CN102174138B - Preparation method and application of codonopsis lactone molecularly imprinted solid phase extraction column - Google Patents
Preparation method and application of codonopsis lactone molecularly imprinted solid phase extraction column Download PDFInfo
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- CN102174138B CN102174138B CN 201110027123 CN201110027123A CN102174138B CN 102174138 B CN102174138 B CN 102174138B CN 201110027123 CN201110027123 CN 201110027123 CN 201110027123 A CN201110027123 A CN 201110027123A CN 102174138 B CN102174138 B CN 102174138B
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Abstract
The invention discloses a preparation method and application of a molecularly imprinted polymer which is used for directly and directionally extracting and separating codonopsis lactone from extraction solution of codonopsis which is a Chinese medicinal herb. The polymer can be used as a filler to be made into a solid-phase extraction column used for extracting and separating codonopsis lactone from the extraction solution of a Chinese medicinal herb. Compared with a C18 bonded solid-phase extraction column and a silica gel solid-phase extraction column, the codonopsis lactone molecularly imprinted solid phase extraction column has better selectivity to the codonopsis lactone in the extraction solution, has higher capacity of up to 8. 6 mumol/g, is two to three times the capacity of both the C18 bonded solid-phase extraction column silica and the gel solid-phase extraction column, and also has elution rate of 93% higher than the C18 bonded solid-phase extraction column silica and the gel solid-phase extraction column. The method used for extracting and separating the codonopsis lactone ensures that the prepared product has high purity, is easy to operate and realize industrialization, adopts less solvent, is safer and more environmental friendly and can achieve the purposes of removing impurities, purifying and enriching the codonopsis lactone.
Description
Technical field:
What patent of the present invention related to is the technical field of Polymer Synthesizing and application in active ingredient of Chinese herbs separates thereof, and being specifically related to the preparation of codonolactone's molecularly imprinted polymer and utilizing this polymkeric substance is the method for the codonolactone in solid extracting agent separation, the purifying natural product.
Background technology:
(1) Radix Codonopsis, the dry root of Campanulaceae Radix Codonopsis Codonopsis pilosula (Franch.) Nannf., element flower Radix Codonopsis Codonopsis pilosula Nannf.var.modesta (Nannf.) L.T.Shen or radix codonpsis tangshen Codonpsistangshen Oliv..Codonolactone is that it mainly contains effective constituent, has strengthening immunity, vasodilation, step-down, improves microcirculation, strengthens the effects such as hemopoietic function.
(2) the herbal medicine ingredient is very complicated, and existing effective constituent has again invalid components and toxic ingredient.In order to improve the result for the treatment of of herbal medicine, will use up to greatest extent extracting effective components, remove invalid components and toxic ingredient.Therefore, herbal medicine activeconstituents separation and Extraction is all very important for the inner quality and the clinical efficacy that improve Chinese medicine preparation.The separation and Extraction of traditional Chinese medicine activeconstituents often adopts silicagel column, C
18Bonding phase column, Al
2O
3Posts etc. utilize the adsorption index difference of composition to realize separating, but disadvantage is poor selectivity, the enrichment capacity is low, especially to some complex structures, many chiral carbon atoms, and the low active compound of content, the separating-purifying difficulty is large, adopt these conventional separation means often to need repeatable operation, extraction yield is extremely low, and therefore chiral configuration may change and inactivation.Molecularly imprinted polymer is the high molecular polymer of making to measure for template molecule, because it is behind the wash-out template molecule, can stay the hole that all is complementary with template molecule at shape, size and recognition site, and this cavity energy again recognition template divides.Because it has concurrently efficiently, stable and specific selectivity and synthetic cheap, thereby has than wide application prospect.
