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A rapid qualitative detection method for polychlorinated biphenyl pollutants

A qualitative detection, polychlorinated biphenyl technology, applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of time-consuming operation, high analysis cost, difficulty in identification and screening at the same time, etc., to eliminate false positives, save solvents and The effect of processing time

Inactive Publication Date: 2011-12-14
RES CENT FOR ECO ENVIRONMENTAL SCI THE CHINESE ACAD OF SCI +1
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0008] The purpose of the present invention is to provide a method for the qualitative detection of polychlorinated biphenyls in soil and / or sediments, which overcomes the high cost of analysis, time-consuming operation, analysis only for specific monomers, and difficulty in simultaneous identification in existing PCBs analysis techniques Defects such as screening 209 PCBs homologues

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  • A rapid qualitative detection method for polychlorinated biphenyl pollutants
  • A rapid qualitative detection method for polychlorinated biphenyl pollutants
  • A rapid qualitative detection method for polychlorinated biphenyl pollutants

Examples

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Embodiment 1

[0025] Embodiment 1, the selection of accelerated solvent extraction conditions

[0026]Preparation of spiked soil samples: Select representative PCBs pollutants substituted by different chlorine atoms, and use the background soil (5.00g) without PCBs pollution collected in the border area of ​​Xinjiang to carry out the spike recovery experiment to determine the accelerated solvent extraction conditions. The operation steps are as follows: Accurately weigh 5.00 g of the above-mentioned soil, add 50 μL of PCBs mixed standard (concentration is 1.2 μg / mL) to the soil, and the concentration level of each single PCBs in the soil after adding the standard is 0.012 mg / kg; Mix well, seal it tightly, and place it in a dry and cool place overnight for later use.

[0027] The extraction solvent is one of the important factors affecting the recovery rate. When other extraction conditions are fixed, four different polarities of n-hexane, n-hexane:dichloromethane (1:1, volume ratio), dichlo...

Embodiment 2

[0028] Embodiment 2, optimization of gel permeation chromatography purification conditions

[0029] According to the purification principle of gel permeation chromatography, corn oil (COFCO, China) was selected as the marker of interfering substances in the purification process, and perbromethrin (AccuStandard, the United States; molecular weight 665.01) was used as the marker of the target substance to determine The collection time to separate target substances from interfering substances. The Bio-Beads SX3 column was selected, and the peak elution time of corn oil and perbromethrin was determined under the condition that the mixture of ethyl acetate and cyclohexane with a volume ratio of 1:1 was used as the mobile phase and the flow rate was 4.7mL / min. The results showed that the peak time of corn oil was 5-9.2min, and the peak appeared at 7.1min, and the peak time of perbromethrin was 9.5-13.5min, and the peak appeared at 11.9min. Therefore, when using the above method to ...

Embodiment 3

[0031] Embodiment 3, determination of elution conditions in Florisil solid-phase extraction purification mode

[0032] Select representative PCBs pollutants substituted by different chlorine atoms to optimize the elution conditions of Florisil. The solid-phase extraction cartridge was a Florisil extraction cartridge (Supeclo, USA; 500mg, 6mL). The solid-phase extraction cartridge was activated with 6mL of methanol and 6mL of n-hexane in sequence, and the cartridge should be kept moist during the activation process. When the n-hexane liquid level in the small column was about 1 mm away from the upper sieve plate, turn off the solid phase extraction device, take 50 μL of PCBs mixed standard (concentration of 1.2 μg / mL) and dilute it to about 1 mL with n-hexane, and transfer it to the small column. Use different volumes and different types of solvents for rinsing, take the eluent into the K-D concentrator, then blow it to nearly dry with soft nitrogen and replace the solvent, and...

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Abstract

The invention discloses a method for qualitatively detecting polychlorinated biphenyl in soil and / or sediment. The method comprises the following steps of: (1) extracting the soil and / or sediment to be detected by adopting an accelerated solvent extraction method, thereby acquiring an extracting solution; (2) purifying the extracting solution through a gel permeation chromatograph, thereby acquiring an extract; (3) eluting the extract through a solid phase extraction column, and collecting the eluent; and (4) analyzing the eluent by a gas chromatograph-mass spectrometer so as to acquire full scan data, and then performing deconvolution analysis on the acquired full scan data according to a retention time locking database in the gas chromatograph-mass spectrometer, thereby qualitatively detecting the polychlorinated biphenyl in the soil and / or water body sediment to be detected.

Description

technical field [0001] The invention relates to a rapid qualitative detection method for polychlorinated biphenyls (PCBs) pollutants, in particular to a high-throughput, rapid qualitative detection method for PCBs in sediment and / or soil. Background technique [0002] Polychlorinated biphenyls (PCBs) are a class of chlorinated aromatics produced by chlorinating biphenyls at high temperatures under the action of metal catalysts, and their general molecular formula can be expressed as (C 12 h 10 ) n Cl m , according to the number of substitutions of chlorine atoms and the position of substitution, there are a total of 209 homologues. [0003] PCBs are one of the 12 persistent organic pollutants (POPs) proposed by the United Nations Environment Program (UNEP) in 1977 and banned in the Stockholm Convention signed in 2001. It is an endocrine disruptor, which is very harmful to the nervous system, reproductive system and immune system of animals and humans, and even induces ca...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 王子健卜庆伟王东红张东罗茜
Owner RES CENT FOR ECO ENVIRONMENTAL SCI THE CHINESE ACAD OF SCI
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