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Gel chromatographic column and detection method for detecting poly brominated diphenyl ethers and metabolites thereof through GC-MC (gas chromatography and mass spectrography)

A gel chromatographic column and polybrominated diphenyl ether technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of interference of organic pollutant detection results, influence of detection results, sample impurity content, etc., to achieve accuracy promotion, pollution Small, less toxic effect

Active Publication Date: 2015-09-09
CHINA CERTIFICATION & INSPECTION GRP HUBEI CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the relatively mature detection method for the determination of PBDEs and metabolites is gas chromatography-mass spectrometry, but the accuracy of the results is largely limited by the impurity content of the sample
If these impurities are not treated, they will cause great interference to the detection results of subsequent organic pollutants and affect the detection results

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Take 100g of polystyrene gel, soak it in 500mL of cyclohexane:ethyl acetate (1:1), shake well, and then swell, the swelling time is one day, after the swelling is balanced, pour out the supernatant and suspended particles Impurities, spare. Take a clean chromatographic column (ID: 2.5cm×L:20cm), add about 5cm of cyclohexane: ethyl acetate (1:1), let it stand until there is no The air bubbles overflow, then open the piston, squeeze the silicone hose, discharge the air bubbles under the glass sand core filter plate and between the piston, make the solvent fill this part of the space, and then close the piston. Pour the swollen polystyrene gel and solvent into a beaker, stir well until the polystyrene gel is evenly suspended in the solvent to prepare a gel suspension, and then slowly pour the gel suspension from the top of the chromatographic column Pour it into the chromatographic column to allow the gel suspension to settle naturally. When the gel suspension at the bott...

Embodiment 2

[0035] Take 100g of polystyrene gel, soak it in 800mL of cyclohexane: ethyl acetate (1:1), shake well, and then swell, the swelling time is one day, after the swelling is balanced, pour out the supernatant and suspended particles Impurities, spare. Take a clean chromatographic column (ID: 3cm×L:30cm), add about 7.5cm of cyclohexane: ethyl acetate (1:1), let it stand until there is no The air bubbles overflow, then open the piston, squeeze the silicone hose, discharge the air bubbles under the glass sand core filter plate and between the piston, make the solvent fill this part of the space, and then close the piston. Pour the swollen polystyrene gel and solvent into a beaker, stir well until the polystyrene gel is evenly suspended in the solvent to prepare a gel suspension, and then slowly pour the gel suspension from the top of the chromatographic column Pour it into the chromatographic column to allow the gel suspension to settle naturally. When the gel suspension at the bot...

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Abstract

The invention provides a gel chromatographic column for detecting poly brominated diphenyl ethers and metabolites thereof through a GC-MC (gas chromatography and mass spectrography) method. The gel chromatographic column is prepared by the method comprising the following steps: weighing gel and a solvent, mixing the gel in the solvent, shaking to be uniform and swelling; taking a dry and clean chromatographic column, adding the solvent into the chromatographic column, discharging air bubbles between the lower part of a glass sand core filter plate and a piston, so that the space is filled with the solvent; and pouring the gel suspension liquid into the chromatographic column, and adding sea sand on the gel layer, thereby obtaining the gel chromatographic column. The preparation method of the gel chromatographic column is simple, complicated matrix effect can be overcome, and multiple impurities in the matrix containing organic pollutants can be separated, so that the multiple impurities can be effectively removed, and influences to follow-up detection for the organic pollutants are avoided. The invention further provides a method for detecting poly brominated diphenyl ethers and metabolites thereof based on the gel chromatographic column. The method has the advantages of simplicity in operation, good reproducibility, high sensitivity and high accuracy.

Description

technical field [0001] The invention relates to a preparation method of a gel chromatographic column for detecting polybrominated diphenyl ethers and metabolites by gas chromatography, and a detection method for detecting polybrominated diphenyl ethers and metabolites thereof by the gel chromatographic column, belonging to the technical field of environmental or food detection. Background technique [0002] At present, there are more and more types of organic pollutants in the environment and food, such as polybrominated diphenyl ethers and their metabolites, which are a class of halogenated organic brominated flame retardants (BFRs). Due to their good flame retardancy, they are used in industrial fields It is widely used in various commercial products, such as electrical and electronic products and textiles. Commercial PBDE products mainly include Penta-, Octa-, and Deca-BDEs. Such products have been widely distributed in the natural environment due to their physicochemica...

Claims

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Application Information

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IPC IPC(8): G01N30/60G01N30/88
Inventor 胡小钟胡德聪陈魏吴斌林长军
Owner CHINA CERTIFICATION & INSPECTION GRP HUBEI CO LTD
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