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Method for simultaneously detecting 21 hydroxyl polybrominated diphenyl ethers (OH-PBDEs) in soil

A technology of hydroxypolybrominated diphenyl ethers and soil, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of environmental and human health threats, high biological toxicity, lack of reliable and effective analysis methods, etc., achieve fast analysis speed, reduce matrix Interfering, avoiding cumbersome and dangerous effects

Inactive Publication Date: 2016-08-24
RES CENT FOR ECO ENVIRONMENTAL SCI THE CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, the researchers found that OH-PBDEs exhibited higher biological toxicity than their parent PBDEs in some aspects, posing a greater threat to the environment and human health
At present, reports on the pollution status of OH-PBDEs in soil are limited to congeners with a bromine atom substitution number less than 5, and there have been no reports on high-brominated OH-PBDEs (bromine atom substitution number greater than 5) in the environment. Reliable and effective analytical method

Method used

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  • Method for simultaneously detecting 21 hydroxyl polybrominated diphenyl ethers (OH-PBDEs) in soil
  • Method for simultaneously detecting 21 hydroxyl polybrominated diphenyl ethers (OH-PBDEs) in soil
  • Method for simultaneously detecting 21 hydroxyl polybrominated diphenyl ethers (OH-PBDEs) in soil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0095] Example 1 Evaluation of recovery of hydroxy-polybrominated diphenyl ethers in blank soil samples

[0096]Weigh 1.0 g of freeze-dried soil and add 21 kinds of OH-PBDEs standard solutions at three concentration levels (5, 10, 20 ng / g). At the same time, 10 ng of internal standard 13C-6-OH-BDE-47 was added and aged for 24 hours. Add 2mL 37% HCl and 10mL isopropanol, mix well, then add 5-10mL 1:1 n-hexane / MTBE, shake at 120-160r / min for 10-24h, then centrifuge at 3000-4000r / min for 5-30min, take the organic Put the phase into a clean centrifuge tube, add 5-10mL 1:1 n-hexane / MTBE to repeat the extraction twice, combine the organic phases, blow dry with nitrogen, dissolve in 2mL n-hexane, add 1-2.5mL NaOH solution (0.5mol / LNaOH dissolved in 50% ethanol) for extraction, the organic phase was removed, the aqueous phase was extracted again with 2 mL of n-hexane, 300-500 μL of 2M HCl was added to the aqueous phase, and extracted with 2 mL of n-hexane:MTBE (9:1, v / v) Three time...

Embodiment 2

[0100] Example 2 Analysis of OH-PBDEs in environmental soil samples of plastic waste disposal sites

[0101] The soil of the plastic waste disposal site in Xinle City, Hebei Province was selected as the analysis object. The analysis methods and results are as follows:

[0102] Weigh 1.0-5.0g of freeze-dried soil and add internal standard 13 C-6-OH-BDE-47 10ng, aging for 24h; add 2mL 37% HCl and 10mL isopropanol, mix well, then add 5-10mL 1:1 n-hexane / MTBE, shake at 120-160r / min for 10-24h , then centrifuge at 3000-4000r / min for 5-30min, take the organic phase into a clean centrifuge tube, add 5-10mL 1:1 n-hexane / MTBE to repeat the extraction twice, combine the organic phase, blow dry with nitrogen, dissolve in 2mL n-hexane, add 1-2.5mL NaOH solution (0.5mol / L NaOH dissolved in 50% ethanol) for extraction, remove the organic phase, extract the water phase again with 2mL n-hexane, add 300-500μL 2M HCl to the water phase, and wash with 2mL n-Hexane: MTBE (9:1, v / v) was extracte...

Embodiment 3

[0106] Example 3 Analysis of OH-PBDEs in environmental soil samples of electronic waste dismantling sites

[0107] The soil of the electronic waste dismantling site in Qingyuan City, Guangdong Province was selected as the analysis object. The analysis methods and results are as follows:

[0108] Weigh 1.0-5.0g of freeze-dried soil and add internal standard 13 C-6-OH-BDE-47 10ng, aging for 24h; add 2mL 37% HCl and 10mL isopropanol, mix well, then add 5-10mL 1:1 n-hexane / MTBE, shake at 120-160r / min for 10-24h , then centrifuge at 3000-4000r / min for 5-30min, take the organic phase into a clean centrifuge tube, add 5-10mL 1:1 n-hexane / MTBE to repeat the extraction twice, combine the organic phase, blow dry with nitrogen, dissolve in 2mL n-hexane, add 1-2.5mL NaOH solution (0.5mol / L NaOH dissolved in 50% ethanol) for extraction, remove the organic phase, extract the water phase again with 2mL n-hexane, add 300-500μL 2M HCl to the water phase, and wash with 2mL n-Hexane: MTBE (9:1...

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Abstract

The invention discloses a method for simultaneously detecting 21 hydroxyl polybrominated diphenyl ethers (OH-PBDEs) in soil. The method includes the following steps that 1, a soil sample to be detected is extracted with organic solvent, and the organic solvent is selected from normal hexane, acetonitrile, methyl alcohol, dichloromethane, methyl tertiary butyl ether and NaOH-ethyl alcohol; 2, an extracting solution obtained in the step 1 is concentrated and purified; 3, a product in the step 2 is detected through an ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometer and compared with a hydroxyl polybrominated diphenyl ether standard substance in parallel operation to obtain quantitative results. The method has the advantages of being high in detection speed, accurate in result, high in recovery rate, low in detection limit, high in sensitivity and matrix interference resistance and the like.

Description

technical field [0001] The invention relates to a method for simultaneously detecting monobromo to octabromo and 21 kinds of hydroxy polybrominated diphenyl ethers in soil samples. Background technique [0002] Soil is an important part of the ecological environment, and it is also the main collection area of ​​environmental pollutants. With the rapid development of industrial and agricultural production, soil pollution has become increasingly serious, which has become one of the important factors restricting the sustainable development of agriculture and endangering human health. Pollutants can migrate to the surrounding soil through leaching, volatilization, surface runoff, and wet and dry deposition, and then enter the food chain through plants or animals and produce biomagnification effects, bringing great potential risks to human survival and health. [0003] Polybrominated diphenyl ethers (PBDEs) are additive flame retardants widely used in industrial and household pr...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027
Inventor 温蓓许学慧张宏娜王森黄红林张淑贞
Owner RES CENT FOR ECO ENVIRONMENTAL SCI THE CHINESE ACAD OF SCI
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