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Method for preparing pyrethroid fragment imprinted polymer

An imprinted polymer and pyrethroid technology, which is applied in the field of pesticide residue detection, can solve the problems of template molecule toxicity, template leakage, and health hazards.

Active Publication Date: 2013-01-16
INSPECTION & QUARANTINE TECH CENT HENAN ENTRY EXIT INSPECTION & QUARANTINE BUREAU +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Traditional molecular imprinting technology has been relatively mature in synthesis, but it faces an unavoidable interference—template leakage: because molecularly imprinted polymers have both the selectivity of bioabsorbent materials and the physical and chemical stability of conventional fillers, it is difficult to The template molecule is not completely removed in the elution step, so that the unused adsorbent already contains the template molecule; or the template molecule in the adsorbed sample remains in the adsorbent during use and is not finally eluted, which is harmful to molecular imprinting technology. Applications in trace analysis have a lot of interference
It may also be that the template molecule itself has toxic side effects, direct manipulation is harmful to health, or is difficult to obtain, which limits the preparation of molecularly imprinted polymers

Method used

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  • Method for preparing pyrethroid fragment imprinted polymer
  • Method for preparing pyrethroid fragment imprinted polymer
  • Method for preparing pyrethroid fragment imprinted polymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] Example 1. Preparation method of pyrethroid fragment imprinted polymer (bulk polymerization method), measure 0.153 mL (0.5 mmol) of diphenyl ether-biphenyl co-crystal instead of template, add 0.324 mL (3 mmol) of functional monomer 4- vp, 1.881 mL (10 mmol) of cross-linking agent EDMA and 24.3 mg of initiator AIBN were placed in a test tube, and 10 mL of chloroform was added, vortexed and mixed, nitrogen gas was passed for 10 min, and reacted in an oil bath at 70 °C for 24 h to obtain a light yellow rod-shaped solid The product (polymer), milled, and the resulting powder passed through a 100-200 mesh sieve.

[0054] At the same time, use the same ratio and method to prepare non-imprinted polymer NIP (without substituted template).

[0055] Weigh 500 mg of the obtained solid product and place it in the extraction cell of ASE-200 (Dionex, U.S.A.) (ASE extraction conditions: pressure: 1500 psi; temperature: 100 °C; heating time: 5 min; solvent washing time: 5 min; solvent...

Embodiment 2

[0161] Example 2, the preparation method of pyrethroid fragment imprinted polymer microspheres (suspension polymerization method), measure 100.0 mL of 1% polyvinyl alcohol solution and add it to a 250.0 mL round bottom flask, diphenyl ether-biphenyl cocrystal Add 2.0 mL, α-MAA 4.0 mL, DVB 20.0 mL, and BPO 0.25 g together into a small beaker and stir to dissolve, then pour into the dropping funnel and slowly drop into the flask. , reaction four h. Repeatedly stir and dissolve the prepared product with hot water, filter it with suction, wash away the polyvinyl alcohol adhered to the polymer until a relatively dry polymer is obtained, dry the prepared polymer, and sieve the 360-200 mesh (80μm-120μm) for standby use.

[0162] Weigh 500 mg of the prepared polymer, put it in the extraction cell of ASE-200, use the methanol-acetic acid mixed solution with a volume ratio of 4:1 to extract the replacement template in the receiving bottle according to the above steps, and take it out a...

Embodiment 3

[0163]Example 3. Preparation method of pyrethroid fragment imprinted polymer microspheres (precipitation polymerization method), measure 0.229 mL (0.75 mmol) of diphenyl ether-biphenyl cocrystal, 0.381 mL (4.5 mmol) of α-MAA and 5.640 EDMA mL (30 mmol) into a 250 mL round bottom flask, then add 0.0633 g of AIBN and 120 mL of chloroform, stir to dissolve completely, place in a constant temperature oil bath, and react at a temperature of 70 °C and magnetic stirring for 8 h. After the reaction, a white turbid solution is obtained, and a white powdery polymer is obtained after suction filtration. After drying, the product between 45 μm and 75 μm is sieved for use.

[0164] At the same time, the same ratio and method were used to prepare non-imprinted polymer microspheres (NIP) without substituted templates.

[0165] Weigh 500 mg of the prepared white powdery polymer, place it in the extraction cell of ASE-200, use the methanol-acetic acid mixed solution with a volume ratio of 4:1 ...

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Abstract

The invention discloses a method for preparing a pyrethroid fragment imprinted polymer and belongs to the technical field of pesticide residue detection. The method comprises the following steps of: performing thermal-initiation polymerization between a substitute template between a functional monomer and a cross-linking agent by utilizing the fragment imprinted solid phase extraction technology and selecting one fragment of pyrethroid or a similar structure of the fragment to serve as the substitute template, and washing off template molecules to prepare the pyrethroid fragment imprinted polymer. The prepared fragment imprinted polymer can be used for effectively realizing selective enrichment of pyrethroid matter.

Description

technical field [0001] The invention belongs to the technical field of pesticide residue detection, in particular to a preparation method of a pyrethroid fragment imprinted polymer suitable for detecting pyrethroid pesticide residues. Background technique [0002] Pyrethroids (synthetic pyrethroids) are synthetic esters derived from changing the chemical structure of natural pyrethroids. They are a class of biomimetic synthesis of broad-spectrum insecticides. class increased by 10 to 100 times. The action of pyrethroids is characterized by low concentration and small dosage, which is safer for humans and animals and has little environmental pollution. The main disadvantage is that it is highly toxic to fish, and long-term repeated use will also lead to resistance of pests. Therefore, mandatory regulations have been made in the relevant articles of CAC, stating that the residue limit of pyrethroids in most plant foods shall not exceed 2 mg kg-1, and the residue limit in ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F222/14C08F212/36C08F222/38C08F220/06C08F220/44C08F220/14C08F220/18C08F220/56C08F226/06C08F220/34C08F220/32C08F2/34C08F2/18C08F2/06C08J9/26
Inventor 王素方何娟沈妍铮陈思唐红哲庞文月
Owner INSPECTION & QUARANTINE TECH CENT HENAN ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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