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Molecular imprinting polymer for roxarsone detection, and preparation method thereof

A molecular imprinting and polymer technology, applied in the field of material chemistry, can solve the problems of low specificity, affecting the sensitivity and accurate quantification of detection methods, lack of selectivity, etc., and achieve strong specific recognition ability, high affinity and selection Sexuality, the effect of improving specificity

Inactive Publication Date: 2013-08-07
SOUTH CHINA AGRI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, all current pretreatment methods for roxarsone detection are purified by traditional solid-phase extraction cartridges (such as MAX), which lack selectivity and specificity, thus affecting the sensitivity and accurate quantification of the entire detection method.

Method used

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  • Molecular imprinting polymer for roxarsone detection, and preparation method thereof
  • Molecular imprinting polymer for roxarsone detection, and preparation method thereof
  • Molecular imprinting polymer for roxarsone detection, and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] (1) Weigh 0.166g (1mmoL) of ethyl p-hydroxybenzoate into a test tube, add 1mL of acetonitrile, vortex to dissolve, then add 0.434mL (4mmoL) of 2-vinylpyridine functional monomer, ultrasonic for 5min, let stand for 1h , Form a prepolymer.

[0049] (2) Add 4mL (20mmoL) of ethylene glycol dimethacrylate and 60mg (0.365mmol) of azobisisobutyronitrile to the above-mentioned prepolymer, ultrasonicate for 5min, let nitrogen gas for 5min under ice bath, seal, vacuum at 60℃ Polymerize in a dry box for 24 hours to obtain a bulk polymer.

[0050] (3) Grind the aforesaid block polymer, sieving through a 200-mesh sieve, repeatedly settling with methanol to remove fine particles, and put it into a 15mL solid phase extraction column, first use a mixed solution of acetic acid and methanol (the volume ratio of acetic acid to methanol is 1 9) 200mL wash to remove template ethyl p-hydroxybenzoate, the flow rate is controlled below 1mL / min, and then 40mL methanol wash to remove acetic acid, dr...

Embodiment 2

[0053] (1) Weigh 0.217g (1mmoL) of arsanic acid into a test tube, add 6mL methanol-acetonitrile solution (the volume ratio of methanol to acetonitrile is 1:1), vortex to dissolve, add 0.434mL (4mmoL) 2-ethylene Pyridine functional monomer, ultrasonic for 5min, stand for 1h to form a prepolymer.

[0054] (2) Add 4mL (20mmoL) of ethylene glycol dimethacrylate and 60mg (0.365mmol) of azobisisobutyronitrile to the above-mentioned prepolymer, ultrasonicate for 5min, let nitrogen gas for 5min under ice bath, seal, vacuum at 60℃ Polymerize in a dry box for 24 hours to obtain a bulk polymer.

[0055] (3) Grind the aforesaid block polymer, sieving through a 200-mesh sieve, repeatedly settling with methanol to remove fine particles, and put it into a 15mL solid phase extraction column, first use a mixed solution of acetic acid and methanol (the volume ratio of acetic acid to methanol is 1 : 9) Wash with 200mL to remove the template arsanic acid, control the flow rate below 1mL / min, then was...

Embodiment 3

[0058] (1) Weigh 0.217g (1mmoL) arsanic acid into a test tube, add 6mL methanol-acetonitrile (1:1, V / V) solution, vortex to dissolve, add 0.171mL (2mmoL) methacrylic acid functional monomer , Ultrasound for 5 minutes, and let stand for 1 hour to form a prepolymer.

[0059] (2) Add 3.19mL (10mmoL) of trimethylolpropane trimethacrylate and 10mg (0.06mmoL) of azobisisobutyronitrile to the above-mentioned prepolymer, ultrasonicate for 5min, bubbling nitrogen for 5min under ice bath, and seal. Polymerize in a vacuum drying oven at 50°C for 48 hours to obtain a bulk polymer.

[0060] (3) Grind the above-mentioned bulk polymer, sieving through a 200-mesh sieve, repeatedly settling with methanol to remove fine particles, and put it into a 15 mL solid phase extraction column. First use a mixed solution of acetic acid and methanol (1:9, V / V). ) Wash with 200mL to remove the template arsanic acid, control the flow rate below 1mL / min, then wash with 40mL methanol to remove acetic acid, and pl...

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Abstract

The invention belongs to the technical field of material chemistry, and discloses a molecular imprinting polymer for roxarsone detection, and a preparation method thereof. The molecular imprinting polymer preparation method comprises the following steps: carrying out polymerization of a template, a pore forming agent, a functional monomer, a cross-linking agent and an initiator for 8-48 h at a temperature of 50-80 DEG C, and removing the template to obtain the molecular imprinting polymer for roxarsone detection. According to the present invention, a roxarsone recovery rate of the prepared molecular imprinting polymer is more than 90%, and the prepared molecular imprinting polymer shows a high roxarsone cross reaction, has high selectivity and high specificity, and provides broad application prospects in the field of application of the prepared molecular imprinting polymer as a sample purification pretreatment material for roxarsone analysis in feeds, animal tissues, environment water and other matrixes.

Description

Technical field [0001] The invention belongs to the technical field of material chemistry, and particularly relates to a molecularly imprinted polymer for detecting roxarsone and a preparation method thereof. Background technique [0002] Roxarsone, chemical name: 3-nitro-4-hydroxy-phenylarsonic acid, and P-Arsanilic acid are two arsenic-containing feed additives that have been widely used in various countries around the world for many years , And roxarsone is more widely used than arsanic acid. Roxarsone is the most economical multifunctional organic arsenic preparation. It can promote the growth of livestock and poultry, improve feed conversion rate, promote livestock pigmentation, and increase the effect of other anticoccidial drugs on poultry; treat swine dysentery and enteritis, Improve the laying rate of laying hens. my country's Ministry of Agriculture approved the use of the drug in 1996, and then gradually began mass production in the country, and it is widely used in ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F226/06C08F220/06C08F212/14C08F220/56C08F222/14C08F212/36C08J9/26C08J9/28B01J20/26B01J20/30G01N1/34
Inventor 贺利民张高奎刘雅红方炳虎杨建文王宗楠杨海翠
Owner SOUTH CHINA AGRI UNIV
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