CN105617867B - A kind of method for removing heavy metal ion in asparagus saponin extract solution - Google Patents
A kind of method for removing heavy metal ion in asparagus saponin extract solution Download PDFInfo
- Publication number
- CN105617867B CN105617867B CN201610020661.XA CN201610020661A CN105617867B CN 105617867 B CN105617867 B CN 105617867B CN 201610020661 A CN201610020661 A CN 201610020661A CN 105617867 B CN105617867 B CN 105617867B
- Authority
- CN
- China
- Prior art keywords
- asparagus
- extract solution
- saponin extract
- heavy metal
- metal ion
- 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.)
- Active
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/42—Electrodialysis; Electro-osmosis ; Electro-ultrafiltration; Membrane capacitive deionization
- B01D61/44—Ion-selective electrodialysis
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/88—Liliopsida (monocotyledons)
- A61K36/899—Poaceae or Gramineae (Grass family), e.g. bamboo, corn or sugar cane
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07G—COMPOUNDS OF UNKNOWN CONSTITUTION
- C07G3/00—Glycosides
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
Abstract
The invention discloses a kind of method for removing heavy metal ion in asparagus saponin extract solution, it is characterised in that：The heavy metal ion in asparagus saponin extract solution is effectively removed using electrodialytic technique；Its process concentrates to take asparagus raw material to be extracted by organic solvent, obtains asparagus saponin extract solution, regulates and controls its concentration and reaches operation requirement, and the desalination indoor circulation for entering electrodialysis plant carries out electrodialysis, and tap water is placed by enriched chamber, and pole room places electrode solution；Control operation temperature operates 40~100V of voltage, removes heavy metal ion therein below 35 DEG C.The present invention ensure that the high yield pulp1 of product while heavy metal ion in effectively eliminating asparagus saponin extract solution, be a kind of more efficient, environmentally protective method.
Description
Technical field
The present invention relates to a kind of new method for removing heavy metal ion in asparagus saponin extract solution, belong to natural medicinal component
Preparation field.
Background technology
Asparagus is a kind of low in calories, low fat, the nutraceutical of high amino acid content, is one of ten big famous dish of the world.It is existing
For nutrition analysis shows, asparagus contain flavone compound, saponin(e, steroidal, amino acid, multivitamin, selenium, zinc, iron and
The multiple nutritional components such as protein, polysaccharide, therefore asparagus is eaten for a long time can improve a poor appetite, help digest, is fatigue-relieving, beneficial
Taste, but also there is the effect of reducing blood lipid, blood pressure lowering, softening blood vessel, the smart body by force of the calm benefit of diuresis and beauty.Asparagus is several at the same time
There is the effect of certain to all cancers.
Asparagus saponin(e is a kind of native compound of the extraction purification from asparagus, can be as food, medicine, cosmetics
Raw materials for production.Asparagus saponin(e has the function that strengthen immunity, reducing blood lipid.At present, it is extracted in asparagus to have separated more than ten
Kind saponin monomer, domestic and international many documents point out that steroid saponin compound is main anti-cancer principle.With isolation technics
Develop rapidly, increasingly attract people's attention to the purification ＆ isolation of asparagus saponin(e.The main method of asparagus saponin extraction is first
By being extracted to the organic solvent extracting solution of asparagus or its leftover bits and pieces, then separated using macroreticular resin chromatographic column
Purifying removes heavy metal ion therein.It is prepared by the extraction that a kind of asparagus saponin(e is disclosed such as Chinese patent (CN101791371A)
Method, asparagus saponin(e is can obtain after asparagus medicinal material ethanol extract is concentrated through extraction, macroreticular resin separation.Chinese patent
(CN102190697A) a kind of method for disclosing ultrasound-enhanced extraction and grading purification asparagus saponin(e, is that asparagus leftover bits and pieces exists
Reinforcing extraction is carried out in ultrasonic extraction device, concentrate adds saturation extracting n-butyl alcohol, carries out foam fraction factor purifying, and recycling obtains
Foam, is purified using macroporous resin column chromatography, is collected eluent, is drying to obtain high-purity asparagus saponin(e.These separation are pure
Although change method can realize the removal to heavy metal ion in asparagus saponin extract solution, it is usually required in removal process
His chemical reagent, be easy to cause secondary pollution, the damage that is inefficient and be easy to causeing asparagus saponin(e active ingredient removed
Lose.At the same time ion exchange resin in use particle size reduction easily exchange capacity is had an impact, regenerative process it is complicated, increase
Add production cost, waste of resource, and easily cause environmental pollution.Therefore, how to select a kind of more efficient, environmentally protective
Technology be applied to asparagus saponin separation purge process, the heavy metal ion removed in asparagus saponin extract solution seems particularly urgent
Cut.
