CN110038527A - A kind of preparation method for the chromatography agent of separating-purifying rutin plant fiber - Google Patents
A kind of preparation method for the chromatography agent of separating-purifying rutin plant fiber Download PDFInfo
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- CN110038527A CN110038527A CN201910215316.5A CN201910215316A CN110038527A CN 110038527 A CN110038527 A CN 110038527A CN 201910215316 A CN201910215316 A CN 201910215316A CN 110038527 A CN110038527 A CN 110038527A
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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Abstract
The invention discloses a kind of preparation methods for the chromatography agent of separating-purifying rutin plant fiber, which is characterized in that is pre-processed using sulfuric acid and potassium permanganate mixed solution to soybean fiber；Amination is carried out to pretreated soybean azelon using hexamethylene diamine and ammonium carbonate；Then, in the reactor, it is added by following composition mass percentage concentration, deionized water: 74 ~ 77%, sulfuric acid: 10 ~ 14%, cucurbit [8] urea: 3 ~ 5%, stirring and dissolving, adds amination soybean fiber: 8 ~ 10%, the sum of each component is absolutely, in 60 ± 2 DEG C of constant temperature, stirring, back flow reaction 6h, after cooling, it is washed with deionized to neutrality, is separated by solid-liquid separation, it is dry, it obtains chromatographing agent for separating-purifying rutin plant fiber.The adsorbent has very high adsorption capacity to rutin, has specificity with specifically, at low cost, high mechanical strength can be Reusability 10 times or more, and adsorbent can be easily separated.
Description
Technical field
The present invention relates to a kind of preparation methods of modified magnetic biological adsorption agent, in particular to a kind of to be used for separating-purifying reed
Fourth plant fiber chromatographs the preparation method of agent and the application to the purification of rutin adsorbing separation, belongs to separation and purification technical field.
Background technique
Rutin is the flavonols glycocide being widely present in plant, and two glycocides are glucose and rhamnose.It is light
Yellow or light green acicular crystal or crystalline powder can be used as edible antioxidant and nutrition enhancer etc..Rutin has dimension to give birth to
The effect of plain P sample and anti-inflammatory effect can be reduced if mustard oil is to inflammation caused by animal eyes or skin, there is an antivirus action, and 200
When μ g/mL concentration, there is maximum inhibiting effect to vesicular stomatitis virus.There is strong antioxidant, rutin addition is imbued with molten
In the homogenate of enzyme body, the formation of lipoids peroxide can be inhibited.The ultraviolet light in 280~335nm can be absorbed strongly, can be used for
Sun-proof whitening type cosmetics.Have the effects that maintain vascular resistance, reduce its permeability, reduce brittleness.It can be used for preventing and treating brain
The diseases such as hemorrhage, hypertension, retinal hemorrhage, purpura and acute hemorrhagic ephritis.From plant separating-purifying rutin, drug,
The separation of rutin has great importance in biological sample.
Cucurbituril [n] (cucurbit [n] uril, n=4 ~ 12, CB [n]) is supramolecular chemistry relaying cyclodextrin, crown ether
And the symmetrical tubbiness series macrocyclic compound of a kind of novel high to grow up after calixarenes, 1905, German chemist
It is this with urea and methylene that the simple reaction that Behrend etc. passes through between urea, glyoxal and formaldehyde is prepared for Cucurbituril for the first time
For the cyclic compound of unit.Cucurbituril is bonded by n glycoluril unit and 2n methylene units, has hydrophobic inside
Cavity and the port being made of circular carbonylic oxygen atom.This allows for it can be by hydrophobic effect, hydrogen bond, ion dipole
Equal bonding actions are bonded a variety of organic molecules, can form inclusion compound with polarity and the organic object being dimensioned for.
