CN103570870A - Multi-template monodisperse active notoginsenoside molecular imprinted polymer and preparation method thereof - Google Patents
Multi-template monodisperse active notoginsenoside molecular imprinted polymer and preparation method thereof Download PDFInfo
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- 229920000344 molecularly imprinted polymer Polymers 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 229930189092 Notoginsenoside Natural products 0.000 title abstract 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 30
- 239000000178 monomer Substances 0.000 claims abstract description 29
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 28
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- 150000007949 saponins Chemical class 0.000 claims description 44
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- 230000000694 effects Effects 0.000 claims description 32
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- 229940089161 ginsenoside Drugs 0.000 claims description 23
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical group C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 16
- 241000180649 Panax notoginseng Species 0.000 claims description 15
- 235000003143 Panax notoginseng Nutrition 0.000 claims description 15
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 10
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 8
- GZYPWOGIYAIIPV-JBDTYSNRSA-N ginsenoside Rb1 Chemical group C([C@H]1O[C@H]([C@@H]([C@@H](O)[C@@H]1O)O)O[C@@](C)(CCC=C(C)C)[C@@H]1[C@@H]2[C@@]([C@@]3(CC[C@H]4C(C)(C)[C@@H](O[C@H]5[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O5)O[C@H]5[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O5)O)CC[C@]4(C)[C@H]3C[C@H]2O)C)(C)CC1)O[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O GZYPWOGIYAIIPV-JBDTYSNRSA-N 0.000 claims description 7
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 6
- STVZJERGLQHEKB-UHFFFAOYSA-N ethylene glycol dimethacrylate Substances CC(=C)C(=O)OCCOC(=O)C(C)=C STVZJERGLQHEKB-UHFFFAOYSA-N 0.000 claims description 6
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 4
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical group NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 4
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 4
- 238000004090 dissolution Methods 0.000 claims description 4
- VPJDULFXCAQHRC-UHFFFAOYSA-N prop-2-enylurea Chemical compound NC(=O)NCC=C VPJDULFXCAQHRC-UHFFFAOYSA-N 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- DBCAQXHNJOFNGC-UHFFFAOYSA-N 4-bromo-1,1,1-trifluorobutane Chemical group FC(F)(F)CCCBr DBCAQXHNJOFNGC-UHFFFAOYSA-N 0.000 claims description 3
- OKKRPWIIYQTPQF-UHFFFAOYSA-N Trimethylolpropane trimethacrylate Chemical compound CC(=C)C(=O)OCC(CC)(COC(=O)C(C)=C)COC(=O)C(C)=C OKKRPWIIYQTPQF-UHFFFAOYSA-N 0.000 claims description 3
- VVWRJUBEIPHGQF-UHFFFAOYSA-N propan-2-yl n-propan-2-yloxycarbonyliminocarbamate Chemical group CC(C)OC(=O)N=NC(=O)OC(C)C VVWRJUBEIPHGQF-UHFFFAOYSA-N 0.000 claims description 3
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 2
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 2
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 2
- 229920000642 polymer Polymers 0.000 abstract description 13
- 238000000034 method Methods 0.000 abstract description 7
- 230000006378 damage Effects 0.000 abstract description 3
- 239000004005 microsphere Substances 0.000 abstract description 3
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- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 1
- OZAIFHULBGXAKX-VAWYXSNFSA-N AIBN Substances N#CC(C)(C)\N=N\C(C)(C)C#N OZAIFHULBGXAKX-VAWYXSNFSA-N 0.000 description 1
- 241000590428 Panacea Species 0.000 description 1
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- 229940127219 anticoagulant drug Drugs 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a multi-template monodisperse active notoginsenoside molecular imprinted polymer and a preparation method thereof. The method comprises the following steps of mixing and dissolving template molecules and functional monomers into a pore-forming agent, performing uniform ultrasonic mixing to form a template molecule-functional monomer composite, adding an effective amount of initiator and an effective amount of cross-linking agent, and performing ultrasonic nitrogen introduction and sealing; placing a molecular imprinted polymer in a shaking incubator for polymerization reaction under the protection of nitrogen and thermal initiation; after the polymerization reaction is finished, eluting an obtained molecular imprinted polymer by using a methanol-glacial acetic acid to remove the template molecules, washing the molecular imprinted polymer to be neutral by using methanol, and performing vacuum drying to obtain the multi-template monodisperse active notoginsenoside molecular imprinted polymer. Prepared precipitated molecular imprinted polymer microspheres have the advantages of high monodispersity, uniform particle diameter, size controllability, simplicity in preparation, high yield and the like; damage to binding sites and imprinted cavities is reduced, and high affinity and high selectivity of the polymer to the template molecules are ensured.
