Prometryn molecular imprinting solid phase extraction column and application method thereof

A solid-phase extraction column and molecular imprinting technology, which is applied in chemical instruments and methods, preparation of test samples, and other chemical processes, can solve the problem of overlapping matrix signals and analyte signals, uneven material particles, and affecting detection results, etc. question

Active Publication Date: 2013-12-11
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Triazine herbicides are a class of pesticides widely used in the world. They are suspicious substances of environmental hormones, which can cause cancer and interfere with endocrine. However, the residual concentration of triazine herbicides in food is very low, and often need to Proper enrichment is carried out before detection. In addition, in the multi-residue chromatographic detection after extraction, a large number of coexisting matrices extracted at the same time are particularly likely to contaminate the chromatographic column, and purification is required to remove the matrix. Due to the complex matrix of some types of samples, the signal of the matrix and the signal of the analyte may overlap, which affects the accuracy of the quantitative results. The sample also needs to be purified. Therefore, for this type of herbicide residues in food For detection, enrichment and purification are necessary
[0003] Solid-phase extraction is increasingly widely used in sample pretreatment for pesticide residue detection due to the use of less reagents, less harm to operators, and shorter operation time, and has become one of the most commonly used methods for enrichment and purification. One, but as we all know, the fillers used in solid-phase extraction columns are usually non-specific and selective adsorption materials. In practical applications, it is often easy to extract other interfering substances at the same time, which affects the test results. Most of the phase extraction columns are disposable, which also increases the detection cost; the molecularly imprinted polymer is a polymer tailored for the molecular weight of the template, which has high recognition for the template molecule and its structural analogues, and It can be reused many times, which is unmatched by ordinary solid-phase extraction fillers. Most of the molecularly imprinted solid-phase extraction fillers reported at present use the bulk polymerization method. The material particles obtained after grinding are not uniform, and many binding sites are wrapped in Inside the particle, the function of the imprinted material cannot be fully exerted

Method used

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  • Prometryn molecular imprinting solid phase extraction column and application method thereof
  • Prometryn molecular imprinting solid phase extraction column and application method thereof

Examples

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Embodiment 1

[0032] 1 Preparation of promethazine molecularly imprinted solid-phase extraction column

[0033] A Mix and dissolve promethazin (0.242 g) and methacrylic acid in 35 mL of dichloromethane at a molar ratio of 1:4, and leave it at room temperature overnight. The ester molar ratio is 1:20 and the azobisisobutyronitrile molar ratio is 1:0.24. The two are added to the above solution and ultrasonically oscillated for 5 minutes, and nitrogen gas is passed into the round bottom flask containing the solution for 5 minutes. Then place the flask at 55 ° C reacted at 350 rpm for 15 h in a constant temperature electric heating mantle to prepare polymer microspheres, put the polymer microspheres in a Soxhlet extractor, and wash away the template with a mixed solvent of acetic acid-methanol (10:90, V / V) Molecules, and then washed with methanol to remove residual acetic acid in the polymer microspheres, and repeated sedimentation with acetone to remove fine particles, and finally dried in a ...

Embodiment 2

[0048] 1 Preparation of promethazine molecularly imprinted solid-phase extraction column

[0049] A Mix and dissolve promethazine (0.242g) and methacrylic acid in a molar ratio of 1:4 in 35 mL of dichloromethane, and leave it overnight at room temperature. According to the ratio of promethazine and ethylene glycol dimethacrylate molar ratio of 1:20 and the ratio of azobisisobutyronitrile molar ratio of 1:0.24, the two were added to the above solution for ultrasonic vibration for 5min, and The round-bottomed flask containing the solution was ventilated with nitrogen for 5 minutes, and then the flask was placed at 55 ° C reacted at 350 rpm for 15 h in a constant temperature electric heating mantle to prepare polymer microspheres, put the polymer microspheres in a Soxhlet extractor, and wash away the template with a mixed solvent of acetic acid-methanol (10:90, V / V) Molecules, and then washed with methanol to remove residual acetic acid in the polymer microspheres, and repeated ...

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Abstract

The invention relates to the technical field of solid phase extraction, and particularly discloses a prometryn molecular imprinting solid phase extraction column and an application method thereof. With prometryn as a template, methacrylic acid as a functional monomer, glycol dimethyl methacrylate as a cross-linking agent, azodiisobutyronitrile as an initiating agent, dichloromethane as a solvent, a precipitation polymerization method is adopted to prepare prometryn molecular imprintingpolymeric microsphere; microballoons are uniformly filled in the solid phase extraction column, thus obtaining the prometryn molecular imprinting solid phase extraction column; dichloromethane is utilized as, residuals of simazine, atrazine, szimetrin, propazine, ametryn, terbuthylazine, prometryn and terbutryn in a grain sample are simultaneously enriched and purified by taking a sample solvent and dichloromethane-acetonitrile as a leaching solvent and taking methyl alcohol-water as an eluting solvent, when used together with a capillary electrophoresis multiresidue detection method, the prometryn molecular imprinting solid phase extraction column can simultaneously detect the residuals of the eight herbicideds.

Description

technical field [0001] The invention relates to the technical field of solid-phase extraction, in particular to a promethazine molecularly imprinted solid-phase extraction column and its use method, and combined with capillary electrophoresis for selective separation, enrichment and detection of simazine and atrazine in grain samples Residues of desine, siclozine, proprazine, arazine, terbuthine, promethazine and terbuthine. Background technique [0002] Triazine herbicides are a class of pesticides widely used in the world. They are suspicious substances of environmental hormones, which can cause cancer and interfere with endocrine. However, the residual concentration of triazine herbicides in food is very low, and often need to Proper enrichment is carried out before detection. In addition, in the multi-residue chromatographic detection after extraction, a large number of coexisting matrices extracted at the same time are particularly likely to contaminate the chromatograp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/281B01J20/30G01N1/34G01N1/40
Inventor 方柔陈冠华伊聆晓张丽邵钰秀
Owner JIANGSU UNIV
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