The structure of Cucurbituril has stronger rigidity.Cucurbituril cannot change shape to be suitble to guest molecule, therefore can be with
Prediction coordination must be accompanied by very strong specificity and specificity.Cucurbit [n] though urea polarized carbonyl, due to its point
Minor structure high degree of symmetry causes the presence of some special physics and chemical property.With crown ether, calixarenes, the big ring of cyclodextrin
Cryptand is compared, it has stronger rigid structure, can be accommodated metal ion of different sizes, is not only preferable supplied for electronic
Base, and it is also more stable in terms of dynamics.Cucurbituril two-port size is identical, and port is surround by carbonyl, and carbonyl can be formed
Cationic binding site can also be bonded the electro-mechanical part of organic molecule by the hydrogen bond action of dipolar interaction and allophanyl
Point.Cucurbituril cavity is due to hydrophobicity, it is possible to include organic molecule.Cucurbituril cavity diameter is greater than port diameter,
Carbonyl number on each port is equal with number of monomers (degree of polymerization), and the Cucurbituril that the degree of polymerization is different, has sky of different sizes
Chamber and port diameter, molecular capsule or the main object that with different size of various matter interactions, can form self assembly are real
Body.Therefore, the research of the molecular capsule based on cucurbit [n] urea is in molecular recognition, the fractionation of optically active substance, compound
Trap with separate, catalyst and function nano material, the absorption of various drugs or desorption, self-assembled structures and oversubscription fructification
Equal fields will all have broad application prospects and development potentiality.
Soybean fiber belongs to aftergrowth azelon, using food grade soyabean protein powder as raw material, utilizes biology
Engineering technology extracts the globulin in albumen powder, by adding functional aid, is grafted, altogether with high polymers such as itrile group, hydroxyls
Poly-, blending, is made certain density protein spinning solution, changes protein steric structure, forms through wet spinning.It has
Soft feel as cashmere, the sub-dued lustre as silk are praised better than the excellent performances such as the warmth retention property of cotton and good skin-friendly
For " health and comfort fiber of new century " and " the good fabric that skin is liked ".Soybean fiber outer layer is essentially all albumen
Matter, containing a variety of amino acid needed by human, soybean fiber has carboxyl abundant, amino groups, it is easy to will live
Property group connection on.Soybean fiber is with relative density is low, specific strength is high, large specific surface area, light-weight, good penetrability
The advantages that, usual specific surface area is bigger, hole is more, the site of surface link functional group is abundanter, the active group chained
More, the adsorption capacity of the more adsorbents of active group is bigger, and adsorption capacity is stronger.
Summary of the invention
An object of the present invention is to provide a kind of preparation method for the chromatography agent of separating-purifying rutin plant fiber, separately
One purpose is a kind of carry out separating-purifying for the chromatography agent of separating-purifying rutin plant fiber to rutin obtained.
The purpose of the present invention is achieved through the following technical solutions.
It is a kind of for separating-purifying rutin plant fiber chromatography agent preparation method, which is characterized in that this method have with
Lower processing step:
(1) soybean fiber pre-processes: soybean fiber being crushed, be sieved 20 mesh, with 3mol/L sulfuric acid and 0.5mol/L
In potassium permanganate mixed solution, 8 ~ 10 h of soaking at room temperature, then 10min is boiled, after cooling, filtering is washed with deionized into
Property, it is separated by solid-liquid separation, it is dry, obtain pretreated soybean azelon；
(2) it amination soybean fiber: in the reactor, is added by following composition mass percentage concentration, deionized water: 80 ~
82%, hexamethylene diamine: 6 ~ 8%, ammonium carbonate: 2 ~ 4%, heating stirring dissolution, pretreated soybean azelon: 8 ~ 10%, each group
/ and absolutely, in 80 ± 2 DEG C of constant temperature, stirring, 4 ~ 6h of back flow reaction, after cooling, with ethanol washing, to be separated by solid-liquid separation,
It is dry, obtain amination soybean fiber；
(3) preparation for the chromatography agent of separating-purifying rutin plant fiber: in the reactor, by following composition mass percentage concentration
It is added, deionized water: 74 ~ 77%, sulfuric acid: 10 ~ 14%, cucurbit [8] urea: 3 ~ 5%, stirring and dissolving adds amination soybean protein
Fiber: 8 ~ 10%, the sum of each component is absolutely, to use deionization after cooling in 60 ± 2 DEG C of constant temperature, stirring, back flow reaction 6h
Water washing is separated by solid-liquid separation, drying to neutrality, obtains chromatographing agent for separating-purifying rutin plant fiber.