Description
Technical field
The invention belongs to technical field of bioengineering, be specifically related to a kind of preparation method of molecularly imprinted polymer, relate in particular to a kind of multi-template list and disperse pseudo-ginseng activity saponin(e molecularly imprinted polymer and preparation method thereof.
Background technology
Pseudo-ginseng is the dry root and rhizome of panax araliaceae plant (Panax notoginseng (Burk.) F.H.Chen), there is enhancing body function, increase one of traditional valuable ingredient of traditional Chinese medicine of the effect ，Shi China such as coronary flow, vasodilation, reduction myocardial consumption of oxygen, anticoagulant, reduction blood viscosity.The main effective constituent of pseudo-ginseng is Panax Notoginseng saponin R
1, ginsenoside Rg
1with ginsenoside Rb
1, ginsenoside Rg wherein
1with ginsenoside Rb
1content higher.Because its effect is distinguished, praised highly by numerous doctors from ancient times, be described as the panacea of metal-inflicted wound cane sore, the chief component of have won fame both at home and abroad especially " Yunnan white powder ".Since 20 century 70s, people have carried out a large amount of research work to the chemical composition of pseudo-ginseng single medicinal material and compound thereof, pharmacological action, yet because pseudo-ginseng ingredient is complicated, and content is low, traditional separation method is as purifying pseudo-ginseng activity saponin(es such as polymeric adsorbent, gacs, step is various, complex operation, poor selectivity, separation efficiency is low and poor reproducibility, quality product is difficult to accurate control, having had a strong impact on clinical drug safety, is also the bottleneck problem that restricts at present the development of pseudo-ginseng injection.Therefore in the urgent need to a kind of novel method of high efficiency separation pseudo-ginseng activity saponin(e.
Molecular imprinting is the technology of imitating a kind of specific recognition target molecule of " Ag-Ab " recognition principle development.It take the molecule of wish identification is template, mode by key covalently or non-covalently and specific function monomer are combined generation polymkeric substance with linking agent, then use specific solvent by template molecule wash-out, obtain having molecularly imprinted polymer (the molecular imprinted polymers in specific recognition site, MIPs), thus template molecule and analog thereof are shown to the specific recognition performance of height.Because molecular imprinting is simple to operate, strong to the specific recognition capability of target molecule, in recent years in increasing field widespread use, and obtain good result.Application multi-template molecularly imprinted polymer carrys out the research of separation and purification pseudo-ginseng activity saponin(e, there is not yet bibliographical information.
Summary of the invention
The technical problem solving: the invention provides a kind of multi-template list and disperse pseudo-ginseng activity saponin(e molecularly imprinted polymer and preparation method thereof, thereby overcome the deficiency of existing separating and purifying technology, pseudo-ginseng activity saponin(e molecule be can adsorb simply, fast, specifically, selective separation, efficiently concentrating to chemical composition in pseudo-ginseng extract realized.
