, referring to Figure of description 1, get dry Folium Eucommiae 10Kg, pulverize after cross 80 mesh sieves, add 120Kg water, regulate 55 DEG C of temperature, constant temperature also regulates pH value to 4.5, then adds 20g cellulase, extract with this understanding 60min, filter, filtering residue extracts for the second time by aforementioned extraction conditions again, merges twice filtrate, conventional filtration, total flavones extraction ratio is 90.6%; Be P=0.3Mpa in operating condition, T=45 DEG C, PH=4.5, Q=70L/min filtrate is crossed 0.03 μ m ultrafilter membrane, and extracting solution has concentrated 12.1 times under this condition, and this ultrafilter membrane average flux is 222.0L/m
2h; At operating condition P=1.5Mpa, T=50 DEG C, PH=4.5, Q=20 L/min is by ultrafiltrate after 200 molecular weight NF membrane, and ultrafiltrate has concentrated 17.0 times under this condition, and inorganic ion clearance is 62%, and this NF membrane average flux is 18.4 L/m
2h, nanofiltration liquor C OD is 90; Nanofiltration concentrated solution is passed through to ADS-17 resin purification, first use 2 times of resin column volume pure water eluting impurity, then be 65% ethanol elution with the concentration of volume percent of 2.5 times of resin column volumes, after collecting ethanol elution concentrating under reduced pressure, vacuum drying (the dry temperature of its concentrating under reduced pressure and vacuum is not all higher than 60 DEG C), can obtain total flavones powder, detecting total flavones purity through HPLC is 76.3%, and yield is 4.14%.
Example 2, referring to Figure of description 1, get dry Folium Eucommiae 10Kg, pulverize after cross 80 mesh sieves, add 120Kg water, regulate temperature 50 C, constant temperature also regulates pH value to 4.5, then adds 20g cellulase, extract with this understanding 80min, filter, filtering residue extracts for the second time by aforementioned extraction conditions again, merges twice filtrate, conventional filtration, total flavones extraction ratio is 95.8%; Be P=0.3Mpa in operating condition, T=45 DEG C, PH=4.5, Q=70L/min filtrate is crossed 0.02 μ m ultrafilter membrane, and extracting solution has concentrated 12.2 times under this condition, and this ultrafilter membrane average flux is 223.3L/m
2h; At operating condition P=1.5Mpa, T=50 DEG C, PH=4.5, Q=20 L/min is concentrated after 400 molecular weight NF membrane by ultrafiltrate, and ultrafilter membrane filtrate has concentrated 15.2 times under this condition, and inorganic ion clearance is 60%, and this NF membrane average flux is 19.9 L/m
2h, nanofiltration liquor C OD is 92; Nanofiltration concentrated solution is passed through to ADS-17 resin purification, first use 2 times of resin column volume pure water eluting impurity, then be 65% ethanol elution with the concentration of volume percent of 2.5 times of resin column volumes, after collecting ethanol elution concentrating under reduced pressure, vacuum drying (the dry temperature of its concentrating under reduced pressure and vacuum is not all higher than 60 DEG C), can obtain total flavones powder, detecting total flavones purity through HPLC is 73.2%, and yield is 4.27%.
Claims (3)
1. produce the method for total flavones in Folium Eucommiae for one kind, comprise the total flavones in waste Folium Eucommiae taking Folium Eucommiae, it is characterized in that: in the Folium Eucommiae powder of pulverizing, add the total flavones in cellulase and middle warm water extraction Folium Eucommiae, by two-stage membrane separation technique binding resin absorb-elute technique, the total flavones extracting is carried out to separation and purification, collection ethanol elution concentrating under reduced pressure, vacuum drying obtain product total flavones powder.
2. a kind of method of producing total flavones in Folium Eucommiae according to claim 1, is characterized in that: the method for total flavones in Folium Eucommiae of producing comprises the following steps:
(1), the pulverizing of raw material leaf: by water content≤14% Folium Eucommiae, cross 80 mesh sieves after pulverizing by conventional method;
(2), the auxiliary middle warm water extraction of enzyme process: will add a certain amount of water in the raw material leaf of pulverizing, regulating pH is 4.5, and constant temperature to 50 DEG C-60 DEG C, add appropriate cellulase to extract under the following conditions: cellulase addition is concentration of substrate 0.2%, every kg feed material leaf need consume cellulase, the Folium Eucommiae powder water of 0.002 kilogram mass ratio=1:12, extract 2 times, each 60-80min;
(3), filter: merge after extracted twice liquid, remove the impurity such as float by conventional filtration method;
(4), ultrafilter membrane remove impurity: adopting pore size filter is the ultrafiltration membrane treatment Folium Eucommiae water extraction liquid of 0.02-0.0.06 μ m, hold back the impurity such as macro-molecular protein and polysaccharide with ultrafilter membrane, and total flavones molecular weight can see through completely in 400Dal left and right, the operating condition of this film is: P=0.2-0.6Mpa, T=30-50 DEG C, PH=4-5, Q=60-70L/min;
(5), nanofiltration is concentrated: adopt the NF membrane that interception molecular weight is 200-400Dal to concentrate one-level membrane filtration liquid, partially desalted, this grade of membrance concentration multiple can reach more than 15 times, and inorganic ion clearance can reach 60%; The operating condition of this film is: P=1.0-1.5Mpa, T=30-60 DEG C, PH=4-5, Q=20 L/min;
(6), the separation and purification of macroporous resin: NF membrane concentrated solution carries out absorb-elute by macroporous resin, first wash away impurity with the pure water of 2 times of resin column volumes, then be 65% ethanol elution with the concentration of volume percent of 2.5 times of resin column volumes, collect ethanol elution;
(7), concentrated and dry: the ethanol elution of collection can be obtained to total flavones powder after by conventional concentrating under reduced pressure and vacuum drying.
