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Detection method of perfluorocarboxylic acid compound

A technology of perfluorocarboxylic acid and detection method, applied in the field of chemical detection

Pending Publication Date: 2020-06-26
秦皇岛海关技术中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In summary, there are no reports on the detection method of perfluorocarboxylic acid compounds by bis(dimethylamino)methoxymethane derivatization by gas chromatography tandem mass spectrometry.

Method used

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  • Detection method of perfluorocarboxylic acid compound
  • Detection method of perfluorocarboxylic acid compound
  • Detection method of perfluorocarboxylic acid compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] Example 1 Quantitative Standard Curve Drawing, Method Detection Limit and Precision

[0057] (1) Take multiple parts of ethyl acetate solution, add appropriate amount of perfluorocarboxylic acid compound standard substance and internal standard therein, mix well,

[0058] (2) The concentration range of each perfluorocarboxylic acid standard substance in the standard curve is set as: 0.5-500ng / mL;

[0059] (3) Set 10 concentrations of the target substance (0.5, 1, 2, 5, 10, 20, 50, 100, 200, 500 ng / mL respectively); the concentration of the internal standard is 100 ng / mL.

[0060] (4) Add 20 μL of bis(dimethylamino)methoxymethane, and derivatize in an oven at 35° C. for 30 minutes.

[0061] (5) Perform instrumental testing according to the method of the present invention.

[0062] Take the concentration X of perfluorocarboxylic acid as the abscissa, and take the ratio Y of the peak area of ​​the perfluorocarboxylic acid derivative to the peak area of ​​the internal sta...

Embodiment 2

[0074] The optimization of embodiment 2 derivatizing agent adding amount

[0075] (1) Take 10 μL of 500 mg / L perfluorocarboxylic acid mixed standard solution and add it to the derivation bottle;

[0076] (2) Add 1 μL, 2 μL, 5 μL, 10 μL, 20 μL, and 50 μL of bis(dimethylamino)methoxymethane respectively, and dilute to 1 mL with ethyl acetate;

[0077] (3) React at 35° C. for 30 minutes, cool down, and transfer the solution after passing through a 0.22 μm organic filter membrane to an injection bottle for gas chromatography-tandem mass spectrometry (GC-MS / MS) detection.

[0078] The experimental results show that as the amount of derivatizer increases, the peak area of ​​perfluorocarboxylic acid derivatives gradually increases, and a larger peak area can be obtained in the range of 5-50 μL, of which 20 μL is the optimal value of the amount of derivatizer .

Embodiment 3

[0079] The optimization of embodiment 3 derivation time

[0080] (1) Take 10 μL of 500 mg / L perfluorocarboxylic acid mixed standard solution and add it to the derivation bottle;

[0081] (2) Add 20 μL of bis(dimethylamino)methoxymethane, and dilute to 1 mL with ethyl acetate;

[0082] (3) React at 35°C for 5, 10, 30, 60, 120, and 240 min respectively, cool down, and transfer the solution after passing through a 0.22 μm organic filter membrane to an injection bottle for gas chromatography-tandem mass spectrometry (GC- MS / MS) detection.

[0083] The experimental results show that the larger peak area can be obtained when the reaction time is within 5-240 minutes, and 30 minutes is the optimal time for the derivatization reaction.

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Abstract

The invention, which belongs to the technical field of chemical detection, particularly relates to a detection method of a perfluorocarboxylic acid compound. The method comprises the following steps:(1), carrying out a derivatization reaction on perfluorocarboxylic acid by taking bis(dimethylamino) methoxymethane as a derivatization reagent, and deriving the perfluorocarboxylic acid into bis(dimethylamino) methyl perfluorosubstituted alkane; (2), performing quantitative detection by adopting a gas chromatography-tandem mass spectrometry method; to be specific, setting the sample to be perfluorocarboxylic acid extracted from a target substance to be detected after a target substance is purified and enriched by combining an alkali digestion method and solid-phase extraction. The perfluorocarboxylic acid is perfluorocarboxylic acid with the carbon atom number of 2-20, and preferably, the perfluorocarboxylic acid is perfluorocarboxylic acid with the carbon atom number of 4-12.

Description

technical field [0001] The invention belongs to the technical field of chemical detection, and in particular relates to a detection method for perfluorocarboxylic acid compounds. Background technique [0002] Perfluoroalkylcarboxylic acids (PFCAs) are a class of persistent organic pollutants (POPs) consisting of a carbon backbone (typically 4–14 in length) linked to fluorine atoms and a carboxylic acid functional group. The unique physical and chemical properties of compounds endowed by fluorine atoms, including water repellency, oil repellency, heat resistance, and surfactant properties, make them widely used in industrial and commercial fields. The recalcitrant nature and global distribution of PFCAs allow them to persist in the environment and accumulate in biota. [0003] With the deepening of environmental toxicology research, PFCAs have been found to have toxicity in immunity, reproduction, development and neurology. Therefore, more and more countries and organizatio...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/72G01N30/86
CPCG01N30/02G01N30/06G01N30/7206G01N30/8637G01N2030/045G01N2030/067G01N2030/062
Inventor 崔宗岩纪涌彦曹彦忠黄学者李学民李阿丹
Owner 秦皇岛海关技术中心
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