Soybean fiber as described in step (1) and 3mol/L sulfuric acid and 0.5mol/L potassium permanganate mixed solution are consolidated
Liquor ratio is between 1g:20 ~ 25mL.
Adsorbent uses the characteristics of method are as follows: preparation is used for separating-purifying rutin plant fiber chromatography agent deionized water
0.5 ~ 1h is impregnated, is adsorbed by static method.
The separating-purifying rutin plant fiber chromatography agent deionized water that is used for of preparation is impregnated into 0.5 ~ 1h, is inhaled by dynamic method
It is attached.
Compared with the prior art, the present invention has the following advantages and beneficial effects:
(1) what the present invention obtained has good physical and chemical stability and excellent for the chromatography agent of separating-purifying rutin plant fiber
Different mechanical strength, have big specific surface area, adsorption capacity is big, to rutin maximum adsorption capacity reach 65.25mg/g, it is wear-resisting can
Reusability number is up to 10 times or more, and the speed of absorption is fast, and absorption chooses, and desorption performance is good, can be in wider soda acid
It is used in range.
(2) what the present invention obtained had both had the excellent of solid support material for the chromatography agent of separating-purifying rutin plant fiber
Point also solves the losing issue in active group application, to rutin with very strong specificity and specifically.
(3) condition for crossing range request of synthesis is easy to control, and low energy consumption, easy to operate, is belonged to process for cleanly preparing, is easy to
Industrialized production is natural green product, biodegradable.
Specific embodiment
Embodiment 1
(1) soybean fiber pre-processes: in the reactor, being separately added into, 3mol/L sulfuric acid and 0.5mol/L potassium permanganate are mixed
500 mL of solution, milling soya seeds azelon 25 g, soaking at room temperature 9h are closed, then boils 10min, after cooling, deionization is used in filtering
Water washing is separated by solid-liquid separation, drying obtains pretreated soybean azelon to neutrality；
(2) it amination soybean fiber: in the reactor, is separately added into, deionized water: 81 mL, hexamethylene diamine:
7g, ammonium carbonate: 3g, heating stirring dissolution, pretreated soybean azelon: 9g, in 80 ± 2 DEG C of constant temperature, stirring, back flow reactions
5h after cooling, with ethanol washing, is separated by solid-liquid separation, dry, obtains amination soybean fiber；
(3) it the preparation for the chromatography agent of separating-purifying rutin plant fiber: in the reactor, is separately added into, deionized water: 75
ML, sulfuric acid: 6.5 mL, cucurbit [8] urea: 4g, stirring and dissolving add amination soybean fiber: 9g, in 60 ± 2 DEG C of perseverances
Temperature, stirring, back flow reaction 6h after cooling, be washed with deionized to neutrality, be separated by solid-liquid separation, dry, obtain for separating-purifying
Rutin plant fiber chromatographs agent.
Embodiment 2
(1) soybean fiber pre-processes: in the reactor, being separately added into, 3mol/L sulfuric acid and 0.5mol/L potassium permanganate are mixed
Close 1250 mL of solution, milling soya seeds azelon 50 g, soaking at room temperature 8h, then boil 10min, after cooling, filtering, spend from
Sub- water washing is separated by solid-liquid separation, drying obtains pretreated soybean azelon to neutrality；
(2) it amination soybean fiber: in the reactor, is separately added into, deionized water: 400 mL, hexamethylene diamine:
32g, ammonium carbonate: 10g, heating stirring dissolution, pretreated soybean azelon: 50g is anti-in 80 ± 2 DEG C of constant temperature, stirring, reflux
4h is answered, after cooling, with ethanol washing, is separated by solid-liquid separation, it is dry, obtain amination soybean fiber；
(3) it the preparation for the chromatography agent of separating-purifying rutin plant fiber: in the reactor, is separately added into, deionized water:
370mL, sulfuric acid: 38 mL, cucurbit [8] urea: 15g, stirring and dissolving add amination soybean fiber: 50g, in 60 ± 2
DEG C constant temperature, stirring, back flow reaction 6h after cooling, be washed with deionized to neutrality, be separated by solid-liquid separation, dry, obtain for separating
It purifies rutin plant fiber and chromatographs agent.
Embodiment 3
(1) soybean fiber pre-processes: in the reactor, being separately added into, 3mol/L sulfuric acid and 0.5mol/L potassium permanganate are mixed
880 mL of solution, milling soya seeds azelon 40g, soaking at room temperature 10h are closed, then boils 10min, after cooling, deionization is used in filtering
Water washing is separated by solid-liquid separation, drying obtains pretreated soybean azelon to neutrality；
(2) it amination soybean fiber: in the reactor, is separately added into, deionized water: 330 mL, hexamethylene diamine:
24g, ammonium carbonate: 16g, heating stirring dissolution, pretreated soybean azelon: 32g is anti-in 80 ± 2 DEG C of constant temperature, stirring, reflux
6h is answered, after cooling, with ethanol washing, is separated by solid-liquid separation, it is dry, obtain amination soybean fiber；
(3) it the preparation for the chromatography agent of separating-purifying rutin plant fiber: in the reactor, is separately added into, deionized water:
310mL, sulfuric acid: 22 mL, cucurbit [8] urea: 20g, stirring and dissolving add amination soybean fiber: 32g, in 60 ± 2
DEG C constant temperature, stirring, back flow reaction 6h after cooling, be washed with deionized to neutrality, be separated by solid-liquid separation, dry, obtain for separating
It purifies rutin plant fiber and chromatographs agent.
Embodiment 4
(1) soybean fiber pre-processes: in the reactor, being separately added into, 3mol/L sulfuric acid and 0.5mol/L potassium permanganate are mixed
Close 250 mL of solution, milling soya seeds azelon 10 g, soaking at room temperature 9.5h, then boil 10min, after cooling, filtering, spend from
Sub- water washing is separated by solid-liquid separation, drying obtains pretreated soybean azelon to neutrality；
(2) it amination soybean fiber: in the reactor, is separately added into, deionized water: 80 mL, hexamethylene diamine:
7g, ammonium carbonate: 4g, heating stirring dissolution, pretreated soybean azelon: 9g, in 80 ± 2 DEG C of constant temperature, stirring, back flow reactions
4.5h after cooling, with ethanol washing, is separated by solid-liquid separation, dry, obtains amination soybean fiber；
(3) it the preparation for the chromatography agent of separating-purifying rutin plant fiber: in the reactor, is separately added into, deionized water:
76mL, sulfuric acid: 6mL, cucurbit [8] urea: 4g, stirring and dissolving add amination soybean fiber: 9g, in 60 ± 2 DEG C of perseverances
Temperature, stirring, back flow reaction 6h after cooling, be washed with deionized to neutrality, be separated by solid-liquid separation, dry, obtain for separating-purifying
Rutin plant fiber chromatographs agent.
Embodiment 5
It weighs 1.0g and is placed in 0.5 ~ 1.0h of immersion in 250mL stuffed conical flask for the chromatography agent of separating-purifying rutin plant fiber,
After filtration washing, it is in 100mg/L rutin standard solution, with the pH value of diluted acid or alkali regulation system for 5.0 that 100mL concentration, which is added,
~ 7.0,30 min of concussion absorption, take supernatant at room temperature, with the concentration of determined by ultraviolet spectrophotometry rutin, according to absorption
The concentration difference of rutin in the solution of front and back calculates the removal rate for the chromatography agent of separating-purifying rutin plant fiber to rutin, this
The obtained separating-purifying rutin plant fiber that is used for of invention chromatographs agent to the removal rate of rutin all 95.82% or more, and highest can
Up to 96.5%.The concentration of rutin standard solution is increased into 800mg/L by same steps, measurement is used for separating-purifying rutin plant
It is 65.25mg/g to rutin adsorption capacity that fiber, which chromatographs agent,.