Summary of the invention:
The object of the invention is to avoid the problem of above-mentioned traditional extraction process technology existence, setting up a kind of is the Novel adsorption parting material based on codonolactone's molecularly imprinted polymer, and with this method of doing stationary phase directional separation, enrichment, purifying codonolactone from the Chinese medicine crude extract of solid-phase extraction column, can obtain thus the target component of high extraction.The present invention realizes by following technical scheme, comprises that specifically step is as follows:
1. the preparation of codonolactone's molecularly imprinted polymer:
(1) be dissolved in codonolactone, function monomer and linking agent in the round-bottomed flask that 68mL pore-creating agent acetonitrile solution is housed at 1: 4: 20 according to mol ratio;
(2) add again initiator Diisopropyl azodicarboxylate 78mg after, logical nitrogen deoxidation 15min;
(3) round-bottomed flask of good seal is put into 60 ℃ water-bath, constant temperature polymerization 24h obtains polymkeric substance;
(4) polymkeric substance that makes is used methyl alcohol-Glacial acetic acid (9: 1, V/V) mixed solution is extraction agent, the method flush away template molecule that extracts by Soxhlet and function monomer and the linking agent that does not have polymerization, check until till can't detect the absorption of above material, then remove residual Glacial acetic acid with methyl alcohol with UV spectrum;
(5) polymkeric substance that will remove template molecule obtains codonolactone's molecularly imprinted polymer at 60 ℃ of dry 2h;
(6) preparation method of non-imprinted polymer, except not adding the template molecule, all the other steps are the same.
2. the codonolactone in the Solid phase extraction separation purifying Chinese medicine crude extract:
(1) codonolactone in the Solid phase extraction separation purifying Chinese medicine crude extract: take by weighing codonopsis pilosula powder (crossing 50 mesh sieves) 5.0g, add methanol extract liquid 40mL, behind the immersion 1h, after putting into the ultrasonic 40min of ultrasonic wave, rotary evaporated to dryness, with dissolve with methanol and be settled to 5mL, for subsequent use;
(2) adopt dry column-packing to be filled in the solid-phase extraction column codonolactone obtained above molecularly imprinted polymer, and with methanol solution balance pillar; After getting codonopsis pilosula crude extract 5mL loading, be retained in codonolactone in the column extractor with methanol-eluted fractions, elutriant collected and concentrated, dry, namely obtain highly purified codonolactone.
The molecularly imprinted polymer pattern of the present invention's preparation is regular spherical and single the dispersion, about particle diameter 5 μ m, codonolactone is had good recognition performance, as the filler of Solid-Phase Extraction, can be used for high efficiency separation, enrichment and the purifying of codonolactone's composition in the Chinese medicine.
With C
18The bonding solid-phase extraction column, silica gel solid-phase extraction column and Al
2O
3Solid-phase extraction column is compared, and the Radix Codonopsis molecularly imprinted solid phase extraction column has better selectivity to the codonolactone in the extracting solution, and column capacity is the highest, reaches 8.6 μ mol/g, is C
18The 2-3 of bonding solid-phase extraction column and silica gel solid-phase extraction column times, Al
2O
310 times of solid-phase extraction column.Eluting rate reaches 93% simultaneously, also is higher than other sorbent material solid-phase extraction column.
Description of drawings:
Accompanying drawing 1 is the synthetic schematic diagram of codonolactone's molecularly imprinted polymer, show between codonolactone and the function monomer 1-vinyl imidazole by hydrogen bond generation Intermolecular Forces, linking agent is behind polymerization reaction take place under the initiator thermal initiation, fixed the mixture that codonolactone and 1-vinyl imidazole form, stay the cavity of action site behind the wash-out template molecule, obtain imprinted polymer; Fig. 2 is the form electron-microscope scanning figure of polymer particles, amplifies 6000 times, and particle diameter is about 5 μ m.
