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Dibutyl phthalate molecularly imprinted polymer (DBP-MIP) solid phase extraction column and preparation method and application thereof

A technology of dibutyl phthalate and solid-phase extraction cartridges, which is applied in the field of analytical chemistry and can solve the problems of poor specificity of adsorbents and interference detection of impurities

Inactive Publication Date: 2012-03-14
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to overcome the problem that the specificity of the adsorbent is not strong in the sample pretreatment process in the detection of dibutyl phthalate in the prior art, and it is easy to introduce impurities that interfere with the detection, the invention provides a dibutyl phthalate molecule Imprinted polymer and preparation method thereof, the compound can be used to prepare dibutyl phthalate molecularly imprinted solid-phase extraction column, so that it can simply, quickly and highly selectively detect phthalic acid in complex matrix samples Separation and enrichment of dibutyl esters for the detection of trace amounts of dibutyl phthalate

Method used

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  • Dibutyl phthalate molecularly imprinted polymer (DBP-MIP) solid phase extraction column and preparation method and application thereof
  • Dibutyl phthalate molecularly imprinted polymer (DBP-MIP) solid phase extraction column and preparation method and application thereof
  • Dibutyl phthalate molecularly imprinted polymer (DBP-MIP) solid phase extraction column and preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0028] (1) Synthesis of dibutyl phthalate molecularly imprinted polymer

[0029] (1) Dissolve 0.5mmol of DBP, 2mmol of MMA, 10mmol of EDMA, and 0.05mmol of AIBN in 20mmol of acetonitrile, put the mixed solution in a round-bottomed flask, pre-act 0.5h in an ice-water bath (ultrasonic wave makes various reactants fully mixed Uniform, ice-water bath prevents various reactants from being heated and polymerized in advance during the ultrasonic process, this step is a routine operation method in the laboratory);

[0030] (2) Introduce nitrogen gas for 10 minutes, seal with a rubber stopper, and react in an oil bath at 60° C. for 24 hours to obtain a reaction product. After the reaction, the polymer is ground, sieved, and rinsed with acetone to remove fine particles to obtain a polymer with a particle size of 20-200 μm;

[0031] (3) Use 200 mL of methanol solution containing 10% acetic acid as the extraction agent, perform Soxhlet extraction for 24 hours to remove template molecules...

Embodiment 2

[0041] (1) Synthesis of dibutyl phthalate molecularly imprinted polymer

[0042] (1) Dissolve 0.5mmol of DBP, 2mmol of MMA, 10mmol of EDMA, and 0.05mmol of AIBN in 20mmol of chloroform, put the mixture in a round-bottomed flask, and ultrasonically pre-act for 0.5h in an ice-water bath;

[0043] (2) Introduce nitrogen gas for 10 minutes, seal with a rubber stopper, and react in an oil bath at 60° C. for 24 hours to obtain a reaction product. After the reaction, the polymer is ground, sieved, and rinsed with acetone to remove fine particles to obtain a polymer with a particle size of 20-200 μm;

[0044](3) Use 200 mL of methanol solution containing 10% acetic acid as the extraction agent, perform Soxhlet extraction for 24 hours to remove template molecules, add the extraction agent once at about 12 hours in the middle, and use 100 mL of methanol to wash after the extraction to remove residual formic acid;

[0045] (4) The molecularly imprinted polymer from which template molecu...

Embodiment 3

[0052] (1) Synthesis of dibutyl phthalate molecularly imprinted polymer

[0053] (1) Dissolve 0.5mmol of DBP, 2mmol of MMA, 10mmol of EDMA, and 0.05mmol of AIBN in 20mmol of acetonitrile, put the mixture in a round-bottomed flask, and pre-act for 0.5h in an ice-water bath;

[0054] (2) Introduce nitrogen gas for 10 minutes, seal with a rubber stopper, and react in an oil bath at 70° C. for 48 hours to obtain a reaction product. After the reaction, the polymer is ground, sieved, and rinsed with acetone to remove fine particles to obtain a polymer with a particle size of 20-200 μm;

[0055] (3) Use 200 mL of methanol solution containing 5% acetic acid as the extractant, perform Soxhlet extraction for 48 hours to remove template molecules, add the extractant once every 12 hours, and wash with 100 mL of methanol to remove residual formic acid after the extraction;

[0056] (4) The molecularly imprinted polymer from which template molecules have been removed is vacuum-dried at 70°...

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Abstract

The invention provides a dibutyl phthalate molecularly imprinted polymer (DBP-MIP) solid phase extraction column and a preparation method and application method thereof, belonging to the technical field of analytical chemistry. The DBP-MIP is prepared by dissolving a template molecule DBP, a functional monomer methacrylic acid and a crosslinking agent ethylene glycol dimethacrylate into a porogen chloroform or acetonitrile, adding an initiator azobisisobutyronitrile, filling nitrogen to remove oxygen, carrying out initiated polymerization at 55-75 DEG C, and grinding, sieving and washing a polymer after completing reaction. The preparation method is characterized by weighing a certain amount of polymer and filling the polymer into a polypropylene column to prepare the solid phase extraction column. The prepared MIP solid phase extraction column can highly selectively separate and enrich DBP in samples such as environment, food, chemical products and the like and effectively remove matrix interference, and has great application values and market prospects.

Description

technical field [0001] The invention relates to an analytical chemical technology method, in particular to a dibutyl phthalate molecularly imprinted solid-phase extraction small column and a preparation method and application thereof. Background technique [0002] Dibutyl phthalate (DBP) is mainly used as an industrial plasticizer, as well as a raw material for the production of pesticide carriers, insect repellents, cosmetics, fragrances, lubricants, and defoamers. DBP is widely present in natural environments such as air, water, soil, and organisms as industrial production continues to enter the environment, and has become one of the most common pollutants in the world. DBP is an important environmental endocrine disruptor, similar to estrogen, which seriously interferes with the endocrine system of humans and animals, especially the reproductive function, and has the possibility of carcinogenic, teratogenic and mutagenic, so it has attracted people's attention. [0003] ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D15/22B01J20/285B01J20/30G01N30/08G01N30/36G01N30/72G01N1/34
Inventor 孙姝琦王红姚青张颖
Owner CHINA PETROLEUM & CHEM CORP
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