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Determination method of perfluorinated compound isomer in soil and/or plants

A technology of isomers and perfluorinated compounds, which is applied in the field of determination of isomers of perfluorinated compounds, can solve the problem of distinguishing few isomers, achieve more effective separation, less matrix interference, good selectivity

Inactive Publication Date: 2016-07-20
RES CENT FOR ECO ENVIRONMENTAL SCI THE CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the limitations of analytical methods, the current reports on PFASs pollution in soil and plants are almost all the total amount of PFOA, PFOS, etc., and the isomers are rarely distinguished.

Method used

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  • Determination method of perfluorinated compound isomer in soil and/or plants
  • Determination method of perfluorinated compound isomer in soil and/or plants
  • Determination method of perfluorinated compound isomer in soil and/or plants

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0105] The standard recovery rate of PFOA, PFOS and PFHxS isomers in the soil and plant sample of embodiment 1

[0106] Blank soil and plant samples (corn plants) were collected from the experimental field of Beijing Academy of Agriculture and Forestry Sciences. Soil samples were freeze-dried, ground and sieved (50 mesh) and stored in the refrigerator; plant samples were divided into roots, stems and leaves, washed thoroughly with tap water, rinsed with ultrapure water, freeze-dried and ground, and stored in the refrigerator. Store in the refrigerator. Weigh 3 parts of soil and plant samples respectively, 2.0g for each part of soil, and 0.5g for each part of plants (roots, stems and leaves), place them in polypropylene centrifuge tubes, and add 20μl PFOA, PFOS and PFHxS to each sample The mixed standard solution of isomers was aged in dark place for 24h.

[0107] Add 1.5mL0.4MNaOH, 1mL0.5MTBAHs, 2mL0.25MNa to the weighed soil and plant samples 2 CO 3 , then add 5mL MTBE, s...

Embodiment 2

[0109] The analysis of embodiment 2 environmental soil samples

[0110] The soil of two different sludge application fields in Dezhou City, Shandong Province was selected as the analysis object. The analysis method and effect are as follows:

[0111] The soil sample was freeze-dried, ground and sieved (50-mesh sieve), and 1.0-5.0 g of sludge was weighed to apply the soil to a polypropylene centrifuge tube, and 2 ng each of three alternative internal standards (MPFOA, MPFOS and MPFHxS) were added, Aging for 24h; add 1-3mL0.4MNaOH, 1-2mL0.5MTBAHs, 2-4mL0.25MNa 2 CO 3 , then add 5-10mLMTBE, shake and extract at 120-180r / min for 6-12h, then centrifuge at 3000-5000r / min for 10-30min, take the supernatant into a clean centrifuge tube, add 5-10mLMTBE to repeat the extraction twice, combine Extract solution; dry the extract solution with nitrogen gas, add methanol 1-2mL to dissolve the residue, add ultrapure water to 20-40mL, pass through a 0.22-0.45μm nylon membrane; pass the super...

Embodiment 3

[0117] The analysis of embodiment 3 environmental plant samples

[0118] The experimental crop (corn) in the sludge application field of Dezhou City, Shandong Province was selected as the analysis object. The analysis method and effect are as follows:

[0119] Wash the plant samples thoroughly with tap water, then rinse with ultrapure water, freeze-dry and grind; weigh 0.1-1.0g of plant samples into a polypropylene centrifuge tube, add 3 alternative internal standards (MPFOA, MPFOS and MPFHxS) 2ng each, aging for 24h; add 1-3mL0.4MNaOH, 1-2mL0.5MTBAHs, 2-4mL0.25MNa 2 CO 3 , then add 5-10mLMTBE, shake and extract at 120-180r / min for 6-12h, then centrifuge at 3000-5000r / min for 10-30min, take the supernatant into a clean centrifuge tube, add 5-10mLMTBE to repeat the extraction twice, combine Extract solution; dry the extract solution with nitrogen gas, add methanol 1-2mL to dissolve the residue, add ultrapure water to 20-40mL, pass through a 0.22-0.45μm nylon membrane; pass th...

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Abstract

The invention discloses a determination method of a perfluorinated compound isomer in soil and / or plants. The method comprises the following steps: (1) extracting a soil and / or plant sample with an ion pair extraction method; (2) concentrating and purifying an extracting solution obtained by the step (1); and (3) detecting a product of the step (2) with an ultra performance liquid chromatography-triple quadrupole tandem mass spectrometer, and comparing the product with an isomer standard product of parallel operation; and quantifying by adopting an internal standard method to obtain the content of each isomer of a perfluorinated compound. The determination method disclosed by the invention is accurate in detection result and has the advantages of high recycling rate, low detection limit, high sensitivity and strong matrix interference resisting capability.

Description

technical field [0001] The invention relates to a method for determining isomers of perfluorinated compounds in soil and / or plants. Background technique [0002] Perfluorochemicals (PFASs), represented by perfluoroalkyl carboxylic acids (PFCAs) and perfluoroalkyl sulfonic acids (PFSAs), are a class of persistent organic pollutants with environmental persistence, bioaccumulation, and biomagnification. The research on the environmental behavior of PFASs has become a hotspot in the field of environmental chemistry. It has been found that PFASs in the environment, especially perfluorooctane carboxylic acid (PFOA) and perfluorooctane sulfonic acid (PFOS), have a variety of linear and branched isomers, and various PFAS isomers in There are differences in behavior in the environment and may exhibit different enrichment, metabolism and toxicity effects in organisms. [0003] PFC isomers arise from how they are produced. Electrochemical fluorination and telomerization are the two ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/062
Inventor 温蓓张宏娜张淑贞
Owner RES CENT FOR ECO ENVIRONMENTAL SCI THE CHINESE ACAD OF SCI
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