Embodiment:
The below elaborates to embodiments of the invention: the present embodiment is implemented under take technical solution of the present invention as prerequisite, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1:
1. the preferred preparation method of codonolactone's molecularly imprinted polymer: the 0.6mmol of codonolactone; function monomer 1-vinyl imidazole 2.4mmol and linking agent DVB-80 12mmol mix; be dissolved in the round-bottomed flask that 61mL pore-creating agent acetonitrile liquid is housed; add initiator A IBN 78mg; logical nitrogen deoxidation 15min, rapidly sealing under nitrogen protection.After the test tube of good seal being put into 60 ℃ water-bath constant temperature polymerization 24h, obtain polymkeric substance.Polymkeric substance is put into cable type extractor according, with methyl alcohol-Glacial acetic acid (9: 1, V/V) mixed solution wash-out template molecule and do not have function monomer and the linking agent of polymerization is used the residual Glacial acetic acid of methyl alcohol flush away again, at 60 ℃ of dry 2h, obtain codonolactone's molecularly imprinted polymer.
2. the codonolactone in the Solid phase extraction separation purifying Chinese medicine crude extract:
Take by weighing Radix Codonopsis powder 5.0g, add people's methanol solution 40ml, put into the ultrasonic 40min of ultrasonic wave after, weigh and supply weight with methyl alcohol, filter and namely to get the Radix Codonopsis crude extract.Take by weighing the good codonolactone's imprinted polymer of 200mg wash-out, adopt dry column-packing, after adding successively methyl alcohol and 40% methanol solution balance solid-phase extraction column, get Radix Codonopsis crude extract 5mL, loading, pressurize in post, coutroi velocity is 0.5mL/min, is retained in codonolactone on the column extractor with 10mL methanol solution wash-out again.Obtain the 1.6mg of codonolactone through concentrated, drying.
Claims (2)
1. codonolactone's molecularly imprinted polymer solid-phase extraction column, it is characterized in that and can obtain by following steps: at first with codonolactone, function monomer and linking agent in molar ratio 1: 3-5: 20 are dissolved in the round-bottomed flask that the pore-creating agent acetonitrile solution is housed, add the initiator Diisopropyl azodicarboxylate, polymerization 24h in 60 ℃ of water-baths; The method flush away template molecule that reacted polymkeric substance extracts by Soxhlet through methyl alcohol-glacial acetic acid solution and unreacted be reagent completely, check with UV spectrum, until can't detect till the absorption of above material, use again the residual Glacial acetic acid of methyl alcohol flush away, obtain codonolactone's molecularly imprinted polymer; Fill it in the Solid-Phase Extraction void column, namely get codonolactone's molecularly imprinted solid phase extraction column; The function monomer that codonolactone's molecularly imprinted polymer preparation is adopted is the 1-vinyl imidazole, and linking agent is Vinylstyrene.
2. codonolactone according to claim 1 molecularly imprinted solid phase extraction column, template molecule and what do not have that linking agent, function monomer and the initiator of polymerization adopt is the mixed solution of methyl alcohol-Glacial acetic acid in the eccysis polymkeric substance, volume ratio is 9: 1.
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| CN102775554B (en) * | 2012-07-06 | 2014-12-03 | 江南大学 | Preparation method for cinnamaldehyde surface molecularly imprinted polymer |
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| CN101012294A (en) * | 2007-02-09 | 2007-08-08 | 华南师范大学 | Method of preparing benzodiazepines pharmaceutical molecular engram solid phase extractant |
| CN101092490A (en) * | 2007-06-28 | 2007-12-26 | 上海交通大学 | Method for preparing polymer microballons of molecular engram of nitrogen benzyl penicillin |
| CN101445576A (en) * | 2008-12-30 | 2009-06-03 | 南京医科大学 | Preparation method for puerarin imprinted polymer and application thereof in puerarin purification |
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| CN101012294A (en) * | 2007-02-09 | 2007-08-08 | 华南师范大学 | Method of preparing benzodiazepines pharmaceutical molecular engram solid phase extractant |
| CN101092490A (en) * | 2007-06-28 | 2007-12-26 | 上海交通大学 | Method for preparing polymer microballons of molecular engram of nitrogen benzyl penicillin |
| CN101445576A (en) * | 2008-12-30 | 2009-06-03 | 南京医科大学 | Preparation method for puerarin imprinted polymer and application thereof in puerarin purification |
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