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Production method and use of anion exchange online purification solid phase extraction monolithic column

A monolithic column and anion technology, which is applied in the field of analytical chemistry, can solve the problems of poor extraction capacity and pressure resistance, and achieve the effect of significant enrichment and purification, stable properties, and simple preparation methods

Active Publication Date: 2016-09-28
INSPECTION & QUARANTINE TESTING CENT OF HEBEI ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It can be seen from the above applications that the on-line purification monolithic column is mainly prepared in a capillary tube. The extraction capacity and pressure resistance of this monolithic column are poor, and the type is also mainly reversed-phase adsorption. The column with ion exchange is used in high-pressure liquid The online solid phase extraction monolithic column of the phase system is still blank

Method used

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  • Production method and use of anion exchange online purification solid phase extraction monolithic column
  • Production method and use of anion exchange online purification solid phase extraction monolithic column
  • Production method and use of anion exchange online purification solid phase extraction monolithic column

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Embodiment 1: the preparation method of ploy (DMAEMA-co-EDMA) monolithic column

[0024] (1) Based on the total volume of reactants (1.25 mL), 3.7% monomer DMAEMA, crosslinking agent 20% EDMA, porogen 70%, initiator azobisisobutyronitrile 10 mg. Ultrasonic mixing and degassing at room temperature for 30 min.

[0025] (2) The solution was poured into a dry stainless steel empty column tube (10 mm×2.1 mm i.d.), both ends were sealed, and the temperature of the water bath was fixed at 55° C. and the reaction time was 30 h to prepare the monolithic column. And the monolithic column after the completion of the reaction is connected to the high-performance liquid chromatography high-pressure pump, and the monolithic column is washed with methanol to remove unreacted monomer and porogen to obtain a poly(DMAEMA-co-EDMA) monolithic column, which is ready for use .

Embodiment 2

[0026] Embodiment 2: the preparation method of ploy (DMAEMA-co-EDMA) monolithic column

[0027] (1) Based on the total volume of reactants (2.0 mL), 6.1% monomer DMAEMA, cross-linking agent EDMA 17%, porogen 80%, and initiator azobisisobutyronitrile 10 mg. Ultrasonic mixing and degassing at room temperature for 30 min.

[0028] (2) Afterwards, the solution was poured into a stainless steel column tube, both ends were sealed, and the temperature of the water bath was fixed at 65° C., and the reaction time was 20 h to prepare the monolithic column. And the monolithic column after the reaction is completed is connected to the high-performance liquid chromatography high-pressure pump, and the monolithic column is washed with methanol to remove unreacted monomers and porogens to obtain a poly(DMAEMA-co-EDMA) monolithic column, which is ready for use.

Embodiment 3

[0029] Example 3: Using the monolithic column prepared in Example 1 as the extraction medium, combined with liquid chromatography tandem mass spectrometry, the online purification and enrichment detection of five acidic pesticides in fruits

[0030] 1 sample processing

[0031] Accurately weigh about 10.0g of fresh pear and apple samples, put them in a 50mL centrifuge tube, add 10mL of acetonitrile, 5g of anhydrous sodium chloride, homogenize at 15000rpm for 1min, centrifuge at 5000rpm for 5min, take the supernatant in a 50mL centrifuge tube middle. Repeat the above extraction process twice, combine the supernatant, take 1mL of the supernatant, filter through a 0.22 μm microporous membrane, and wait for the test.

[0032] 2 test conditions

[0033] 2.1 Online purification conditions

[0034] The online SPE conditions are divided into 4 parts: loading, washing, elution and conditioning.

[0035] a) Loading: The mobile phase A of the loading pump is 5mmol / L ammonium acetate ...

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Abstract

The invention relates to a production method and a use of an anion exchange online purification solid phase extraction monolithic column. The monolithic column adopts dimethylaminoethyl methacrylate as a monomer, ethylene glycol methacrylate as a cross-linking agent, n-propanol and PEG-400 as a pore foaming agent and azodiisobutyronitrile as an initiator. The production method comprises the following steps: carrying out ultrasonic mixing, degassing the obtained mixture, filling a stainless steel tube with the degassed mixture, sealing the stainless steel tube, and carrying out a reaction in 55-65DEG C water bath for 20-30h to obtain the poly(DMAEMA-co-EDMA) monolithic column. The monolithic column can be used for detecting and analyzing the residual of acidic pesticides in vegetables and fruits. The monolithic column polymerized on a stainless steel chromatographic column in an in-situ manner can tolerate a certain pressure, and is connected to an online purification and enrichment system to realize automation of the solid phase extraction purification. The monolithic column has the advantages of simple production method, continuous porous structure, convenient flow-out of a mobile phase, and obvious reduction of the mass transfer resistance, has a higher extraction efficiency and a lower column back pressure than traditional packed columns, and can be repeatedly used.

Description

technical field [0001] The present invention belongs to the field of analytical chemistry. It specifically relates to an anion-exchange on-line purification solid-phase extraction monolithic column, especially a polymer monolithic column formed by the copolymerization reaction of dimethylaminoethyl methacrylate and ethylene glycol dimethacrylate in a stainless steel chromatographic column. method and application. Background technique [0002] As a new solid phase extraction material in rapid development, the monolithic column has good permeability and small mass transfer resistance because of its special penetrating hole structure, which improves the extraction efficiency. The advantages of fast mass transfer, easy modification, and reusability have been used more and more. Compared with packed extraction columns, the use of monolithic columns not only saves the tedious filling process, but also eliminates the The unique penetrating holes provide large-pore channels for th...

Claims

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Application Information

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IPC IPC(8): B01J41/12C08F220/34C08F220/28B01J41/20G01N30/06G01N30/08
CPCB01J41/20C08F220/34G01N30/06G01N30/08G01N2030/062C08F220/281
Inventor 艾连峰王曼曼
Owner INSPECTION & QUARANTINE TESTING CENT OF HEBEI ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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