CN1265195C - Ethylene equol molecular engram solid phase extracting small pole and its its prepn process - Google Patents
Ethylene equol molecular engram solid phase extracting small pole and its its prepn process Download PDFInfo
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- CN1265195C CN1265195C CN 200410046861 CN200410046861A CN1265195C CN 1265195 C CN1265195 C CN 1265195C CN 200410046861 CN200410046861 CN 200410046861 CN 200410046861 A CN200410046861 A CN 200410046861A CN 1265195 C CN1265195 C CN 1265195C
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- diethylstilbestrol
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- molecular engram
- polymer
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Abstract
The present invention discloses a diethylstilbestrol molecular engram solid-phase extracting small pole for measuring the high-selectivity purification and enrichment of the sample solutions of the residual amount of artificial synthetic estrogen diethylstilbestrol in animal foods, and a preparation method thereof. The diethylstilbestrol is used as a molecule template to prepare a molecular engram polymer which is a cross-linked polymer with fixed hole size and shape and definite arranged function groups. The molecular engram polymer also has a memory function on the stereo structure of the diethylstilbestrol template molecule and is filled into a small polypropylene pole to obtain the diethylstilbestrol molecular engram solid-phase extracting small pole which is used for the high-selectivity separation and enrichment of the diethylstilbestrol in the residual analysis sample solutions. Compared with a common solvent extraction method and a C18 solid-phase extraction method, the engram pole has the advantages of simplicity, high speed and high efficiency.
Description
Technical field
The present invention relates to the analytical chemistry field, specifically be applied to measure the high selectivity purifying of the sample solution of synthetic estrogen diethylstilbestrol (DES) residual quantity in the animal food, diethylstilbestrol molecular imprinted solid phase extraction cartridge of enrichment and preparation method thereof.
Background technology
(Diethylstilbestrol DES) is a kind of synthetic estrogen with phenolic hydroxyl structure to diethylstilbestrol, and many countries such as America and Europe forbid using it in the animal feed.Because the abuse of diethylstilbestrol, the residue detection of diethylstilbestrol in the animal food has been caused great attention both domestic and external.If measure in accordance with regulations, the residual situation of diethylstilbestrol is in animal tissue and the body fluid: the concentration in muscle, fat is very low, usually＜0.5 μ g/kg, the concentration in the liver＜2 μ g/kg, though concentration is the highest in excreta and the bile, also has only 0.5～20 μ g/kg.In order to make low concentration sample influential on detecting device, be necessary sample is carried out the enrichment of DES with concentrated.Under the usual conditions, extract DES with organic solution and can obtain the good recovery, but also extracted a large amount of liposoluble substances simultaneously, be difficult for separating, want extraction with NaOH with DES, but NaOH again with fatty acid generation saponification.Directly extract again less than the good recovery with rare NaOH solution.The Solid-Phase Extraction method is a kind of simple, convenient, suitable pre-service.But C
18Solid phase extraction column can not well separate DES and fat.
Summary of the invention
The object of the present invention is to provide and a kind ofly can simply, fast, efficiently measure the high selectivity purifying of the sample solution of synthetic estrogen diethylstilbestrol (DES) residual quantity in the animal food and diethylstilbestrol molecular imprinted solid phase extraction cartridge of enrichment and preparation method thereof.
Technical scheme of the present invention is achieved in that
(1) diethylstilbestrol molecular imprinted solid phase extraction cartridge: be to be filled in the pillar of polypropylene shell with diethylstilbestrol (DES) the microsphere polymkeric substance 0.2～1.0g that is ground to 10～60 μ m.
(2) preparation method of diethylstilbestrol molecular imprinted solid phase extraction cartridge: may further comprise the steps
(1). the preparation of diethylstilbestrol (DES) microsphere polymkeric substance:
With polymer raw template molecule stilbestrol Diethylstilbestrol (DES), function monomer methacrylic acid (MAA), crosslinking chemical Ethylene glycol dimethacrylate (EDMA), press template molecule: function monomer: crosslinking chemical=1～5: 4～10: 20～100, join in the round-bottomed flask successively, add initiating agent azoisobutyronitrile (AIBN), pore-foaming agent ethanol, chloroform, ether etc. again, ultrasonic 5～30min, logical nitrogen 5～40min, vacuum is reacted 5～48h in 40～90 ℃ of water-baths;
(2) the microsphere polymkeric substance is ground to about 10～60 μ m, uses V
(acetic acid)/ V
(ethanol)=5～30: 95～70 flushings, tiny particle is removed in the acetone sedimentation;
(3) the quality 0.2～1.0g of weighing molecularly imprinted polymer;
(4) be filled in the pillar of polypropylene shell;
Because diethylstilbestrol (DES) microsphere polymkeric substance is a kind of cross-linked polymer that fixing hole size and shape is arranged and the functional group of determining arrangement is arranged, it is to the spatial structure tool of the DES template molecule back of the body " memory " function, can be applicable to be used for measure high selectivity purifying, the enrichment of the sample solution of animal food synthetic estrogen diethylstilbestrol (DES) residual quantity.
This trace post is more simple, quick, efficient than usual vehicle extraction, C18 solid phase extraction.The pillar of selection polypropylene material shell helps the last DES solid phase extraction column that obtains can carry out online fast purification, elution in microwave cavity, and forms integrated on-line system with chromatographic fractionation system.
Embodiment
Below the invention will be further described by embodiment.