The content of the invention
For overcome it is existing using the technique present in macroreticular resin chromatography it is cumbersome, easily cause in asparagus saponin(e effectively into
Point loss, there are chemical agent in saponin(e extract residual, waste of resource, be easy to cause the shortcomings of environmental pollution, this hair
It is bright to aim to provide a kind of method for conveniently removing heavy metal ion in asparagus saponin extract solution, to substitute macroporous resin column
Chromatography.
The present invention solves technical problem, adopts the following technical scheme that：
The method that the present invention removes heavy metal ion in asparagus saponin extract solution, its feature are：Utilize electrodialytic technique
Effectively remove the heavy metal ion in asparagus saponin extract solution；Comprise the concrete steps that：
Set electrodialysis plant, the electrodialysis plant by diluting compartment material pot, enriched chamber's material pot, pole room material pot,
Membrane module, three circulating pumps, DC power supply and pipeline composition；The membrane module is by anode, cathode and alternately superposition is arranged successively
Cation-exchange membrane, filter, the anion-exchange membrane of row are formed, composition anode chamber, diluting compartment, enriched chamber and cathode chamber, film pair
Number is 10~40 pairs, and membrane area is 200mm × 400mm；The anode chamber and cathode chamber by a circulating pump jointly and pole room
Material pot is connected；Diluting compartment is connected by circulating pump with diluting compartment material pot, and enriched chamber passes through circulating pump and enriched chamber's thing
Batch can is connected；Anode and cathode are connected on the cathode and anode of DC power supply by conducting wire respectively；During specific setting, three
The delivery outlet of material pot is connected by inlet of the pipeline respectively with three circulating pumps, and the infusion port of three circulating pumps passes through respectively
The inlet of pipeline compartment corresponding on membrane module connects, and the infusion port of each compartment passes through pipeline and corresponding material pot on membrane module
On inlet connection.
The asparagus saponin extract solution that solid content is 5%~10% is introduced to the diluting compartment material pot of electrodialysis plant first,
And tap water is added in enriched chamber's material pot, electrode solution (0.3M metabisulfite solutions) is added in pole room material pot；
Then control asparagus saponin extract solution to be circulated between diluting compartment and diluting compartment material pot by circulating pump, control
Tap water processed circulates between enriched chamber and enriched chamber's material pot, and control electrolyte is in anode chamber, cathode chamber and pole room thing
Circulated between batch can；
Constant voltage finally by from DC power supply to 40~100V of application on the cathode and anode of membrane module, control operation
Temperature passes through the electrical conductivity of asparagus saponin extract solution in conductivity meter monitoring diluting compartment below 35 DEG C；When electrical conductivity is 200
μScm-1When following, that is, complete the removal of heavy metal ion in asparagus saponin extract solution.
The amberplex can be the homogeneous ion-exchange membrane or heterogeneous ion-exchange membrane produced both at home and abroad, preferential to select
Homogeneous ion-exchange membrane.
The asparagus saponin extract solution is to take asparagus raw material to extract concentration by organic solvent to obtain, asparagus raw material used
For new fresh asparagus, asparagus fresh leaf, asparagus peel, dry product asparagus or asparagus leftover bits and pieces, organic solvent used is ethanol or n-butanol.
If the solid content of the asparagus saponin extract solution is higher than 10%, can be diluted by water or ethanol.
After being handled using electrodialytic technique asparagus saponin extract solution, the opposite removal efficiency of heavy metal ion reaches
More than 99%, the yield of asparagus saponin(e reaches 60.4%.
Asparagus saponin extract solution after the removing heavy metal ion of gained can be fed directly to decoloration back tender in next step
Skill, obtains asparagus saponin(e product.
The beneficial effects of the invention are as follows：
(1) present invention realizes the removal of heavy metal ion in asparagus saponin extract solution, whole mistake by electrodialysis process
Journey does not add additional chemical reagent, does not produce solid slag, alleviates the technique burden in downstream.
(2) present invention is more than 99% by electrodialysis process to the removal rate of heavy metal ion in asparagus saponin extract solution,
The yield of its asparagus saponin(e can reach 60.4%.
