Method for detecting atmosphere granule trace polychlorinated biphenyls by ion trap tandem mass spectrometry

An atmospheric particulate matter and tandem mass spectrometry technology, which is applied in the field of ion trap tandem mass spectrometry to detect trace PCBs in atmospheric particulate matter, can solve the problems of time-consuming, labor-intensive, mutual interference, cumbersome steps, etc., to save analysis time and achieve accurate and reliable qualitative analysis , The effect of saving analysis costs

Inactive Publication Date: 2008-01-16
NANJING UNIV
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Problems solved by technology

[0006] Aiming at the problem of mutual interference between polychlorinated biphenyls and other chlorinated organic compounds in the analysis of atmospheric particulate matter samples, the present invention improves the cumbersome, time-consuming and labor-intensive purification and separation steps in the traditional analysis method, and uses gas chromatography / ion trap mass spectrometry (GC / ITMS) established and optimized the MS / MS detection method for 31 kinds of polychlorinated biphenyls (1-10 chlorinated compounds), using the advantages of MS / MS in compound qualitative, it can be achieved in only one step Purification treatment can quickly and accurately detect 31 kinds of PCB target compounds in atmospheric particles of different particle sizes, saving analysis time and cost

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  • Method for detecting atmosphere granule trace polychlorinated biphenyls by ion trap tandem mass spectrometry

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Embodiment 1: (chromatograph under initialization condition, mass spectrometry condition)

[0025] (1) Concentration of standard substance. Prepare 31 PCBs standard solutions with a concentration of 100pg / μL;

[0026] (2) Chromatography (GC) conditions: the chromatographic column adopts DB-XLB chromatographic column, and the specification is 15m×0.25mm (inner diameter)×0.25m (film thickness); 150°C, 2.5°C / min to 250°C (hold for 5min); inlet temperature 270°C; splitless injection 1L.

[0027] Helium (purity>99.999%) was used as the carrier gas, and the flow rate was 1.0 mL / min (constant flow mode).

[0028] (3) Mass spectrometry (MS) conditions: the ionization mode is EI ionization, the ionization voltage is 70eV, the ion source temperature is 250°C, and the transfer line temperature is 280°C.

Embodiment 2

[0029] Embodiment 2: (optimize the secondary mass spectrometry condition: select parent ion, product ion)

[0030] (1) The concentration, chromatographic conditions, and mass spectrometry conditions of 31 kinds of polychlorinated biphenyl standard substances are the same as in Example 1;

[0031] (2) Secondary mass spectrometry (MS 2 ) conditions: 31 kinds of PCBs standard substances with a concentration of 100pg / μL were operated under the conditions of the present embodiment (1) to obtain corresponding primary mass spectrometry (MS 1 ) spectrum, record the retention time (RT) of each target compound according to the peak order of the target compound in the chromatographic column, and select the molecular ion peak [M] + As the precursor ion in MS / MS conditions, the MEE parameter value is set to 0.3, the EV parameter value is selected to be 1.5V, and the two most abundant fragment ions [M-CI] in the fragmentation fragments of the precursor ion are selected [M-CI] + or [M-2CI]...

Embodiment 3

[0035] Embodiment 3: (optimize the secondary mass spectrometry condition: the optimization of MEE parameter)

[0036] (1) The concentration, chromatographic conditions, and mass spectrometry conditions of 31 kinds of polychlorinated biphenyl standard substances are the same as in Example 1;

[0037] (2) Secondary mass spectrometry (MS 2 ) conditions: the selection of parent ions and product ions of 31 polychlorinated biphenyl target compounds is detailed in Example 2 (2). Set the parameter value of MEE (maximum resonance energy) to 0.225, the parameter range of EV (dissociation voltage) from 0.5 to 6.0V with an interval of 0.25V, a total of 17 parameters, select 2 product ions as quantitative ions, and obtain by integration The peak area response of the response, from which the best peak area response is selected, and the total peak area is 60108;

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Abstract

The invention provides a method of detecting the trace polychlorinated biphenyls in atmospheric particulates by ion trap tandem mass spectrometry; the steps of the method comprises sample collection, sample leach, sample concentration and purification and the detection of pilot sample by chromatography-ion trap mass spectrometry; by optimizing the conditional parameters of gas phase chromatography and tandem mass spectrometry, the invention has better selectivity and better sensitivity in the detection of titled compound compared with the conventional detection method; the invention solves the mutual interference between PCBs and multi-chlorine organic compounds in the traditional analysis and detection method by SRM technique of gas phase chromatography/ion trap tandem mass spectrometry (GC/ITMS), and greatly simplifies the fussy steps of purification and separation in sample pretreatment; SRM technique has the advantages of sensitivity, selectivity, low detecting expense and reliable and accurate determination of the nature; therefore, the invention has remarkable advantage compared with the traditional detecting instrument such as GC/ECD,GC/LRMS,GC/HRMS.

Description

technical field [0001] The invention relates to a method for rapid and quantitative detection of trace polychlorinated biphenyl organic pollutants in atmospheric particulate matter, specifically, a method for realizing a simple purification by using gas chromatography / ion trap tandem mass spectrometry (GC / ITMS) technology On the basis of the pretreatment steps, it is an analytical method that can quickly and accurately detect 31 kinds of polychlorinated biphenyl (1-10 chlorinated) organic pollutants in atmospheric particles of different particle sizes. Background technique [0002] Polychlorinated Biphenyls (PCBs) are an important class of endocrine disruptors (EDCs) and persistent organic pollutants (Persistent Organic Pollutants, POPs). There are 209 compound monomers in total. Polychlorinated biphenyls have all the characteristics of persistent organic pollutants. They are not easy to degrade in the environment and have high fat solubility. They can be enriched and enlar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N1/20G01N30/08G01N30/14
Inventor 赵欣刘树深王格慧王晓栋高士祥冯建昉王连生
Owner NANJING UNIV
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