Embodiment 1:
(1). the preparation of diethylstilbestrol (DES) microsphere polymkeric substance:
The reaction raw materials tabulation
| Reaction reagent | Molecular weight (g/mol) | The reaction consumption | |||
| Molar weight (mmol) | Quality (g) | Actual amount | |||
| Diethylstilbestrol DES methacrylic acid MAA Ethylene glycol dimethacrylate EDMA azoisobutyronitrile AIBN | 268.4 68.01 198.22 164.21 | 0.50 2.0 10.0 0.12 | 0.134 0.136 1.687 19.7 | 270mg 0.136ml 2.0ml 19.7g | |
| Pore-foaming agent | The above-mentioned three kinds of liquid of acetonitrile chloroform ether | 6ml 6ml 6ml 6ml | |||
Successively join in round-bottomed flask by the consumption of above table reaction reagent Diethylstilbestrol (MES), methacrylic acid (MAA), Ethylene glycol dimethacrylate (EDMA), azoisobutyronitrile (AIBN), pore-foaming agent, ultrasonic 15min, logical nitrogen 5min, sealing, 60 ℃ of water-baths, 24h.
(2), the preparation of diethylstilbestrol molecular imprinted solid phase extraction cartridge
The microsphere polymkeric substance is ground to about 26 μ m, uses V
(acetic acid)/ V
(ethanol)=10: 90 flushings, tiny particle is removed in the acetone sedimentation, obtains particle diameter in a certain interval
3, the quality 0.2～1.0g of weighing microsphere polymkeric substance;
4, the microsphere polymkeric substance is filled in the solid phase pillar
(3) the diethylstilbestrol molecular imprinted solid phase extraction cartridge is used for measuring high selectivity purifying, the enrichment of the sample solution of animal food synthetic estrogen diethylstilbestrol (DES) residual quantity.
Concrete operations are as follows:
(1) earlier with the pillar washed with methanol,
(2) add sample solution 1.5ml;
(3) elute soln is the mixed solution of methyl alcohol, second alcohol and water, and the ratio of organic solvent and water is 0.5～4: 1.The effluent volume scope is at 2～10 pillar volumes.
Claims (2)
1. diethylstilbestrol molecular imprinted solid phase extraction cartridge, it comprises: the pillar of polypropylene shell, and 0.2～1.0g is filled in diethylstilbestrol (DES) the microsphere polymkeric substance in the described pillar, it is characterized in that described molecularly imprinted polymer is with polymer raw template molecule diethylstilbestrol, function monomer methacrylic acid (MAA), crosslinking chemical Ethylene glycol dimethacrylate (EDMA), by template molecule: function monomer: crosslinking chemical=1～5: 4～10: 20～100 are polymerized, and are ground to 10～60 μ m.
2. the preparation method of diethylstilbestrol molecular imprinted solid phase extraction cartridge is characterized in that may further comprise the steps:
(1). the preparation of diethylstilbestrol (DES) microsphere polymkeric substance:
With polymer raw template molecule diethylstilbestrol Diethylstilbestrol (DES), function monomer methacrylic acid (MAA), crosslinking chemical Ethylene glycol dimethacrylate (EDMA), press template molecule: function monomer: crosslinking chemical=1～5: 4～10: 20～100, join in the round-bottomed flask successively, add initiating agent azoisobutyronitrile (AIBN), pore-foaming agent ethanol, chloroform, ether again, ultrasonic 5～30min, logical nitrogen 5～40min, vacuum is reacted 5～48h in 40～90 ℃ of water-baths;
(2) the microsphere polymkeric substance is ground to about 10～60 μ m, uses V
(acetic acid)/ V
(ethanol)The solution flushing of=5～30: 95～70 preparations, tiny particle is removed in the acetone sedimentation;
(3) weighing molecularly imprinted polymer 0.2～1.0g;
(4) described molecularly imprinted polymer is filled in the pillar of polypropylene shell.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410046861 CN1265195C (en) | 2004-10-26 | 2004-10-26 | Ethylene equol molecular engram solid phase extracting small pole and its its prepn process |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410046861 CN1265195C (en) | 2004-10-26 | 2004-10-26 | Ethylene equol molecular engram solid phase extracting small pole and its its prepn process |
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| CN1265195C true CN1265195C (en) | 2006-07-19 |
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| CN 200410046861 Expired - Fee Related CN1265195C (en) | 2004-10-26 | 2004-10-26 | Ethylene equol molecular engram solid phase extracting small pole and its its prepn process |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100374860C (en) * | 2006-02-16 | 2008-03-12 | 上海交通大学 | Process for producing chloromycetin molecular engram solid phase extraction small column |
| CN100382869C (en) * | 2006-03-13 | 2008-04-23 | 中山大学 | Molecular blotting solid phase microextraction coating preparation method |
| CN101177501B (en) * | 2007-10-30 | 2010-05-19 | 湖北出入境检验检疫局检验检疫技术中心 | Method for preparing progesterone molecular engram polymer |
| CN102580353B (en) * | 2012-02-23 | 2014-04-16 | 宁波市疾病预防控制中心 | Preparation method of solid phase extraction column of molecular imprinted of phenolic environmental estrogens |
| CN104193875B (en) * | 2014-06-25 | 2016-03-23 | 齐鲁工业大学 | The preparation method of stilboestrol magnetic molecularly imprinted polymer and application thereof |
| CN108519445B (en) * | 2018-02-11 | 2020-11-24 | 桂林理工大学 | Method for separating and enriching trace estrogen in environmental water sample |
| CN114950394A (en) * | 2022-06-01 | 2022-08-30 | 江苏大学 | Preparation method of magnetic surface molecularly imprinted nano material for selective adsorption separation of diethylstilbestrol |
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