(3) present invention is relatively low by electrodialysis process processing asparagus saponin extract solution energy consumption, and method is simple, and operation control is held
Easily, the original structure of asparagus saponin(e will not be destroyed, environmental pollution will not be caused, is a kind of ideal technology side suitably promoted and applied
Method.
Brief description of the drawings
Fig. 1 is the process flow chart of the present invention；
Figure label：1 is enriched chamber's material pot；2 be diluting compartment material pot；3 be pole room material pot；4 be membrane module；5 are
DC power supply；6 be circulating pump.
Embodiment
Embodiment 1
As shown in Figure 1, the present embodiment removes heavy metal ion in asparagus saponin extract solution as follows：
Take asparagus raw material to extract by organic solvent ethanol to concentrate, obtain asparagus saponin extract solution 15L and (mainly contain asparagus
Saponin(e and a small amount of heavy metal ion and pigment etc., its solution ph are 5.4 or so, and electrical conductivity is about 11.65mS/cm, solid content
9.0%) content is；
Electrodialysis plant is set, as shown in Figure 1, electrodialysis plant is by diluting compartment material pot 2, enriched chamber's material pot 1, pole room
Material pot 3,4, three circulating pumps 6 of membrane module, DC power supply 5 and pipeline composition；Membrane module is by anode, cathode and replaces successively
Cation-exchange membrane, filter, the anion-exchange membrane being arranged under the overlay are formed, composition anode chamber, diluting compartment, enriched chamber and cathode
Room, film logarithm are 30 to (selected homogeneous ionic membrane is the production of Hefei Ke Jia high molecular materials Science and Technology Ltd., and cationic membrane is
Model CJMC-2, anionic membrane model CJMA-2), membrane area is 200mm × 400mm；Anode chamber and cathode chamber pass through one
A circulating pump is connected with pole room material pot jointly；Diluting compartment is connected by circulating pump with diluting compartment material pot, and enriched chamber leads to
Circulating pump is crossed with enriched chamber's material pot to be connected；Anode and cathode are connected to the cathode of DC power supply by conducting wire respectively and bear
Pole；
15L asparagus saponin extract solution is introduced to the diluting compartment material pot of electrodialysis plant, and is added in enriched chamber's material pot
Enter 15L tap water, 15L 0.3M metabisulfite solutions are added in pole room material pot；
Then control asparagus saponin extract solution to be circulated between diluting compartment and diluting compartment material pot by circulating pump, control
Tap water processed circulates between enriched chamber and enriched chamber's material pot, and control electrolyte is in anode chamber, cathode chamber and pole room thing
Circulated between batch can；
DC power supply is finally connected, applies the constant voltage of 40V to membrane module by DC power supply, control operation temperature exists
Less than 35 DEG C, start the heavy metal ion in electroosmose process removal asparagus saponin extract solution, diluting compartment is monitored by conductivity meter
The conductivity value of interior asparagus saponin extract solution, and time recording operation electric current and voltage.When electrical conductivity is in 200 μ Scm-1When following,
Complete the removal of heavy metal ion in asparagus saponin extract solution.
The operating time of the whole electrodialytic process of the present embodiment is 65min, and the removal rate of heavy metal ion is 99.0%, reed
The rate of recovery of bamboo shoot saponin(e is 60.4%.
Embodiment 2
The present embodiment removes heavy metal ion in asparagus saponin extract solution by the identical mode of embodiment 1, differs only in
The pH value of asparagus saponin extract solution used is 5.3 or so, and electrical conductivity is about 10.52mS/cm, solid content 8.2%；Into
During row electrodialysis, it is 60V to control voltage.
The operating time of the present embodiment whole process is 60min, and the removal rate of heavy metal ion is 99.05%, asparagus soap
The rate of recovery of glycosides is 59.6%.
Embodiment 3
The present embodiment removes heavy metal ion in asparagus saponin extract solution by the identical mode of embodiment 1, differs only in
The pH value of asparagus saponin extract solution used is 5.4 or so, and electrical conductivity is about 9.25mS/cm, solid content 7.2%；Into
During row electrodialysis, it is 70V to control voltage.
The operating time of the present embodiment whole process is 60min, and the removal rate of heavy metal ion is 99.12%, asparagus soap
The rate of recovery of glycosides is 58.6%.
Embodiment 4
The present embodiment removes heavy metal ion in asparagus saponin extract solution by the identical mode of embodiment 1, differs only in
The pH value of asparagus saponin extract solution used is 5.4 or so, and electrical conductivity is about 11.5mS/cm, solid content 9.0%；Into
During row electrodialysis, it is 80V to control voltage.
