CN103788152A - Method for preparing geniposide in eucommia leaf - Google Patents
Method for preparing geniposide in eucommia leaf Download PDFInfo
- Publication number
- CN103788152A CN103788152A CN201210425767.XA CN201210425767A CN103788152A CN 103788152 A CN103788152 A CN 103788152A CN 201210425767 A CN201210425767 A CN 201210425767A CN 103788152 A CN103788152 A CN 103788152A
- Authority
- CN
- China
- Prior art keywords
- geniposide
- membrane
- folium eucommiae
- carrying
- resin
- 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
Landscapes
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The invention discloses a method for preparing geniposide in eucommia leaf. The method comprises the following steps of crushing eucommia leaf, carrying out cellulase-assistant middle temperature-water extraction, carrying out routine filtration, carrying out ultrafilter membrane impurity-removal, carrying out nanofiltration condensation, carrying out macroporous resin-based separation purification, carrying out condensation and carrying out drying to obtain geniposide powder. The method utilizes cellulase-assistant middle temperature-water extraction of geniposide in eucommia leaf, has an extraction rate of 95%, a low water extraction temperature and short extraction time, utilizes an ultrafilter membrane to remove impurities and separate other side products in the extract, has simple membrane processes and realizes long-term membrane flux stabilization, easy membrane cleaning, a long service life and industrialization. Through the nanofiltration membrane, the extract subjected to impurity removal is concentrate d so that follow-up technical load is reduced and a resin service life is prolonged. Through the method, a nanofiltrated liquid has a COD value <=100 and can be reused in production and basically, waste water is not produced. Through the macroporous adsorption resin, geniposide can be effectively purified. The powder produced by the method has geniposide purity greater than 80% and an extraction rate more than 1.2%.
Description
Technical field
The present invention relates to a kind of method of producing Geniposide 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 Geniposide.
Background technology
Geniposide is a kind of iridoid glucoside, soluble in water.Geniposide can be hydrolyzed to genipin by beta-glucosidase.Modern study shows, Geniposide during Digestive tract, cardiovascular system are unified general nervous system disorders all have significant curative effect, in addition, Geniposide also has the effect of certain anti-inflammatory and treatment soft tissue injury.Geniposide, except medicinal, is also widely used in other field, as can be used as plant promoter, biological detection agent etc., is a kind of important biologically active substance.Be widely used in medical treatment, field of health care products.Geniposide is mainly present in the natural phant such as the bark of eucommia, cape jasmine.The bark of eucommia is the distinctive economical seeds of China, distributed areas are large, aboundresources, in Folium Eucommiae, the content of Geniposide is 1～3%, it is the desirable feedstock of extracting Geniposide, in domestic existing extraction process scheme, exist that extraction yield is not high, product purity is low, energy consumption greatly, in a large number with an organic solvent, the problem such as wastewater flow rate is large, seriously restricted the development of bark of eucommia industry.
Chinese patent: CN101260131A " extracts the method for iridoid active site and monomer " and discloses a kind of technique of preparing Geniposide from the bark of eucommia (skin, leaf or seed) from the bark of eucommia, this technique comprises the steps such as high temperature extraction, organic solvent extraction, preparative chromatography separation, it is high that this scheme exists high temperature extraction energy consumption, when extraction, consumption of organic solvent is large, adopt preparative chromatography to separate and be difficult to realize scale operation, and the problem such as cost is higher.
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 Geniposide in Folium Eucommiae, the method is in the Folium Eucommiae powder after pulverizing, adopt the Geniposide adding in cellulase and middle warm water extraction Folium Eucommiae, by two-stage membrane separation technique binding resin absorb-elute technique, the Geniposide extracting is carried out to separation and purification again, after collecting ethanol eluate concentrating under reduced pressure, vacuum-drying, obtain product Geniposide, efficiently solve the problem that in original Geniposide production, extraction yield 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 Geniposide 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 Geniposide extracting is carried out to separation and purification, after collection ethanol eluate concentrating under reduced pressure, vacuum-drying, obtain product Geniposide powder.
