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
  • Description
  • 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

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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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Example Embodiment

[0025] Example 1. 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) collected in Xinjiang border areas without PCBs pollution to carry out spike recovery experiments to determine the conditions for accelerated solvent extraction. The operation steps are as follows: accurately weigh 5.00g of the above-mentioned soil, add 50μL of PCBs mixed standard (concentration of 1.2μg / mL) to the soil, and the concentration level of each individual PCBs in the soil after adding the standard is 0.012mg / kg; Mix well, airtightly, place in a dry and cool place overnight, set aside.

[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), dichloromethane and acetone are used. ...

Example Embodiment

[0028] Example 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 tetrabromothrin (AccuStandard, USA; molecular weight 665.01) was used as the marker of the target substance to determine The collection time to separate the target from the interfering substance. The Bio-Beads SX3 column was selected, and the peak time of corn oil and tetraprothrin was determined when a mixture of ethyl acetate and cyclohexane at a volume of 1:1 was used as the mobile phase and the flow rate was 4.7 mL / min. The results showed that the peak time of corn oil was 5-9.2min, the peak appeared at 7.1min, the peak time of tetrabromothrin was 9.5-13.5min, and the peak appeared at 11.9min. Therefore, when the above method is used to purify the pollutants, the initial collection time is initially...

Example Embodiment

[0031] Example 3 Determination of elution conditions in Florisil solid phase extraction purification method

[0032] Select representative PCBs pollutants substituted by different chlorine atoms to optimize the elution conditions of Florisil. The solid phase extraction cartridge is a Florisil extraction cartridge (Supeclo, USA; 500mg, 6mL). The solid phase extraction cartridge is activated with 6mL methanol and 6mL n-hexane in sequence. Note that the cartridge should be kept moist during the activation process. When the liquid level of n-hexane in the small column is about 1 mm away from the upper sieve, close the solid phase extraction device, take 50 μL of PCBs mixed standard (concentration of 1.2 μg / mL) and dilute with n-hexane to about 1 mL, and transfer to the small column. Rinse with different volumes and different types of solvents, take the eluent in the K-D concentrator, and then use gentle nitrogen to blow it to near dryness and replace the solvent, and dilute it to 0.5...

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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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