The operating time of the present embodiment whole process is 60min, and the removal rate of heavy metal ion is 99.18%, asparagus soap
The rate of recovery of glycosides is 59.2%.
Embodiment 5
The present embodiment removes heavy metal ion in asparagus saponin extract solution by the identical mode of embodiment 1, differs only in
The pH value of asparagus saponin extract solution used is 5.4 or so, and electrical conductivity is about 11.53mS/cm, solid content 9.0%；Into
During row electrodialysis, it is 100V to control voltage.
The operating time of the present embodiment whole process is 60min, and the removal rate of heavy metal ion is 99.24%, asparagus soap
The rate of recovery of glycosides is 59.4%.
Embodiment 6
The present embodiment removes heavy metal ion in asparagus saponin extract solution by the identical mode of embodiment 1, differs only in
The pH value of asparagus saponin extract solution used is 5.4 or so, and electrical conductivity is about 11.53mS/cm, solid content 9.0%；Desalination
The volume of asparagus saponin extract solution is 15L in the material pot of room, and originally water volume is 30L in enriched chamber's material pot, pole room material pot
The volume of interior electrolyte is 15L, and when carrying out electrodialysis, it is 60V to control voltage.
The operating time of the present embodiment whole process is 50min, and the removal rate of heavy metal ion is 99.2%, asparagus saponin(e
The rate of recovery be 59%.
Claims (2)
- A kind of 1. method for removing heavy metal ion in asparagus saponin extract solution, it is characterised in that：It is effective using electrodialytic technique The heavy metal ion in asparagus saponin extract solution is removed, is specifically comprised the following steps：Electrodialysis plant is set, and the electrodialysis plant is by diluting compartment material pot, enriched chamber's material pot, pole room material pot, film group Part, three circulating pumps, DC power supply and pipeline composition；The membrane module is by anode, cathode and is alternately arranged under the overlay successively Cation-exchange membrane, filter, anion-exchange membrane are formed, and composition anode chamber, diluting compartment, enriched chamber and cathode chamber, film logarithm are 10~40 pairs, membrane area is 200mm × 400mm；The anode chamber and cathode chamber by a circulating pump jointly with pole room material Tank is connected；Diluting compartment is connected by circulating pump with diluting compartment material pot, and enriched chamber passes through circulating pump and enriched chamber's material pot It is connected；Anode and cathode are connected on the cathode and anode of DC power supply by conducting wire respectively；Diluting compartment material pot first by solid content for 5%~10% asparagus saponin extract solution introducing electrodialysis plant, and Tap water is added in enriched chamber's material pot, electrode solution is added in pole room material pot；The asparagus saponin extract solution is to take asparagus Raw material extracts concentration by organic solvent and obtains, and asparagus raw material used is new fresh asparagus, asparagus fresh leaf, asparagus peel, dry product reed Bamboo shoot or asparagus leftover bits and pieces, organic solvent used are ethanol or n-butanol；Then asparagus saponin extract solution is controlled to be circulated between diluting compartment and diluting compartment material pot by circulating pump, control is certainly Water circulates between enriched chamber and enriched chamber's material pot, and control electrolyte is in anode chamber, cathode chamber and pole room material pot Between circulate；Constant voltage finally by from DC power supply to 40~100V of application on the cathode and anode of membrane module, control operation temperature Below 35 DEG C, and pass through the electrical conductivity of asparagus saponin extract solution in conductivity meter monitoring diluting compartment；When electrical conductivity is in 200 μ Scm-1When following, that is, complete the removal of heavy metal ion in asparagus saponin extract solution；After being handled using electrodialytic technique asparagus saponin extract solution, the opposite removal efficiency of heavy metal ion reaches 99% More than, the yield of asparagus saponin(e reaches 60.4%.
