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Method for rapidly detecting polybrominated diphenyl ether residue in sample

A polybrominated diphenyl ether and detection method technology, which is applied in the field of rapid sample processing of polybrominated diphenyl ether residues, can solve the problems of large solvent consumption, high cost, time-consuming detection, etc., and achieve the effect of less analysis sample, fast extraction speed, fast automation

Inactive Publication Date: 2009-09-09
陈军 +3
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to provide a rapid detection method for polybrominated diphenyl ether residues in samples, especially in textiles, which solves the problems in the prior art that extraction and detection require a large amount of solvent, time-consuming detection, and high cost.

Method used

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  • Method for rapidly detecting polybrominated diphenyl ether residue in sample
  • Method for rapidly detecting polybrominated diphenyl ether residue in sample
  • Method for rapidly detecting polybrominated diphenyl ether residue in sample

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] The content detection of polybrominated diphenyl ethers in the standard lining product of embodiment 1

[0037] Materials and methods

[0038] Instruments and reagents:

[0039] HP6890GC gas chromatograph with 5975MSD, Anggilent TM (CA, US); HP-5 (15m×0.25mm×0.25μm, Fused silica capillary column), Angilent TM (CA, US); solid phase microextraction device (with 15mL operating platform): Supelo TM (PA, USA), dedicated for GC; SPME extraction fiber: 7 μm polydimethylsiloxane (PDMS), Supelo TM (PA, USA); Branson200ULTRASONIC Cleaner ultrasonic machine, Branson TM (MI, USA); chromatography vial: 22ML, La-pha-pack TM (Frankfurt, GM). Standard lining: multi-fiber standard lining MFF#10A (ISO105 / F10-1989), Textile Industry Standardization Institute.

[0040] Acetone (Acetone): HPLC grade, purchased from Ficher TM (MA, USA); Cyclohexane (Cyclohexane): HPLC grade, MERCK TM (NJ, USA); pure water (Water): HPLC grade, MERCK TM (NJ, USA); Sodium chloride (NaCl): AR.; Standar...

Embodiment 2

[0069] The optimization of solid-phase microextraction condition in the content detection method of polybrominated diphenyl ether in the standard lining product of embodiment 2

[0070] The aqueous solution containing part of the target compound at 10 μg / L is used as the sample matrix, that is, different comparisons are taken, and the ideal gas-liquid equilibrium conditions are selected according to the signal response (chromatographic peak area) of the target compound in GC / MS. The results show that the detection result is the most ideal when the ratio is 1:2 (v / v). Therefore, the bottom liquid volume of the extraction system was determined to be 10 mL.

[0071] In view of the factors that may affect the efficiency of solid-phase microextraction, under the determined bottom liquid conditions, the research uses a micro-injector to take a 100ng / mL standard solution in a 50mL volumetric flask, evaporate the solvent and dilute it with water to conduct solid-phase microextraction....

Embodiment 3

[0073] Example 3 The precision and recovery investigation test of the content detection method of polybrominated diphenyl ethers in standard lining products

[0074] Select the standard lining, and prepare a small standard sample with a standard solution of the target compound at a concentration of 10 ng / ml. Each sample was measured 10 times in parallel, and a blank test was performed on samples of the same material. The average value of the three blank measurement results was taken as the background, and the standard addition recovery was calculated after deducting the blank value. The measurement results are shown in Table 2. The recoveries of the blank spiked compounds were 81.9-103.1%, the RSDs were 2.2-8.9%, and the recoveries of the matrix spiked compounds were 71.9-107.1%, the RSDs were 5.8-10.1%.

[0075] Table 2 Blank standard addition and matrix (fabric) standard addition recovery measurement result

[0076]

[0077] Among them, BDE-099: 2,2', 4,4', 5-pentabromod...

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Abstract

The invention discloses a method for rapidly detecting polybrominated diphenyl ether residue in a sample, particularly in textiles. The method is characterized by comprising the following steps: (1) the sample is crushed, dipped in base solution and ultrasonically extracted in water bath, and solid phase microextraction is employed to concentrate a target compound; and (2) polybrominated diphenyl ether is qualitatively and quantitatively determined by gas chromatography-mass spectrometry after thermal desorption. The method helps effectively solve the problem of matrix effect that fabric fibers have no solvent extraction, obtains a satisfactory result for the analysis of a selected target compound, has the advantages of low organic solvent consumption, rapid extraction speed, less interference from impurities, high sample recovery rate and the like, and can be applicable to rapidly detecting polybrominated diphenyl ether flame retardant residue in textiles.

Description

technical field [0001] The invention belongs to the technical field of chemical instrument detection, and in particular relates to a rapid sample processing technology and detection method for polybrominated diphenyl ether residues in samples, especially textiles. Background technique [0002] Polybrominated diphenyl ethers (PBDEs) have the general chemical formula C 12 h (10-n) Br n O, according to the number and position of bromine atoms on the benzene ring, there are many homologues. It is a kind of persistent organic pollutants. It is very stable in the environment, difficult to degrade, and has high lipophilicity and low water solubility. Low in water, readily accumulates in sediments, bioaccumulates and enriches along the food chain. Commercial PBDEs are mixtures of brominated diphenyl ether congeners, mainly containing pentabromodiphenyl ether (PeBDE), octabromodiphenyl ether (OcBDE) and decabromodiphenyl ether (DeBDE), but also include other PBDEs. PeBDE is mainl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/72C07C43/29
Inventor 陈军朱建明柳艳朱振华
Owner 陈军
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