The present invention produces the method steps of Geniposide in Folium Eucommiae and comprises:
1, the pulverizing of raw material leaf: dry Folium Eucommiae, its water content≤14%, crosses 80 mesh sieves after pulverizing by ordinary 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 ℃～60 ℃, 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: mass ratio=1 of water: 12, extract 2 times, each 60～90min;
3, filter: merge after extracted twice liquid, remove the impurity such as suspended substance by conventional filtration method;
4, ultra-filtration membrane removal of impurities: 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 Geniposide molecular weight is can to see through completely about 400Dal, the operational condition of this film is: P=0.2～0.6Mpa, T=30～50 ℃, PH=4～5, Q=60～70L/min;
5, nanofiltration is concentrated: the present invention adopts the nanofiltration membrane that interception molecular weight is 200～400Dal to concentrate one-level membrane filtration liquid, and can be partially desalted.This grade of membrane concentration multiple can reach more than 15 times, and inorganic ion clearance can reach 60%.The operational condition of this film is: P=1.0～1.5Mpa, T=30～60 ℃, PH=4～5, Q=20L/min.
6, the separation and purification of macroporous resin: nanofiltration membrane concentrated solution carries out absorb-elute by macroporous resin, first wash away impurity with the pure water of 2 times of resin Du volumes, then be 70% ethanol elution with the concentration of volume percent of 2.5 times of resin column volumes, collect ethanol eluate.
7, concentrated and dry: the ethanol eluate of collection can be obtained to Geniposide powder after by conventional concentrating under reduced pressure and vacuum-drying.
In above-mentioned steps 2, the extraction yield of Folium Eucommiae Geniposide can reach 95%.
In above-mentioned steps 4,5, two-stage membrane concentration all can concentrate material more than 10 times, and nanofiltration membrane ratio of desalinization can reach 60%, and its liquor C OD value can be reduced to below 100.
In above-mentioned steps 6, macroporous resin is D301R, H103 type resin.
Concentrating under reduced pressure in above-mentioned steps 7 and vacuum-drying temperature be not all higher than 60 ℃.
The present invention has following beneficial effect:
1, the Geniposide in warm water extraction Folium Eucommiae in enzyme process, adding of cellulase contributes to break leaf wall, the Geniposide in release cells, extraction yield can reach 95%, and water extraction temperature is lower, extraction time shortening, energy efficient.
2, adopt ultra-filtration 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 nanofiltration membrane after to removal of impurities to concentrate, ratio of desalinization can reach 60%, can alleviate the load of subsequent technique, extends work-ing 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 purifying Geniposide of macroporous adsorbent resin, the selected resin of this technique is polar macroporous adsorption resin, its, good separating effect large to Geniposide adsorptive capacity, only concentrate wash-out Fractional Collections with a small amount of solvent, just can make higher degree Geniposide.In the powder making through this technique, Geniposide content is greater than 80%, and extraction yield is greater than 1.2%.
Accompanying drawing explanation
Fig. 1 is technical process route schematic diagram of the present invention.
Embodiment
Example 1, referring to Figure of description 1, get dry Folium Eucommiae 10Kg, pulverize after cross 80 mesh sieves, add 120Kg water, regulate 55 ℃ of temperature, constant temperature also regulates pH value to 4.5, then adds 10g cellulase, extract with this understanding 60min, filter, filter residue extracts for the second time by aforementioned extraction conditions again, merges twice filtrate, conventional filtration, Geniposide extraction yield is 95.8%; Be P=0.3Mpa in operational condition, T=45 ℃, PH=4.5, Q=70L/min filtrate is crossed 0.03 μ m ultra-filtration membrane, and extracting solution has concentrated 11.2 times under this condition, and this ultra-filtration membrane average flux is 226.3L/m
2h; At operational condition P=1.5Mpa, T=50 ℃, PH=4.5, Q=20L/min is by ultrafiltrate after 200 molecular weight nanofiltration membrane, and ultrafiltrate has concentrated 16.6 times under this condition, and inorganic ion clearance is 63%, and this nanofiltration membrane average flux is 18.7L/m
2h, nanofiltration liquor C OD is 94; Nanofiltration concentrated solution is passed through to D301R resin purification, first use 2 times of resin column volume pure water wash-out impurity, then be 70% ethanol elution with the concentration of volume percent of 2.5 times of resin Du volumes, after collecting ethanol eluate concentrating under reduced pressure, vacuum-drying (the dry temperature of its concentrating under reduced pressure and vacuum is not all higher than 60 ℃), can obtain Geniposide powder, detecting Geniposide purity through HPLC is 82.5%, and yield is 1.35%.
