Preparation of triazine phytocide molecular imprinting solid phase extracting material

A solid-phase extraction material and molecular imprinting technology, which is applied in the analysis of materials, material separation, ion exchange, etc., can solve the problems of low mass spectrometry analysis, low mechanical strength, optimization, etc., and achieve the effect of accurate and reliable methods and saving experimental costs

Inactive Publication Date: 2011-09-07
安徽出入境检验检疫局检验检疫技术中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Even a trace amount of template molecule leakage will pose a threat to the use of high-sensitivity chromatography-mass spectrometry, resulting in false positive results. Reason for analysis
Because only chromatography is used for qualitative and quantitative analysis, it is difficult to meet the requirements of low-quantity analysis and confirmatory analysis methods
[0012] B. The application of molecular imprinting technology in the analysis of triazine herbicides is mainly concentrated in soil and environmental water. The effective use conditions were not optimized when the samples were used, so the selective adsorption effect of molecularly imprinted materials was not reflected to the greatest extent.
[0013] C. The existing molecularly imprinted solid phase extraction materials for triazine herbicides are prepared by bulk polymerization, so their irregular shapes lead to uneven adsorption of the adsorbent. Due to their low mechanical strength, the adsorbent is not pressure-resistant and prone to Collapses during use resulting in loss of adsorption performance

Method used

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  • Preparation of triazine phytocide molecular imprinting solid phase extracting material
  • Preparation of triazine phytocide molecular imprinting solid phase extracting material
  • Preparation of triazine phytocide molecular imprinting solid phase extracting material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0122] The preparation of the triazine herbicide molecularly imprinted solid-phase extraction material comprises the following steps:

[0123] 1. Preparation of suspension phase I

[0124] Take 0.8 g of butylmelamine, 1.1 g of α-methacrylic acid (MAA), 9.6 mL of ethylene glycol di(methacrylate) (EDGMA) and 0.33 g of azobisisobutyronitrile (AIBN), and dissolve them in 24 mL Chloroform, mix homogeneously, obtain suspension phase I;

[0125] Among them, butylmelamine was used as the imprinting template, α-methacrylic acid (MAA) was used as the functional monomer, ethylene glycol di(methacrylate) (EDGMA) was used as the crosslinking agent, and azobisisobutyronitrile (AIBN) was used as the initiator. Agent, trichloromethane as solvent;

[0126] The molar ratio of the imprinted template to the functional monomer is 1:3, the molar ratio of the cross-linking agent to the functional monomer is 4:1, the molar ratio of the initiator to the functional monomer is 1:6, the volumetric amou...

Embodiment 2

[0138] The preparation of the triazine herbicide molecularly imprinted solid-phase extraction material comprises the following steps:

[0139] 1. Preparation of suspension phase I

[0140] Take 1.5 g of butylmelamine, 2.1 g of α-methacrylic acid (MAA), 24 mL of ethylene glycol di(methacrylate) (EDGMA) and 0.79 g of azobisisobutyronitrile (AIBN), and dissolve them in 40 mL of three Chloromethane, mixed uniformly to obtain suspension phase I;

[0141] Among them, butylmelamine was used as the imprinting template, α-methacrylic acid (MAA) was used as the functional monomer, ethylene glycol di(methacrylate) (EDGMA) was used as the crosslinking agent, and azobisisobutyronitrile (AIBN) was used as the initiator. Agent, trichloromethane as solvent;

[0142] The molar ratio of the imprinted template to the functional monomer is 1:3, the molar ratio of the cross-linking agent to the functional monomer is 5:1, the molar ratio of the initiator to the functional monomer is 1:5, the volu...

Embodiment 3

[0154] The preparation of the triazine herbicide molecularly imprinted solid-phase extraction material comprises the following steps:

[0155] 1. Preparation of suspension phase I

[0156] Take 1.5 g of butylmelamine, 2.1 g of α-methacrylic acid (MAA), 29 mL of ethylene glycol di(methacrylate) ester (EDGMA) and 0.99 g of azobisisobutyronitrile (AIBN), dissolve in 36 mL Chloroform, mix homogeneously, obtain suspension phase I;

[0157] Among them, butylmelamine was used as the imprinting template, α-methacrylic acid (MAA) was used as the functional monomer, ethylene glycol di(methacrylate) (EDGMA) was used as the crosslinking agent, and azobisisobutyronitrile (AIBN) was used as the initiator. Agent, trichloromethane as solvent;

[0158] The molar ratio of the imprinted template to the functional monomer is 1:3, the molar ratio of the cross-linking agent to the functional monomer is 6:1, the molar ratio of the initiator to the functional monomer is 1:4, the volume of the solve...

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Abstract

The invention relates to a preparation method of a triazine phytocide molecular imprinting solid phase extracting material. The method comprises the following steps of: 1. dissolving butyltripolycyanamide, alpha-methacrylic acid, glycol di(methacrylic acid)ester and azodiisobutyronitrile into trichloromethane and uniformly mixing to obtain a suspending phase I; 2. dissolving polyvinyl alcohol 1788 into water to obtain a suspending phase II; and 3. stirring and reacting the suspending phase I with the suspending phase II and drying in vacuum to obtain the triazine phytocide molecular imprinting solid phase extracting material. In the invention, by adopting a substituted molecular template, the imprinting effect is ensured and the problem of template seepage is solved; the optimized use condition is more convenient for solid phase extraction and ensures favorable impurity removing function and favorable repeatability; the matrix effect is remarkably weakened; and the triazine phytocide molecular imprinting solid phase extracting material is better than the traditional main stream solid phase extracting product, not only can ensure the detecting accuracy but also can improve the detecting sensitivity and effectively protect a chromatographic column.

Description

technical field [0001] The invention belongs to the technical field of analysis and determination of triazine herbicide residues, and in particular relates to the preparation and application of pretreatment materials in the analysis and determination of triazine herbicide residues. technical background [0002] At present, with the development of my country's agricultural modernization and the gradual transfer of agricultural labor to cities, cultivation and farming methods tend to be large-scale and intensive, and the demand for agricultural production has increased significantly. Among them, the growth rate of herbicides in recent years is much higher than the development level of insecticides and fungicides. The wide use of herbicides in my country has brought positive benefits such as agricultural modernization and crop yield growth, but it has also caused weed resistance in the field. It is becoming more and more serious, and in turn induces a further increase in the app...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F222/14C08F220/06C08F2/20C08J9/26B01J20/26B01J20/285B01J20/30B01D15/08G01N30/56G01N30/08
Inventor 郑平盛旋姚剑徐业平胡艳云韩芳张蕾孙昊
Owner 安徽出入境检验检疫局检验检疫技术中心
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