3. according to claim 1 and a kind of method of producing total flavones in Folium Eucommiae claimed in claim 2, it is characterized in that: concentrating under reduced pressure and vacuum drying temperature be not all higher than 60 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210541271.9A CN103860626B (en) | 2012-12-14 | 2012-12-14 | Method for preparing total flavonoids in eucommia ulmoides leaves |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210541271.9A CN103860626B (en) | 2012-12-14 | 2012-12-14 | Method for preparing total flavonoids in eucommia ulmoides leaves |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103860626A true CN103860626A (en) | 2014-06-18 |
| CN103860626B CN103860626B (en) | 2015-05-20 |
Family
ID=50900013
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210541271.9A Expired - Fee Related CN103860626B (en) | 2012-12-14 | 2012-12-14 | Method for preparing total flavonoids in eucommia ulmoides leaves |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103860626B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104546992A (en) * | 2015-01-30 | 2015-04-29 | 四川九章生物科技有限公司 | Folium cortex eucommiae extract as well as preparation method and application thereof |
| CN106361799A (en) * | 2016-08-31 | 2017-02-01 | 无锡正大生物股份有限公司 | Eucommia leaf extract and preparation method and application thereof |
| CN108992482A (en) * | 2018-08-27 | 2018-12-14 | 维康腾达生物科技有限公司 | A kind of preparation method of eucommia leaf extract |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1974527A (en) * | 2006-12-01 | 2007-06-06 | 广州汉方现代中药研究开发有限公司 | Process of preparing high purity chlorogenic acid and flavonid with eucommia leaf |
| CN102040519A (en) * | 2009-10-22 | 2011-05-04 | 湖北老龙洞杜仲开发有限公司 | Method for preparing chlorogenic acid in Eucommia ulmoides leaves |
-
2012
- 2012-12-14 CN CN201210541271.9A patent/CN103860626B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1974527A (en) * | 2006-12-01 | 2007-06-06 | 广州汉方现代中药研究开发有限公司 | Process of preparing high purity chlorogenic acid and flavonid with eucommia leaf |
| CN102040519A (en) * | 2009-10-22 | 2011-05-04 | 湖北老龙洞杜仲开发有限公司 | Method for preparing chlorogenic acid in Eucommia ulmoides leaves |
Non-Patent Citations (1)
| Title |
|---|
| 杨玉琼等: "杜仲叶中黄酮的提取、检测方法研究进展", 《中药材》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104546992A (en) * | 2015-01-30 | 2015-04-29 | 四川九章生物科技有限公司 | Folium cortex eucommiae extract as well as preparation method and application thereof |
| CN106361799A (en) * | 2016-08-31 | 2017-02-01 | 无锡正大生物股份有限公司 | Eucommia leaf extract and preparation method and application thereof |
| CN108992482A (en) * | 2018-08-27 | 2018-12-14 | 维康腾达生物科技有限公司 | A kind of preparation method of eucommia leaf extract |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103860626B (en) | 2015-05-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102040519B (en) | Method for preparing chlorogenic acid in Eucommia ulmoides leaves | |
| CN100564373C (en) | From tea tree, extract the complete processing of tea-polyphenol | |
| CN100457765C (en) | Method for producing stabhyose, and method for producing stabhyose and catalpol by using rehmannia root | |
| CN101633676B (en) | Method for preparing high-purity stachyose by using plant chromatographic separation technology | |
| CN103788152A (en) | Method for preparing geniposide in eucommia leaf | |
| CN101935278A (en) | Method for extracting, separating and purifying chlorogenic acid through folium cortex eucommiae | |
| CN103204800B (en) | A kind of extracting method of 1 DNJ | |
| CN101701013A (en) | Method for extracting proanthocyanidin from pine bark by taking water as solvent | |
| CN102351926B (en) | A kind of preparation method of arctinin | |
| CN106866759A (en) | The technique that grosvenor momordica flavonoid is produced from the waste liquid of Momordica-Glycosides decolorizing resin post discharge | |
| CN103772457B (en) | Method for preparing geniposidic acid in eucommia leaf | |
| CN103860626B (en) | Method for preparing total flavonoids in eucommia ulmoides leaves | |
| CN101503357A (en) | Method for extracting chlorogenic acid in honeysuckle | |
| CN102060856B (en) | Method for extracting tabersonine from voacanga seeds | |
| CN102675910A (en) | Preparation method of high-color-value beet root red color | |
| CN102391117B (en) | Method for preparing chlorogenic acid from eucommia leaves | |
| CN106831930B (en) | A kind of extractant and extracting method for ursolic acid extraction | |
| CN103864867B (en) | Method for extracting aucubin from folium cortex eucommiae | |
| CN104292281A (en) | Method for preparing high-purity rutin by using integrated technique | |
| CN107151259B (en) | The method that solid residue after a kind of pair of citrus pectin extraction is comprehensively utilized | |
| CN102274386A (en) | Method for extracting total isoflavones from Allium mongolicum Regel | |
| CN102311379A (en) | Method for preparing 1-deoxynojirimycin by membrane separation technology | |
| CN102391337A (en) | Method for extracting rhoifolin from turpinia formosana leaves | |
| CN102772452A (en) | Method for producing ultra-low-acid ginkgo leaf extract | |
| CN101974048A (en) | Method for extracting morroniside from dogwood |
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 | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20150520 Termination date: 20171214 |