Technical scheme: multi-template list disperses pseudo-ginseng activity saponin(e molecularly imprinted polymer, is made by following steps:
1) by template molecule, function monomer mixed dissolution in pore-creating agent, ultrasonic mixing, standing 2～4h, forms template molecule-function monomer mixture, then adds initiator, the linking agent of significant quantity, ultrasonic 5～10min, logical nitrogen 5～10min, sealing; Wherein, the mol ratio of template molecule and function monomer is 1:2～1:6, and the mol ratio of function monomer and linking agent is 1:1～1:6; The volumetric usage of pore-creating agent is 25～150ml/mmol with the ratio of the molar weight of template molecule; The consumption of initiator is 3%～5% of template molecule, function monomer and linking agent total mass;
2) under nitrogen protection, molecularly imprinted polymer adopts thermal initiation, is placed in shaking culture case and carries out polyreaction, and incubator rotating speed is 100r/min～300r/min, and polymerization temperature is 50 ℃～70 ℃, and polymerization reaction time is 20～36h;
3) after polyreaction finishes, resulting molecularly imprinted polymer carries out wash-out with methyl alcohol-Glacial acetic acid, removes template molecule, then is washed till neutrality with methyl alcohol, then 45 ℃ of vacuum-drying 12～24h, obtain multi-template list and disperse pseudo-ginseng activity saponin(e molecularly imprinted polymer.
Multi-template list disperses the preparation method of pseudo-ginseng activity saponin(e molecularly imprinted polymer, and preparation process is:
1) by template molecule, function monomer mixed dissolution in pore-creating agent, ultrasonic mixing, standing 2～4h, forms template molecule-function monomer mixture, then adds initiator, the linking agent of significant quantity, ultrasonic 5～10min, logical nitrogen 5～10min, sealing; Wherein, the mol ratio of template molecule and function monomer is 1:2～1:6, and the mol ratio of function monomer and linking agent is 1:1～1:6; The volumetric usage of pore-creating agent is 25～150ml/mmol with the ratio of the molar weight of template molecule; The consumption of initiator is 3%～5% of template molecule, function monomer and linking agent total mass;
2) under nitrogen protection, molecularly imprinted polymer adopts thermal initiation, is placed in shaking culture case and carries out polyreaction, and incubator rotating speed is 100r/min～300r/min, and polymerization temperature is 50 ℃～70 ℃, and polymerization reaction time is 20～36h;
3) after polyreaction finishes, resulting molecularly imprinted polymer carries out wash-out with methyl alcohol-Glacial acetic acid, removes template molecule, then is washed till neutrality with methyl alcohol, then 45 ℃ of vacuum-drying 12～24h, obtain multi-template list and disperse pseudo-ginseng activity saponin(e molecularly imprinted polymer.
Described template molecule is ginsenoside Rb
1, ginsenoside Rg
1and Panax Notoginseng saponin R
1, three's mol ratio is 44:43:13.
Described function monomer is acrylamide, methacrylic acid, allyl urea or 4-vinylpridine.
Described initiator is Diisopropyl azodicarboxylate or benzoyl peroxide.
Described pore-creating agent is tetrahydrofuran (THF), DMF, acetonitrile, propyl carbinol, methyl alcohol or ethanol.
Described linking agent is ethylene glycol dimethacrylate or trimethylolpropane trimethacrylate.
The volume ratio of described methyl alcohol-glacial acetic acid solution is methyl alcohol: Glacial acetic acid=9:1.
Beneficial effect: one: the compound structure existing in pseudo-ginseng is closely similar, and content is low, it is large to disturb, and nonselective analysis of material is difficult to it to carry out separation and purification.The synthetic multi-template list of the present invention disperses high-affinity, highly selective separation that pseudo-ginseng activity saponin(e molecularly imprinted polymer is activeconstituents in medicinal material that possibility is provided.
Its two: the precipitation molecular blotting polymer microsphere that the present invention is prepared, compare with traditional body molecularly imprinted polymer, have that monodispersity is good, uniform particle diameter, size be controlled, preparation is simple, productive rate advantages of higher.And do not need to mill, the complicated last handling process such as sieve, has reduced the destruction in binding site and trace hole, has guaranteed that polymkeric substance is to the high-affinity of template molecule and highly selective.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope picture that the synthetic multi-template list of embodiment 3 disperses pseudo-ginseng activity saponin(e molecularly imprinted polymer, ■ MIP wherein, ● NIP;
Fig. 2 is the dynamic adsorption curve that the synthetic multi-template list of embodiment 3 disperses pseudo-ginseng activity saponin(e molecularly imprinted polymer, ■ MIP wherein, ● NIP;
Fig. 3 is the Static Adsorption curve that the synthetic multi-template list of embodiment 3 disperses pseudo-ginseng activity saponin(e molecularly imprinted polymer, ■ MIP wherein, ● NIP.