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 10g cellulase, extract with this understanding 80min, filter, filter residue extracts for the second time by aforementioned extraction conditions again, merges twice filtrate, conventional filtration, Geniposide extraction yield is 95.3%; Be P=0.3Mpa in operational condition, T=45 ℃, PH=4.5, Q=70L/min filtrate is crossed 0.02 μ m ultra-filtration membrane, and extracting solution has concentrated 12.8 times under this condition, and this ultra-filtration membrane average flux is 221.3L/m
2h; At operational condition P=1.5Mpa, T=50 ℃, PH=4.5, Q=20L/min is concentrated after 400 molecular weight nanofiltration membrane by ultrafiltrate, ultra-filtration membrane filtrate has concentrated 15.2 times under this condition, and inorganic ion clearance is 60%, and this nanofiltration membrane average flux is 19.5L/m
2h, nanofiltration liquor C OD is 91; Nanofiltration concentrated solution is passed through to H103 resin purification, first use 2 times of resin column volume pure water wash-out impurity, then be 70% ethanol elution with the concentration of volume percent of 2.5 times of resin Du volumes, after collecting ethanol eluate concentrating under reduced pressure, vacuum-drying (the dry temperature of its concentrating under reduced pressure and vacuum is not all higher than 60 ℃), can obtain Geniposide powder, detecting Geniposide purity through HPLC is 83.6%, and yield is 1.21%.
Claims (3)
1. produce the method for Geniposide in Folium Eucommiae for one kind, comprise the Geniposide in waste Folium Eucommiae take Folium Eucommiae powder, it is characterized in that: in the Folium Eucommiae powder of pulverizing, add the Geniposide in cellulase and middle warm water extraction Folium Eucommiae, by two-stage membrane separation technique binding resin absorb-elute technique, the Geniposide extracting is carried out to separation and purification, collection ethanol eluate concentrating under reduced pressure, vacuum-drying obtain product Geniposide powder.
2. a kind of method of producing Geniposide in Folium Eucommiae according to claim 1, is characterized in that: the method for Geniposide 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 ordinary 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 ℃-60 ℃, 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 of 0.002 kilogram: mass ratio=1 of water: 12, extract 2 times, each 60-90min;
(3), filter: merge after extracted twice liquid, remove the impurity such as suspended substance by conventional filtration method;
(4), ultra-filtration membrane removal of impurities: 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 ultra-filtration membrane, and Geniposide molecular weight can see through completely in 400Dal left and right, the operational condition of this film is: P=0.2-0.6Mpa, T=30-50 ℃, PH=4-5, Q=60-70L/min;
(5), nanofiltration is concentrated: adopt the nanofiltration membrane that interception molecular weight is 200-400Dal to concentrate one-level membrane filtration liquid, partially desalted, this grade of membrane concentration multiple can reach more than 15 times, and inorganic ion clearance can reach 60%; The operational condition of this film is: P=1.0-1.5Mpa, T=30-60 ℃, PH=4-5, Q=20L/min;
(6), the separation and purification of macroporous resin: nanofiltration membrane concentrated solution carries out absorb-elute by macroporous resin, first wash away impurity with the pure water of 2 times of resin Du volumes, then be 70% ethanol elution with the concentration of volume percent of 2.5 times of resin Du volumes, collect ethanol eluate;
(7), concentrated and dry: the ethanol eluate of collection can be obtained to Geniposide powder after by conventional concentrating under reduced pressure and vacuum-drying.
3. according to claim 1 and a kind of method of producing Geniposide 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 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210425767.XA CN103788152A (en) | 2012-10-26 | 2012-10-26 | Method for preparing geniposide in eucommia leaf |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210425767.XA CN103788152A (en) | 2012-10-26 | 2012-10-26 | Method for preparing geniposide in eucommia leaf |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103788152A true CN103788152A (en) | 2014-05-14 |
Family
ID=50664245
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210425767.XA Pending CN103788152A (en) | 2012-10-26 | 2012-10-26 | Method for preparing geniposide in eucommia leaf |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103788152A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105037463A (en) * | 2015-08-31 | 2015-11-11 | 桂林三宝生物科技有限公司 | Method for extracting geniposide from jasmine |
