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Malathion molecularly imprinted polymer and synthetic method of malathion restricted access media-molecularly imprinted polymer

A technology of malathion and molecular imprinting, which is applied in the field of residual pesticide detection, can solve the problems of adsorbent pore blockage, reduce column capacity, shorten column life, etc., and achieve high recovery rate, good extraction effect and low standard deviation.

Inactive Publication Date: 2013-08-28
HENAN UNIVERSITY OF TECHNOLOGY
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  • Abstract
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  • Claims
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Problems solved by technology

This is because the biomacromolecules in the sample will be denatured when encountering the hydrophobic reversed-phase solid-phase extraction filler and then adhere to the surface of the adsorbent, resulting in adverse phenomena such as clogging of the adsorbent pore size and reducing the adsorption efficiency of the analyte on the adsorbent. , so as to reduce column efficiency, reduce column capacity, and shorten column life, not only can not play the advantage of high selectivity of molecular imprinted solid phase extraction for small molecule analytes, but seriously affect the detection results

Method used

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  • Malathion molecularly imprinted polymer and synthetic method of malathion restricted access media-molecularly imprinted polymer

Examples

Experimental program
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Embodiment 1

[0048] Example 1, the synthesis method of malathion molecularly imprinted polymer:

[0049] Accurately measure 0.067mL (0.25mmol) of the template molecule malathion, 0.170mL (2mmol) of the functional monomer MAA (α-methacrylic acid), and 1.889mL of the cross-linking agent EDMA (ethylene glycol dimethacrylate) ( 10mmol) into the test tube (template molecule: functional monomer: crosslinking agent = 1:8:40), then add 24.24mg of initiator AIBN (azobisisobutyronitrile), 5mL of solvent chloroform, shake, and blow nitrogen for 5min Shake it for another 10 minutes to make it fully mixed, seal it, and react in a constant temperature water bath at 70°C for 24 hours. After grinding and sieving, the molecularly imprinted polymer of malathion with a particle size of 75-150 μm is collected. Then wrap it with filter paper, first use methanol / glacial acetic acid (9 / 1, V / V) solution to elute the template molecule in a Soxhlet extractor, and then change to pure methanol for elution until no t...

Embodiment 2

[0109] Example 2. Synthesis method of malathion molecularly imprinted microspheres (precipitation polymerization method):

[0110] (1) Take the template molecule malathion (0.268mL, 1.0mmol) and the functional monomer MAA (0.509mL, 6.0mmol) into a 250mL round-bottom flask, add 40mL of chloroform solvent, put the magnet on the magnetic stirrer to pre- Polymerize for 5h, then add cross-linking agent EDMA (5.642mL, 30.0mmol) and initiator AIBN (0.096g), and finally add 120mL chloroform solvent. Put the round bottom flask containing this mixed solution into a constant temperature magnetic stirrer, and the temperature and speed of the constant temperature magnetic stirrer were set to 70°C and 150r min respectively -1 . Reaction under these conditions for 10h. Molecularly imprinted microspheres were obtained.

[0111] The composition ratio and method of the non-molecularly imprinted microspheres are the same as above, except that the template molecule malathion is not added.

[...

Embodiment 3

[0113] Example 3. Synthesis method of limited-access medium-malathion molecularly imprinted microspheres (precipitation polymerization method): including the synthesis of limited-access medium-molecularly imprinted microspheres, the removal of template molecules in the microspheres and the epoxy on the surface of the microspheres Hydrolytic ring opening of the ring.

[0114] (1) Synthesis of restricted access medium-molecularly imprinted microspheres: A new monomer GMA (glycidyl methacrylate) (0.199 mL, 6.0 mmol) was added to the mixed solution in Example 2 (1), namely The ratio of template molecule, MAA, GMA and EDMA is 1:6:6:30, add initiator AIBN0.146g and 150mL chloroform solvent to a 250mL round bottom flask. Others are the same as embodiment 2 (1).

[0115] The steps for template molecule removal are the same as in Example 2(2).

[0116] The same ratio and method were used to prepare restricted access medium-non-molecularly imprinted microspheres (without adding templa...

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Abstract

The invention provides a malathion molecularly imprinted polymer and a synthetic method of a malathion restricted access media-molecularly imprinted polymer. The malathion molecularly imprinted polymer is synthesized by using a molecular imprinting technique and a bulk polymerization method. A prepared molecularly imprinted solid phase extraction column has a recovery rate of 97.8% for malathion. The extraction effect is obviously better than that of commercialized solid phase extraction columns. By using the restricted access media-molecular imprinted technology, the precipitation polymerization and suspension polymerization are optimized to synthesize malathion molecularly imprinted microspheres and restricted access media-molecularly imprinted microspheres. The resulting microspheres are made into a solid phase extraction column. Compared with the commercialized solid phase extraction columns, the solid phase extraction column has the advantages of high recovery rate, low standard deviation, and good reproducibility.

Description

technical field [0001] The invention belongs to the technical field of residual pesticide detection, and in particular relates to a synthesis method of a malathion molecularly imprinted polymer and a malathion limited access medium-molecularly imprinted microspheres for detecting malathion residues. Background technique [0002] As an important factor affecting food safety, excessive pesticide residues directly affect the health of consumers and become the primary indicator for measuring food quality and safety in various countries. Pesticides can be divided into four categories: organochlorine pesticides, carbamate pesticides, pyrethroid pesticides, and organophosphorus pesticides. Organophosphorus pesticides mainly include malathion, grammephos, terbuthion, phorate, dimethoate, chlorpyrifos, methamidophos, trichlorfon, dichlorvos, parathion, trichlorfon, phoxim Wait. Organophosphorus pesticides can effectively prevent and control pests and diseases, and are convenient to...

Claims

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Application Information

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IPC IPC(8): C08F222/14C08F220/06C08F220/32C08F212/36C08F2/44C08F2/02C08F2/20C08J9/26
Inventor 何娟王素方陈思沈妍铮唐红哲游利琴
Owner HENAN UNIVERSITY OF TECHNOLOGY
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