Embodiment
Below in conjunction with embodiment, the present invention will be further described.
Acrylamide (AM)
Allyl urea (AU)
Methacrylic acid (MAA)
4-vinylpridine (4-VP)
Trimethylolpropane trimethacrylate (TRIM)
Ethylene glycol dimethacrylate (EGDMA)
Tetrahydrofuran (THF) (THF)
DMF (DMF)
Diisopropyl azodicarboxylate (AIBN)
Embodiment 1:
By 348.5mg ginsenoside Rb
1, ginsenoside Rg
1and Panax Notoginseng saponin R
1mixture (three's mol ratio is 44:43:13) and 1.00mmol function monomer MAA be dissolved in 25mL DMF solvent, ultrasonic 10min dissolves, prepolymerization 2～4h.Add 6.00mmol linking agent EGDMA and 48.72mg initiator A IBN, ultrasonic 10min dissolves again.Mixed solution leads to nitrogen 10min, and constant-temperature table is warming up to 60 ℃, 300rpm polymerization 24h.
Centrifugal collection is also carried out wash-out (v/v with methyl alcohol-Glacial acetic acid, 9:1), remove template molecule, until uv-spectrophotometric instrument can not detect template molecule at 204nm place, with methyl alcohol, be washed till neutrality again, then 45 ℃ of vacuum-drying 12h, obtain multi-template list and disperse pseudo-ginseng activity saponin(e molecularly imprinted polymer (MIP-1).
Except in building-up process, do not add template molecule Panax Notoginseng saponin R
1, ginsenoside Rg
1with ginsenoside Rb
1in addition, all the other steps are all identical with imprinted polymer preparation process, obtain non-imprinted polymer (NIP-1).
Embodiment 2:
By 348.5mg ginsenoside Rb
1, ginsenoside Rg
1and Panax Notoginseng saponin R
1mixture (three's mol ratio is 44:43:13) and 1.50mmol function monomer AU be dissolved in 30mL THF solvent, ultrasonic 10min dissolves, prepolymerization 2～4h.Add 6.00mmol linking agent TRIM and 75.88mg initiator A IBN, ultrasonic 5min dissolves again.Mixed solution leads to nitrogen 10min, and constant-temperature table is warming up to 50 ℃, 200rpm polyase 13 6h.
Centrifugal collection is also carried out wash-out (v/v with methyl alcohol-Glacial acetic acid, 9:1), remove template molecule, until uv-spectrophotometric instrument can not detect template molecule at 204nm place, with methyl alcohol, be washed till neutrality again, then 45 ℃ of vacuum-drying 24h, obtain multi-template list and disperse pseudo-ginseng activity saponin(e molecularly imprinted polymer (MIP-2).
Except in building-up process, do not add template molecule Panax Notoginseng saponin R
1, ginsenoside Rg
1beyond ginsenoside Rb, all the other steps are all identical with imprinted polymer preparation process, obtain non-imprinted polymer (NIP-2)..
Embodiment 3:
By 348.5mg ginsenoside Rb
1, ginsenoside Rg
1and Panax Notoginseng saponin R
1mixture (three's mol ratio is 44:43:13) and 2.00mmol function monomer AM be dissolved in 40mL alcohol solvent, ultrasonic 10min dissolves, prepolymerization 2～4h.Add 10.00mmol linking agent EGDMA and 74.20mg initiator A IBN, ultrasonic 10min dissolves again.Mixed solution leads to nitrogen 10min, and constant-temperature table is warming up to 60 ℃, 200rpm polymerization 24h.
Centrifugal collection is also carried out wash-out (v/v with methyl alcohol-Glacial acetic acid, 9:1), remove template molecule, until uv-spectrophotometric instrument can not detect template molecule at 204nm place, with methyl alcohol, be washed till neutrality again, then 45 ℃ of vacuum-drying 24h, obtain multi-template list and disperse pseudo-ginseng activity saponin(e molecularly imprinted polymer (MIP-3).