- 2. the method according to claim 1 for removing heavy metal ion in asparagus saponin extract solution, it is characterised in that：It is used Amberplex is homogeneous ion-exchange membrane.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610020661.XA CN105617867B (en) | 2016-01-11 | 2016-01-11 | A kind of method for removing heavy metal ion in asparagus saponin extract solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610020661.XA CN105617867B (en) | 2016-01-11 | 2016-01-11 | A kind of method for removing heavy metal ion in asparagus saponin extract solution |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105617867A CN105617867A (en) | 2016-06-01 |
| CN105617867B true CN105617867B (en) | 2018-04-20 |
Family
ID=56033444
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610020661.XA Active CN105617867B (en) | 2016-01-11 | 2016-01-11 | A kind of method for removing heavy metal ion in asparagus saponin extract solution |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105617867B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106421494A (en) * | 2016-12-01 | 2017-02-22 | 秦皇岛长胜营养健康科技有限公司 | Application of asparagus extract in preparation of health-care products or health-care drugs for promoting and improving memory |
| CN107252021A (en) * | 2017-07-10 | 2017-10-17 | 秦皇岛长胜营养健康科技有限公司 | Reduce asparagus drink of Intima-medial thickness effect and its preparation method and application |
| CN109105586A (en) * | 2018-09-05 | 2019-01-01 | 安徽农业大学 | A method of preparing low fluorine instant tea powder |
| CN112568303B (en) * | 2020-12-03 | 2023-08-29 | 杭州凯洁膜分离技术有限公司 | Instant tea preparation process based on microfiltration-reverse osmosis technology |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101108306A (en) * | 2007-04-27 | 2008-01-23 | 上海现代中医药技术发展有限公司 | Method for removing heavy metal in plants raffinate with electrodialysis method |
| CN203699994U (en) * | 2013-12-31 | 2014-07-09 | 常州千帆环保科技有限公司 | High-salt wastewater electrodialysis device |
| CN104058537A (en) * | 2014-04-30 | 2014-09-24 | 浙江工业大学 | Method for treating cefalexin enzyme-process synthesizing mother liquor wastewater |
-
2016
- 2016-01-11 CN CN201610020661.XA patent/CN105617867B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101108306A (en) * | 2007-04-27 | 2008-01-23 | 上海现代中医药技术发展有限公司 | Method for removing heavy metal in plants raffinate with electrodialysis method |
| CN203699994U (en) * | 2013-12-31 | 2014-07-09 | 常州千帆环保科技有限公司 | High-salt wastewater electrodialysis device |
| CN104058537A (en) * | 2014-04-30 | 2014-09-24 | 浙江工业大学 | Method for treating cefalexin enzyme-process synthesizing mother liquor wastewater |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105617867A (en) | 2016-06-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105617867B (en) | A kind of method for removing heavy metal ion in asparagus saponin extract solution | |
| CN101879380A (en) | Energy-saving concentration process for extracting active ingredients of plants and concentration device thereof | |
| CN101503469B (en) | Method for extracting soy protein, oligosaccharide and isoflavone from soybean whey by two-stage two-segment film | |
| CN101851297A (en) | High-efficiency extraction process of polygahatous plysaccharides | |
| CN102178003A (en) | Process for extracting tea polyphenol | |
| CN1854149A (en) | Extraction of Momordica grosvenori beet aglucone V | |
| CN101870722A (en) | Process for concentrating protein in soy protein wastewater by two-stage foam separation method | |
| CN104480168A (en) | Method for preparing chondroitin sulfate and co-producing collagen peptide and biological calcium by using fishbone | |
| CN105254500B (en) | A kind of method that high-purity chlorogenic acid is prepared in the Leave extract from the bark of eucommia | |
| CN102432479B (en) | Method for extracting L-valine from L-valine fermentation liquid | |
| CN104119229A (en) | Technology for producing pure chlorogenic acid | |
| CN204824686U (en) | Separation and purification and enrichment facility of lycium barbarum polysaccharide extract | |
| CN106188335B (en) | The synchronous method and system for extracting pectin and polyphenol in citrus can processing technique | |
| CN102228488A (en) | Preparation of Lysimachia capillipes Hemsl total saponin | |
| CN104404094A (en) | Method for extracting taurine by use of enzymatic conversion method on the basis of clams | |
| CN103333213A (en) | Method for extracting oleuropein from olive leaves | |
| CN103992364A (en) | Separation extraction method of fondaparinux sodium | |
| CN105622342A (en) | Method for separating 2,3-butanediol | |
| CN104744241A (en) | Method for purification of citric acid from citric acid fermentation liquid | |
| CN201710997U (en) | Energy-saving plant active ingredient extracting and concentrating device | |
| CN103122018A (en) | Integrated preparation method for mogrosides | |
| CN105481152A (en) | Method for continuously removing chlorine and nitrate in extracting solution of tobacco | |
| CN104447427A (en) | Method for extracting taurine from sea cucumber intestines | |
| CN204447772U (en) | A kind of separation and purification of agate card polysaccharide and enrichment facility | |
| CN103951728A (en) | Method for selectively extracting protein of yeast cell |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |