CN102936315B - Preparation method of molecularly imprinted polymer capable of enriching hispidin - Google Patents
Preparation method of molecularly imprinted polymer capable of enriching hispidin Download PDFInfo
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- CN102936315B CN102936315B CN201210479968.8A CN201210479968A CN102936315B CN 102936315 B CN102936315 B CN 102936315B CN 201210479968 A CN201210479968 A CN 201210479968A CN 102936315 B CN102936315 B CN 102936315B
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Abstract
The invention relates to a preparation method of a molecularly imprinted polymer capable of enriching hispidin, which comprises the following steps: by using hispidin as a template molecule, a tetrahydrofuran-isooctane mixed solvent as a pore-forming agent, acrylamide as a functional monomer, ethylene glycol dimethyl acrylate as a crosslinking agent and azodiisobutyronitrile as an initiator, evenly mixing, carrying nitrogen-blowing deoxidization, carrying out thermostatic water bath reaction, carrying out Soxhlet extraction, and drying to obtain the molecularly imprinted polymer. The preparation method has the advantages of simple technique and low cost, and is easy to implement; and the prepared molecularly imprinted polymer can be used for separating and extracting hispidin from natural products, has the advantages of high specificity and long service life, and especially can implement quick enrichment and purification for some natural products with very low hispidin content.
Description
Technical field
The present invention relates to molecularly imprinted polymer, particularly a kind of preparation method of molecularly imprinted polymer that can enrichment bristle element.
Background technology
Bristle element (hispidin) is one of activeconstituents of multiple medicinal fungi, has the biologic activity such as anti-oxidant, anti-tumour cell proliferative, Inhibit the replication of HIV-1, anti-senile dementia.Research finds that bristle element has stronger restraining effect to protein kinase C, and this may be one of reason of its inducing apoptosis of tumour cell.Yet; the natural origin of the bristle element of report is limited at present; mainly from the mushroom class of Phellinus and pin hole Pseudomonas, as Phellinus bacterium (phellinus igniarius), Phaeopoms obliquus (Inonotus obliquus), oblique raw brown pore fungi (Phaeoporus obliquus) etc.Therefore the natural resource that, further exploitation contains bristle element have important practical significance.
Molecular imprinting is to grow up under the impact of antigen-antibody interaction mechanism.Utilize target molecule as template, and it is combined with the mode of the function monomer with complementary structure by covalent linkage or non covalent bond, and add linking agent to carry out polyreaction, remove again after template molecule, can obtain the imprinted polymer mating completely with template molecule on space structure and functional group.Because this imprinted polymer has single-minded recognition capability to template molecule, and there is good physical and chemical stability, and the advantage such as long service life, make molecular imprinting all represent good application prospect in fields such as chiral drug separation, Solid-Phase Extraction, clinical medicine analysis, membrane separation technique, mimetic enzyme catalysis, Biomimic sensors.Solid phase extraction techniques has the advantages such as easily collecting, simple to operate, enrichment times is large, is a kind of conventional sample-pretreating method.Therefore, adopt molecularly imprinted polymer as Solid phase extraction separation enrichment material, can set up the extraction and separation method of a set of quick, accurate, easy separate targets thing.
Summary of the invention
The object of the invention is for above-mentioned technical Analysis, a kind of preparation method of molecularly imprinted polymer that can enrichment bristle element is provided, utilize this Molecularly Imprinted Polymer and template molecule mating completely at space structure and binding site, directly separation and concentration bristle element from natural product, sets up a kind of bristle element extraction and separation method that can be quick, safe, easy.
Technical scheme of the present invention:
A kind of preparation method of molecularly imprinted polymer that can enrichment bristle element, take bristle element as template molecule, take tetrahydrofuran (THF) and octane-iso mixed solvent as pore-creating agent, take acrylamide as function monomer, take ethylene glycol dimethacrylate as linking agent, take Diisopropyl azodicarboxylate as initiator, and step is as follows:
1) template molecule bristle element and function monomer acrylamide are dissolved in the mixed solvent of pore-creating agent tetrahydrofuran (THF) and octane-iso, mix and stir 2h;
2) add linking agent ethylene glycol dimethacrylate, mix and stir 10min;
3) add again initiator Diisopropyl azodicarboxylate, mix and stir 10min, obtain mixed solution;
4) by water-bath 72h at 60 ℃ of above-mentioned mixed solution nitrogen flushing deoxidation 4min, constant temperature, obtain bulk polymer;
5) above-mentioned bulk polymer is ground, with sizing screen, screen and retain 60 order-100 purpose polymers particles, then polymer beads is passed through to the extracting of Soxhlet extract to remove unreacted reactant, the extracting time is 48h, obtains molecularly imprinted polymer;
6) by above-mentioned molecularly imprinted polymer, in temperature, be dry at 60 ℃, can make can enrichment bristle element molecularly imprinted polymer.
In described pore-creating agent, the volume ratio of tetrahydrofuran (THF) and octane-iso is 5:1.
The mol ratio of described template molecule, function monomer and linking agent is 1:5:35.
The add-on of described initiator Diisopropyl azodicarboxylate is 0.25% of pore-creating agent, function monomer and linking agent total mass.
Described Soxhlet extract is that volume ratio is the methyl alcohol of 9:1 and the mixed solution of acetic acid.
Prepared by aforesaid method can enrichment bristle element the application of molecularly imprinted polymer, for, enrichment separated from Phellinus bacterium to extract bristle element.
Advantage of the present invention and positively effect are: this preparation method's technique is simple, cost is low, easy to implement, the molecularly imprinted polymer of preparation can be used for from natural product separation and Extraction bristle element and specificity is strong, long service life, particularly, for the very low natural product of some bristle cellulose contents, can realize fast enriching purifying.
Accompanying drawing explanation
Accompanying drawing is the test pattern of the bristle element in the separated Phellinus bacterium of this molecularly imprinted polymer of application crude extract.
In figure: peak A is the test value of bristle element; Curve (1) is the test value of Phellinus bacterium crude extract, the test value that curve (2) is the elutriant that obtains through bristle element molecular imprinting column separating purification.
Embodiment
Embodiment:
A preparation method for molecularly imprinted polymer that can enrichment bristle element, step is as follows:
1) 61.5mg bristle element and 88.85mg acrylamide are dissolved in the mixed solvent of 10mL tetrahydrofuran (THF) and 2mL octane-iso, mix and stir 2h;
2) add 1647 μ L ethylene glycol dimethacrylates, mix and stir 10min;
3) add again 30mg Diisopropyl azodicarboxylate, mix and stir 10min, obtain mixed solution;
4), by above-mentioned mixed solution nitrogen flushing deoxidation 4min, sealing is placed in thermostat water bath and reacts 72h at 60 ℃, obtains bulk polymer;
5) above-mentioned bulk polymer is ground with mortar, with sizing screen, screen and retain 60 order-100 purpose polymers particles, then polymer beads is used the extracting of 250mL Soxhlet extract to remove unreacted reactant, Soxhlet extract is that volume ratio is the methyl alcohol of 9:1 and the mixed solution of acetic acid, the extracting time is 48h, obtains molecularly imprinted polymer;
6) by above-mentioned molecularly imprinted polymer, in temperature, be dry at 60 ℃, can make can enrichment bristle element molecularly imprinted polymer.
Molecularly imprinted polymer that can enrichment bristle element by this is for, enrichment separated from Phellinus bacterium to extract bristle element, and experimental technique and effect are as follows:
At the SPE of 4mL blank pipe two ends, place pad, load uniformly therein the prepared molecularly imprinted polymer of 150mg.The 10mL10% methyl alcohol balance for SPE of molecularly imprinted polymer will be filled with; By 300ml methanol extraction three times of 10g Phellinus bacterium, united extraction liquid, utilizes rotary evaporation to remove solvent, and the extract obtaining is dissolved in to 200ml water, with equal-volume ethyl acetate extraction three times.Combined ethyl acetate phase, and remove solvent by rotary evaporation, finally obtain Phellinus bacterium crude extract.The Phellinus bacterium crude extract obtaining is dissolved in to the methanol solution of 150mL 10%; 150mL sample solution is crossed to the SPE post that molecularly imprinted polymer is housed, at this moment bristle element is attracted on enrichment material.Then with 24mL 40% methyl alcohol, wash assorted, wash away the material of non-specific adsorption on pillar, with 20mL methyl alcohol and acetic acid (9:1, V/V) mixing solutions wash-out, the elutriant obtaining utilizes Rotary Evaporators to remove solvent, finally use 2ml dissolve with methanol extract, be by the bristle of molecular blotting column specific adsorption element.
Detected result as shown in drawings, shows in figure: when Phellinus bacterium crude extract is after specific molecular trace post concentration and separation, bristle element has obtained enrichment, and the content of other components in Phellinus crude extract has obvious reduction.As can be seen here, the bristle in the adsorption sample that the bristle of preparation element molecularly imprinted polymer can be single-minded is plain, thereby reaches the object of enriching and purifying.
Claims (2)
- One kind can enrichment bristle element the preparation method of molecularly imprinted polymer, it is characterized in that: take bristle element as template molecule, take tetrahydrofuran (THF) and octane-iso mixed solvent as pore-creating agent, take acrylamide as function monomer, take ethylene glycol dimethacrylate as linking agent, take Diisopropyl azodicarboxylate as initiator, and step is as follows:1) template molecule bristle element and function monomer acrylamide are dissolved in the mixed solvent of pore-creating agent tetrahydrofuran (THF) and octane-iso, mix and stir 2 h;2) add linking agent ethylene glycol dimethacrylate, mix and stir 10 min;3) add again initiator Diisopropyl azodicarboxylate, mix and stir 10 min, obtain mixed solution;4) by water-bath 72 h at 60 ℃ of above-mentioned mixed solution nitrogen flushing deoxidation 4 min, constant temperature, obtain bulk polymer;5) above-mentioned bulk polymer is ground, with sizing screen, screen and retain 60 order-100 purpose polymers particles, then polymer beads is passed through to the extracting of Soxhlet extract to remove unreacted reactant, the extracting time is 48 h, obtains molecularly imprinted polymer;6) by above-mentioned molecularly imprinted polymer, in temperature, be dry at 60 ℃, can make can enrichment bristle element molecularly imprinted polymer;In described pore-creating agent, the volume ratio of tetrahydrofuran (THF) and octane-iso is 5:1;The mol ratio of described template molecule, function monomer and linking agent is 1:5:35;The add-on of described initiator Diisopropyl azodicarboxylate is 0.25% of pore-creating agent, function monomer and linking agent total mass;Described Soxhlet extract is that volume ratio is the methyl alcohol of 9:1 and the mixed solution of acetic acid.
- As claimed in claim 1 method prepare can enrichment bristle element the application of molecularly imprinted polymer, it is characterized in that: for, enrichment separated from Phellinus bacterium to extract bristle element.
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| CN106179283B (en) * | 2016-08-05 | 2018-10-26 | 厦门大学 | One kind is based on quaternary ammonium type poly ion liquid adsorbent and preparation method thereof |
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