Except in building-up process, do not add template molecule Panax Notoginseng saponin R
1, ginsenoside Rg
1with ginsenoside Rb
1in addition, all the other steps are all identical with imprinted polymer preparation process, obtain non-imprinted polymer (NIP-3).
Embodiment 4:
By 348.5mg ginsenoside Rb
1, ginsenoside Rg
1and Panax Notoginseng saponin R
1mixture (three's mol ratio is 44:43:13) and 2.00mmol function monomer 4-VP be dissolved in 50mL alcohol solvent, ultrasonic 10min dissolves, prepolymerization 2～4h.Add 9.00mmol linking agent TRIM and 180.21mg initiator A IBN, ultrasonic 10min dissolves again.Mixed solution leads to nitrogen 5min, and constant-temperature table is warming up to 70 ℃, 100rpm polyase 13 6h.
Centrifugal collection is also carried out wash-out (v/v with methyl alcohol-Glacial acetic acid, 9:1), remove template molecule, until uv-spectrophotometric instrument can not detect template molecule at 204nm place, with methyl alcohol, be washed till neutrality again, then 45 ℃ of vacuum-drying 12h, obtain multi-template list and disperse pseudo-ginseng activity saponin(e molecularly imprinted polymer (MIP-4).
Except in building-up process, do not add template molecule Panax Notoginseng saponin R
1, ginsenoside Rg
1with ginsenoside Rb
1in addition, all the other steps are all identical with imprinted polymer preparation process, obtain non-imprinted polymer (NIP-4).
Test implementation example:
Get molecularly imprinted polymer synthetic in above-described embodiment 3 and non-imprinted polymer carries out following test experiments.
Test implementation example 1. transmission electron microscopes
Fig. 1 is the transmission electron microscope picture that the synthetic multi-template list of the present invention disperses pseudo-ginseng activity saponin(e molecularly imprinted polymer, visible, the imprinted polymer microballoon epigranular of preparation, and monodispersity is good.
Test implementation example 2. dynamic adsorption tests
Precision takes MIP and NIP(20.0mg) each 5 parts, be placed in 15mL triangular flask, be dispersed in respectively 5mL, the Panax Notoginseng saponin R of 2.5mmol/L
1, ginsenoside Rg
1with ginsenoside Rb
1alcohol mixed solution in, room temperature jolting.Respectively 1,2,3,4 and get supernatant liquor during 5h, 0.22 μ m nylon membrane filters, and gets subsequent filtrate dilution constant volume, and spectrophotometry instrument is measured the concentration of absorption front and back sample in 204nm place, calculate equilibrium adsorption capacity Qe, parallel running three times according to formula (1).
In formula: C
0and C
ebe respectively initial concentration and the equilibrium concentration (mmol/L) of template molecule; V is the volume (mL) of adsorbent solution; M is the quality (g) of imprinted polymer.
As can be seen from Figure 2, along with the increase of adsorption time, imprinted material constantly rises to the adsorptive capacity of microsphere, substantially reaches adsorption equilibrium after 4h.Experiment shows, imprinted material has adsorption rate faster, and MIP time of equilibrium adsorption prepared by traditional mass polymerization is generally 12～24h.Its reason is that the present invention adopts that the synthetic molecularly imprinted polymer monodispersity of precipitation polymerization is good, uniform particle diameter, imprinted sites are evenly distributed, and the destruction of imprinted sites while having avoided mass polymerization to grind.
The 3. Static Adsorption tests of test implementation example
Precision takes MIP and NIP(20.0mg) each 5 parts, be placed in 15mL triangular flask, add respectively 1.0mmol/L, 1.5mmol/L, 2.0mmol/L, 2.5mmol/L and 3.0mmol/L Panax Notoginseng saponin R
1, ginsenoside Rg
1with ginsenoside Rb
1alcohol mixed solution 5mL, ultrasonic dispersion, room temperature jolting 4h, get supernatant liquor, 0.22 μ m nylon membrane filters, and gets subsequent filtrate dilution constant volume, spectrophotometry instrument is measured the concentration of each sample in 204nm place, calculate equilibrium adsorption capacity Qe, parallel running three times according to formula (1).
As can be seen from Figure 3, the maximal absorptive capacity of MIP, much larger than NIP, shows that MIP is to Panax Notoginseng saponin R
1, ginsenoside Rg
1with ginsenoside Rb
1absorption be different from physical adsorption, but a kind of selective adsorption that has specific recognition site, this molecular recognition characteristic comes from hydrogen bond action between the conjugated group of this polymkeric substance and the function base of template molecule and the geometry selectivity in hole.
Above-mentioned example is only explanation technical conceive of the present invention and feature, and its object is to allow person skilled in the art can understand content of the present invention and implement according to this, can not limit the scope of the invention with this.All equivalent transformations that spirit is done according to the present invention or modification, within all should being encompassed in protection scope of the present invention.
Claims (8)
1. multi-template list disperses pseudo-ginseng activity saponin(e molecularly imprinted polymer, it is characterized in that being made by following steps:
1) by template molecule, function monomer mixed dissolution in pore-creating agent, ultrasonic mixing, standing 2～4 h, form template molecule-function monomer mixture, then add initiator, the linking agent of significant quantity, ultrasonic 5～10 min, logical nitrogen 5～10 min, sealing; Wherein, the mol ratio of template molecule and function monomer is 1:2～1:6, and the mol ratio of function monomer and linking agent is 1:1～1:6; The volumetric usage of pore-creating agent is 25～150 ml/mmol with the ratio of the molar weight of template molecule; The consumption of initiator is 3% ~ 5% of template molecule, function monomer and linking agent total mass;
2) under nitrogen protection, molecularly imprinted polymer adopts thermal initiation, is placed in shaking culture case and carries out polyreaction, and incubator rotating speed is 100 r/min～300 r/min, and polymerization temperature is 50 ℃～70 ℃, and polymerization reaction time is 20～36 h;
3) after polyreaction finishes, resulting molecularly imprinted polymer carries out wash-out with methyl alcohol-Glacial acetic acid, removes template molecule, then is washed till neutrality with methyl alcohol, then 45 ℃ of vacuum-drying 12～24 h, obtain multi-template list and disperse pseudo-ginseng activity saponin(e molecularly imprinted polymer.
2. multi-template list disperses the preparation method of pseudo-ginseng activity saponin(e molecularly imprinted polymer, it is characterized in that preparation process is:
1) by template molecule, function monomer mixed dissolution in pore-creating agent, ultrasonic mixing, standing 2～4 h, form template molecule-function monomer mixture, then add initiator, the linking agent of significant quantity, ultrasonic 5～10 min, logical nitrogen 5～10 min, sealing; Wherein, the mol ratio of template molecule and function monomer is 1:2～1:6, and the mol ratio of function monomer and linking agent is 1:1～1:6; The volumetric usage of pore-creating agent is 25～150 ml/mmol with the ratio of the molar weight of template molecule; The consumption of initiator is 3% ~ 5% of template molecule, function monomer and linking agent total mass;
2) under nitrogen protection, molecularly imprinted polymer adopts thermal initiation, is placed in shaking culture case and carries out polyreaction, and incubator rotating speed is 100 r/min～300 r/min, and polymerization temperature is 50 ℃～70 ℃, and polymerization reaction time is 20～36 h;
3) after polyreaction finishes, resulting molecularly imprinted polymer carries out wash-out with methyl alcohol-Glacial acetic acid, removes template molecule, then is washed till neutrality with methyl alcohol, then 45 ℃ of vacuum-drying 12～24 h, obtain multi-template list and disperse pseudo-ginseng activity saponin(e molecularly imprinted polymer.
3. multi-template list disperses the preparation method of pseudo-ginseng activity saponin(e molecularly imprinted polymer according to claim 2, it is characterized in that: described template molecule is ginsenoside Rb
1, ginsenoside Rg
1and Panax Notoginseng saponin R
1, three's mol ratio is 44:43:13.
4. multi-template list disperses the preparation method of pseudo-ginseng activity saponin(e molecularly imprinted polymer according to claim 2, it is characterized in that: described function monomer is acrylamide, methacrylic acid, allyl urea or 4-vinylpridine.