Claims (3)
1. a kind of preparation method for the chromatography agent of separating-purifying rutin plant fiber, which is characterized in that this method has following
Processing step:
(1) soybean fiber pre-processes: soybean fiber being crushed, be sieved 20 mesh, with 3mol/L sulfuric acid and 0.5mol/L
In potassium permanganate mixed solution, 8 ~ 10 h of soaking at room temperature, then 10min is boiled, after cooling, filtering is washed with deionized into
Property, it is separated by solid-liquid separation, it is dry, obtain pretreated soybean azelon；
(2) it amination soybean fiber: in the reactor, is added by following composition mass percentage concentration, deionized water: 80 ~
82%, hexamethylene diamine: 6 ~ 8%, ammonium carbonate: 2 ~ 4%, heating stirring dissolution, pretreated soybean azelon: 8 ~ 10%, each group
/ and absolutely, in 80 ± 2 DEG C of constant temperature, stirring, 4 ~ 6h of back flow reaction, after cooling, with ethanol washing, to be separated by solid-liquid separation,
It is dry, obtain amination soybean fiber；
(3) preparation for the chromatography agent of separating-purifying rutin plant fiber: in the reactor, by following composition mass percentage concentration
It is added, deionized water: 74 ~ 77%, sulfuric acid: 10 ~ 14%, cucurbit [8] urea: 3 ~ 5%, stirring and dissolving adds amination soybean protein
Fiber: 8 ~ 10%, the sum of each component is absolutely, to use deionization after cooling in 60 ± 2 DEG C of constant temperature, stirring, back flow reaction 6h
Water washing is separated by solid-liquid separation, drying to neutrality, obtains chromatographing agent for separating-purifying rutin plant fiber.
2. a kind of preparation method for the chromatography agent of separating-purifying rutin plant fiber according to claim 1, special
Sign is, soybean fiber as described in step (1) and 3mol/L sulfuric acid and 0.5mol/L potassium permanganate mixed solution are consolidated
Liquor ratio is between 1g:20 ~ 25mL.
3. prepared by a kind of preparation method for the chromatography agent of separating-purifying rutin plant fiber according to claim 1
Chromatograph agent for separating-purifying rutin plant fiber, which is characterized in that it is described to be used for separating-purifying rutin plant fiber layer
Analyse application of the agent in rutin separating-purifying.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103920469A (en) * | 2014-05-06 | 2014-07-16 | 济南大学 | Preparation method of citric acid silk adsorbent |
| CN104826598A (en) * | 2015-04-14 | 2015-08-12 | 中山大学 | Preparation and applications of novel separation medium magnetic perhydroxycucurbit[8]uril |
| CN109046270A (en) * | 2018-09-04 | 2018-12-21 | 武汉纺织大学 | Cucurbit [8] urea grafted chitosan and its preparation method and application |
-
2019
- 2019-03-21 CN CN201910215316.5A patent/CN110038527A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103920469A (en) * | 2014-05-06 | 2014-07-16 | 济南大学 | Preparation method of citric acid silk adsorbent |
| CN104826598A (en) * | 2015-04-14 | 2015-08-12 | 中山大学 | Preparation and applications of novel separation medium magnetic perhydroxycucurbit[8]uril |
| CN109046270A (en) * | 2018-09-04 | 2018-12-21 | 武汉纺织大学 | Cucurbit [8] urea grafted chitosan and its preparation method and application |
Non-Patent Citations (1)
| Title |
|---|
| 卢惠娟 等: "葫芦脲对活性染料K-GN及X-GR吸附脱色的研究", 《武汉纺织大学学报》 * |
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