| CN105063107A (en) * | 2015-08-31 | 2015-11-18 | 桂林茗兴生物科技有限公司 | Method for preparing crocetin through gardenias |
| CN105063119A (en) * | 2015-08-31 | 2015-11-18 | 桂林茗兴生物科技有限公司 | Method for extracting genipin from gardenias |
| CN105130946A (en) * | 2015-08-31 | 2015-12-09 | 桂林茗兴生物科技有限公司 | Method for extracting genipin from eucommia folium |
| CN105131061A (en) * | 2015-08-31 | 2015-12-09 | 桂林茗兴生物科技有限公司 | Method for extracting geniposide from folium cortex eucommiae |
| CN105131059A (en) * | 2015-08-31 | 2015-12-09 | 桂林茗兴生物科技有限公司 | Method for extracting geniposide from jasmine |
| CN113768945A (en) * | 2021-08-12 | 2021-12-10 | 宁夏医科大学 | Application of geniposide in preparation of medicine for treating oligospermia |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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
- 2012-10-26 CN CN201210425767.XA patent/CN103788152A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 (2)
| Title |
|---|
| 刘慧: "杜仲中活性成分的提取分离纯化技术研究", 《湖南农业大学硕士学位论文（2011年）》 * |
| 刘慧: "活性炭联合大孔树脂分离纯化京尼平苷的研究", 《时珍国医国药》 * |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105037463A (en) * | 2015-08-31 | 2015-11-11 | 桂林三宝生物科技有限公司 | Method for extracting geniposide from jasmine |
| CN105063107A (en) * | 2015-08-31 | 2015-11-18 | 桂林茗兴生物科技有限公司 | Method for preparing crocetin through gardenias |
| CN105063119A (en) * | 2015-08-31 | 2015-11-18 | 桂林茗兴生物科技有限公司 | Method for extracting genipin from gardenias |
| CN105130946A (en) * | 2015-08-31 | 2015-12-09 | 桂林茗兴生物科技有限公司 | Method for extracting genipin from eucommia folium |
| CN105131061A (en) * | 2015-08-31 | 2015-12-09 | 桂林茗兴生物科技有限公司 | Method for extracting geniposide from folium cortex eucommiae |
| CN105131059A (en) * | 2015-08-31 | 2015-12-09 | 桂林茗兴生物科技有限公司 | Method for extracting geniposide from jasmine |
| CN105037463B (en) * | 2015-08-31 | 2018-01-30 | 桂林三宝生物科技有限公司 | A kind of method that geniposide is extracted from cape jasmine |
| CN105063119B (en) * | 2015-08-31 | 2018-11-30 | 广西红瑶药业有限公司 | The method of Geniposide is extracted from cape jasmine |
| CN105063107B (en) * | 2015-08-31 | 2019-03-05 | 桂林三叶生物科技有限责任公司 | A method of preparing bayer acid from cape jasmine |
| CN113768945A (en) * | 2021-08-12 | 2021-12-10 | 宁夏医科大学 | Application of geniposide in preparation of medicine for treating oligospermia |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102040519B (en) | Method for preparing chlorogenic acid in Eucommia ulmoides leaves | |
| CN106008645B (en) | A kind of method that momordica grosvenori glycoside V is extracted from Momordica grosvenori | |
| CN103788152A (en) | Method for preparing geniposide in eucommia leaf | |
| CN100457765C (en) | Method for producing stabhyose, and method for producing stabhyose and catalpol by using rehmannia root | |
| CN102250195B (en) | Method for producing xanthoceraside | |
| CN101095724B (en) | Technics for extracting lotus leaf flavone | |
| CN101336949B (en) | Method for extracting polysaccharide and flavone from Gynura divaricata | |
| CN101935278A (en) | Method for extracting, separating and purifying chlorogenic acid through folium cortex eucommiae | |
| CN102234245A (en) | Method for preparing sulforaphane | |
| CN102060856B (en) | Method for extracting tabersonine from voacanga seeds | |
| CN103772457B (en) | Method for preparing geniposidic acid in eucommia leaf | |
| CN101503357A (en) | Method for extracting chlorogenic acid in honeysuckle | |
| CN103860626B (en) | Method for preparing total flavonoids in eucommia ulmoides leaves | |
| CN104119229A (en) | Technology for producing pure chlorogenic acid | |
| CN107698691B (en) | System and method for separating and purifying flavone and polysaccharide from oldenlandia diffusa | |
| CN107721909B (en) | Method and system for continuously extracting DNJ, flavone and polysaccharide from Moraceae plant | |
| JP6768970B2 (en) | How to prepare rubusoside | |
| CN103864867B (en) | Method for extracting aucubin from folium cortex eucommiae | |
| CN102391337A (en) | Method for extracting rhoifolin from turpinia formosana leaves | |
| CN102391117B (en) | Method for preparing chlorogenic acid from eucommia leaves | |
| CN104292281A (en) | Method for preparing high-purity rutin by using integrated technique | |
| CN102274386A (en) | Method for extracting total isoflavones from Allium mongolicum Regel | |
| CN111116768A (en) | Method for recovering baicalein from baicalin production waste liquid | |
| CN102311379A (en) | Method for preparing 1-deoxynojirimycin by membrane separation technology | |
| CN108997359A (en) | A method of chlorophyll is extracted from stevioside production waste residue |
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: 20140514 |