5. multi-template list disperses the preparation method of pseudo-ginseng activity saponin(e molecularly imprinted polymer according to claim 2, it is characterized in that: described initiator is Diisopropyl azodicarboxylate or benzoyl peroxide.
6. multi-template list disperses the preparation method of pseudo-ginseng activity saponin(e molecularly imprinted polymer according to claim 2, it is characterized in that: described pore-creating agent is tetrahydrofuran (THF), DMF, acetonitrile, propyl carbinol, methyl alcohol or ethanol.
7. multi-template list disperses the preparation method of pseudo-ginseng activity saponin(e molecularly imprinted polymer according to claim 2, it is characterized in that: described linking agent is ethylene glycol dimethacrylate or trimethylolpropane trimethacrylate.
8. multi-template list disperses the preparation method of pseudo-ginseng activity saponin(e molecularly imprinted polymer according to claim 2, it is characterized in that: the volume ratio of described methyl alcohol-glacial acetic acid solution is methyl alcohol: Glacial acetic acid=9:1.
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| CN104371067A (en) * | 2014-10-31 | 2015-02-25 | 南华大学 | Imprinting material with high capacity of recognizing icariin and preparation method thereof |
| CN104710567A (en) * | 2015-03-23 | 2015-06-17 | 山东省分析测试中心 | Preparation method and application of molecularly imprinted polymer for extracting dencichine |
| CN105330782A (en) * | 2015-12-10 | 2016-02-17 | 新疆农垦科学院 | Oleanic acid molecularly imprinted polymer based on computer simulation and preparation method thereof and application |
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| CN1473862A (en) * | 2002-05-10 | 2004-02-11 | 北京化工大学 | Print separating method of natural product with cyclodextrin molecule |
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| CN104710567A (en) * | 2015-03-23 | 2015-06-17 | 山东省分析测试中心 | Preparation method and application of molecularly imprinted polymer for extracting dencichine |
| CN104710567B (en) * | 2015-03-23 | 2016-10-05 | 山东省分析测试中心 | A kind of preparation method and application of the molecularly imprinted polymer for extracting dencichine |
| CN105330782A (en) * | 2015-12-10 | 2016-02-17 | 新疆农垦科学院 | Oleanic acid molecularly imprinted polymer based on computer simulation and preparation method thereof and application |
| CN107703073A (en) * | 2017-09-25 | 2018-02-16 | 云南金七制药有限公司 | A kind of effective substance method of the oral liquid prepared with Radix Notoginseng extract |
| CN107805270A (en) * | 2017-10-30 | 2018-03-16 | 江苏吉生源生物科技有限公司 | A kind of ginsenoside Rh2Extracting method |
| CN109354649A (en) * | 2018-11-06 | 2019-02-19 | 北京农学院 | A kind of preparation method and applications of kresoxim-methyl class molecularly imprinted polymer |
| CN109354649B (en) * | 2018-11-06 | 2021-02-02 | 北京农学院 | Preparation method and application of kresoxim-methyl molecularly imprinted polymer |
| CN110437375A (en) * | 2019-07-08 | 2019-11-12 | 陕西中医药大学 | A kind of molecularly imprinted polymer and preparation method thereof isolating and purifying panax japonicus saponin IVa |
| CN110437375B (en) * | 2019-07-08 | 2021-04-30 | 陕西中医药大学 | Molecularly imprinted polymer for separating and purifying panax japonicus saponin IVa and preparation method thereof |
| CN110669093A (en) * | 2019-09-11 | 2020-01-10 | 江苏吉生源生物科技有限公司 | Method for extracting ginsenoside Rg3 |
| CN111205393A (en) * | 2020-03-06 | 2020-05-29 | 辽宁科技大学 | Imprinted polymeric material for adsorbing and separating ginsenoside Rd and preparation method thereof |
| CN111205393B (en) * | 2020-03-06 | 2021-12-17 | 辽宁科技大学 | Imprinted polymeric material for adsorbing and separating ginsenoside Rd and preparation method thereof |
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