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Perfluoro-capillary extraction monolithic column and preparation method and application thereof

A monolithic column and capillary technology, which is applied in the field of preparation of perfluorocapillary extraction monolithic columns, can solve the problems that the packed extraction column cannot realize remote enrichment sampling, large mass transfer resistance, and low extraction efficiency, and achieves a simple and fast preparation method Reliable, adsorption-specific avoidance, shortened analysis time effects

Inactive Publication Date: 2011-09-14
HUNAN NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The existing pretreatment of perfluorinated compounds is mainly through the packed extraction column, which has high mass transfer resistance and low extraction efficiency, so the detection sensitivity is low, and it is difficult to remove the interference of impurities; in addition, the packed extraction column cannot realize remote enrichment. Set sampling, so the analysis time is longer and the transportation cost is higher
However, there is no report on perfluorinated capillary extraction monolithic column and its preparation method and its application in pretreatment and sample collection of perfluorinated compounds.

Method used

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  • Perfluoro-capillary extraction monolithic column and preparation method and application thereof
  • Perfluoro-capillary extraction monolithic column and preparation method and application thereof
  • Perfluoro-capillary extraction monolithic column and preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0025] The preparation method of perfluorinated capillary extraction monolithic column comprises the following steps:

[0026] (1) Pretreatment: Wash the quartz capillary with an inner diameter of 75 μm with 1 M NaOH overnight, and then wash with H 2 O, 0.1 M HCl, and H 2 Rinse with O, then heat at 180 °C for 3 h in a nitrogen atmosphere for later use;

[0027] (2) Sol-gel treatment: 0.11 g polyethylene glycol (PEG) and 0.113 g urea (Urea) were dissolved in 1.25 ml 0.01 M HAc, and 0.55 ml tetramethoxysilane (TMOS) was slowly added dropwise. The mixture was vigorously stirred under ice bath for 60 min. Sonicate at 0 °C for 5 min, fill the sol into the capillary, seal both ends of the capillary with a rubber pad, place it in a constant temperature water bath, and react at 40 °C for 24 h. Then the capillary was treated at 120 °C for 3 h. Rinse with water and methanol in turn, and then slowly dry at 50 °C for 24 h. Finally, the monolithic column was placed in a gas chromatogr...

Embodiment 2

[0035] The perfluorinated capillary extraction monolithic column (a) prepared in Example 1 is applied to the pretreatment and sample collection of perfluorinated compounds, including the following steps:

[0036] (1) Activation: Rinse the monolithic perfluorocapillary extraction column with 100 μL methanol and 100 μL water respectively, and squeeze out the liquid remaining in the monolithic column;

[0037] (2) Sample loading: Inject 2 mg / L perfluorooctane sulfonic acid (PFOS) aqueous solution into the monolithic column at a flow rate of 5 μL / min with a syringe pump, collect 10 μL of each outflow as a sample solution, and collect a total of 110 μL.

[0038] (3) Elution: use a syringe pump to elute with methanol at a flow rate of 5 μL / min, collect 10 μL of each outflow as a sample solution, and collect a total of 30 μL.

[0039] (4) Detection: All sample solutions are analyzed by liquid chromatography tandem mass spectrometer.

[0040] The liquid chromatography tandem mass sp...

Embodiment 3

[0046] Example 1 Comparison of C18 capillary extraction monolithic column applied to the pretreatment and sample collection of perfluorinated compounds, including the following steps:

[0047] (1) Activation: Rinse the C18 capillary extraction monolithic column with 100 μL methanol and 100 μL water respectively, and squeeze out the liquid remaining in the monolithic column;

[0048] (2) Sample loading: Inject 2 mg / L perfluorooctane sulfonic acid (PFOS) aqueous solution into the monolithic column at a flow rate of 5 μL / min with a syringe pump, collect 10 μL of each outflow as a sample solution, and collect a total of 110 μL.

[0049] (3) Elution: use a syringe pump to elute with methanol at a flow rate of 5 μL / min, collect 10 μL of each outflow as a sample solution, and collect a total of 30 μL.

[0050] (4) Detection: All sample solutions are analyzed by liquid chromatography tandem mass spectrometer.

[0051] Liquid chromatography tandem mass spectrometry conditions are con...

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Abstract

The invention discloses a perfluoro-capillary extraction monolithic column and a preparation method and application thereof. The perfluoro-capillary extraction monolithic column is a monolithic column in which silica gel matrix is polymerized in situ in a quartz capillary tube with diameter of 75 to 530 microns and perfluoro functional groups are bonded on the surface of the silica gel matrix. The perfluoro functional groups comprise perfluoro-octyl (C6F13), perfluoro-decyl (C8F17), N-perfluorooctanoic sulfonyl and derivatives thereof. The monolithic column can be used for enriching a series of trace perfluoro-chemicals, such as perfluorooctane sulfonate (PFOS), perfluorooctane carboxylate (PFOA), perfluorodecanoate (PFDA), perfluorohexyl sulfonate (PFHXS) and the like. The preparation method of the monolithic column is simple, fast and reliable, the average adsorption quantity can reach over 6.0*10<-2>mug, and the average enrichment times is 30 times; the average recovery rate is over 90 percent, the sensitivity of analysis and detection is greatly improved, and interference of impurities is avoided; and the monolithic column is convenient and fast to carry, a trace perfluoro-chemical sample can be directly enriched at a remote acquisition point, the transport cost is reduced, and the analysis time is shortened.

Description

technical field [0001] The invention relates to the field of analytical chemical sample collection and sample pretreatment, in particular to a preparation method and application of a perfluorinated capillary extraction monolithic column. Background technique [0002] Perfluorinated compounds (PFCs) mainly include perfluorooctanoic acid (PFOA), perfluorooctane sulfonic acid (PFOS), perfluorodecanoic acid (PFDA), etc. They are widely used as surfactants in textiles, leather, Pesticides, carpets, furniture and other fields. Studies have shown that it has various toxic effects such as causing lipid peroxidation, teratogenicity, carcinogenicity and neurotoxicity in the body. Perfluorinated compounds are difficult to degrade in the environment, can be transported over long distances, and accumulate and amplify in animals and humans along the food chain, so perfluorinated compounds have been identified as a persistent organic pollutant. [0003] The existing pretreatment of perfl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/60G01N30/50G01N30/08
Inventor 陈波黄科
Owner HUNAN NORMAL UNIVERSITY
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