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Preparation method and application of bitertanol based molecularly-imprinted solid-phase extraction column

A technology of solid phase extraction column and bifentriazole, which is applied in the field of preparation of biphenyltriazole molecularly imprinted solid phase extraction column, can solve the problems of low actual recovery rate of analytes, non-repeatable use, poor selectivity, etc.

Inactive Publication Date: 2013-10-09
HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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Problems solved by technology

[0009] The disadvantages of traditional solid-phase extraction are: (1) the actual recovery rate of the analyte is low; (2) the force between the solid-phase extraction and the adsorbent is non-specific, and the extraction and elution conditions are relatively harsh; (3) the selectivity is poor, and the treatment of impurities Incomplete, easy to cause column contamination; ⑷ can not be used repeatedly

Method used

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  • Preparation method and application of bitertanol based molecularly-imprinted solid-phase extraction column
  • Preparation method and application of bitertanol based molecularly-imprinted solid-phase extraction column
  • Preparation method and application of bitertanol based molecularly-imprinted solid-phase extraction column

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Embodiment Construction

[0079] 1. Preparation of Biphenyltriazole Molecularly Imprinted Polymer

[0080] Put bifentriazole (0.2mmol) and 0.8mmol of MAA into a 50mL ampoule, add 15mL of acetonitrile to react, vibrate at a frequency of 50kHz for 1h, and add a cross-linking agent ethylene glycol dimethacrylate (EDMA) 8mmol and initiator azobisisobutyronitrile (AIBN) 0.02g. Vibration frequency 50kHz Ultrasonic 30min after passing through N 2 After deoxygenation for 15 minutes, vacuumize for 1 minute, seal it, and let it stand in a constant temperature water bath at 55°C for 10 hours to obtain blocky solid MIP. Grinding, pulverizing, passing through a 200-mesh sieve, and then using deionized water to settle the polymer 3 times to remove superfine powder. The final MIP particles were eluted with methanol:acetic acid (volume ratio 95:5) to template-free molecules, and finally soaked in methanol for 1 hour to remove residual acetic acid, and the eluted polymer was placed in a vacuum dryer (45°C) After d...

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Abstract

The invention belongs to the field of organic synthesis, and analytical chemistry and particularly relates to a preparation method and an application of a bitertanol based molecularly-imprinted solid-phase extraction column. The traditional solid-phase extraction column has the disadvantages that the actual recovery rate of analyte is low, the interaction between the solid-phase extract and the adsorbent is nonspecific, and the extraction and elution conditions are severe. In addition, the traditional solid-phase extraction column has poor selectivity, can lead to the incomplete treatment of impurities and the pollution to the chromatographic column easily and can not be used repeatedly. The bitertanol based molecularly-imprinted polymer is prepared by adopting a mass polymerization method, after the prepared molecularly-imprinted polymer is subjected to a series of treatments, such as grinding, rinsing, sieving, eluting and drying, the molecularly-imprinted polymer is evaluated and analyzed by adopting the ultraviolet spectrophotometry and the high-performance liquid chromatography to so as to have a specific adsorption effect, and the molecularly-imprinted solid-phase extraction column is prepared. The molecularly-imprinted solid-phase extraction column is used for purifying a sample, and separating and enriching the bitertanol and structural analogues thereof in food and feed.

Description

technical field [0001] The invention relates to the field of organic synthesis and analytical chemistry, in particular to a preparation method and application of a bifentriazole molecularly imprinted solid-phase extraction column, which is used for the residue analysis of bifentriazole and its structural analogues in food and feed Sample purification and enrichment. Background technique [0002] Bifentriazole is a broad-spectrum systemic fungicide, mainly used to control Venturia ) and Sclerotinia ( Sclerotinia ) caused by fruit tree diseases, and coccidiomycetes ( Mycosphaerella ) caused banana disease and peanut leaf spot; it has the characteristics of high efficiency, broad spectrum, low toxicity, strong systemicity, etc., and its prevention and control mechanism is mainly to inhibit the biosynthesis of pathogenic bacteria ergosterol, so that the cell membrane function of the bacteria is affected destroy. [0003] According to the Chinese pesticide toxicity classifi...

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Application Information

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IPC IPC(8): C08F220/06C08F222/14C08J9/28B01D15/08G01N30/08G01N30/14
Inventor 高文惠刘博
Owner HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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