Gas phase chromatogram- ion trap tandem mass spectrometry method for detecting organochlorine pesticide

A technology of tandem mass spectrometry and gas chromatography, which is applied in the field of rapid quantitative detection of target compounds of organochlorine pesticides, can solve the problems of time-consuming and labor-consuming pretreatment steps, low detection sensitivity, etc., and achieve low detection cost, high sensitivity, and improved Effect of Detection Sensitivity

Inactive Publication Date: 2011-05-04
NANJING UNIV
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Problems solved by technology

[0005] Aiming at the shortcomings of organochlorine pesticides in atmospheric environment samples, such as interference from other chlorinated compounds, time-consuming and labor-consuming pretreatment steps, and low detection sensitivity, the present invention provides a method for detecting organochlorine pesticides in the atmosphere by gas chromatography-ion trap tandem mass spectrometry. Chromatography-ion trap mass spectrometry (GC / ITMS) established and optimized the detection method of 21 kinds of organochlorine pesticides by secondary mass spectrometry (MS / MS). The conventional detection method has better selectivity and higher sensitivity, and utilizes the advantages of MS / MS in compound identification to realize rapid and accurate quantitative detection of 21 organochlorine pesticides in atmospheric samples without pretreatment , can greatly save analysis time and cost

Method used

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  • Gas phase chromatogram- ion trap tandem mass spectrometry method for detecting organochlorine pesticide
  • Gas phase chromatogram- ion trap tandem mass spectrometry method for detecting organochlorine pesticide
  • Gas phase chromatogram- ion trap tandem mass spectrometry method for detecting organochlorine pesticide

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Effect test

Embodiment 1

[0025] Embodiment 1: (chromatography, mass spectrometry conditions under initial condition)

[0026] (1) Configuration of standard solution: prepare 21 OCPs standard solutions (tetrachlorom-xylene, α-666, lindane, β-666, heptachlor, δ-666) with a concentration of 1000pg / μL 6. Aldrin, epoxy heptachlor, γ-chlordane, chlordane, dieldrin, p, p'-Didiyi, endrin, α-endosulfan, p, p'-dididi , endrin, p, p'-DDT, endosulfan sulfate, endrin ketone, methoxychlor, decachlorobenzene).

[0027] (2) Chromatographic conditions: the chromatographic column adopts DB-XLB chromatographic column, and the specification is 15mx0.25mmx0.25m. The temperature was programmed to rise to 100°C (hold for 2min), then to 175°C at 7.5°C / min, then to 220°C at 2.5°C / min, and finally to 270°C at 25°C / min (hold for 5min). Injection port temperature 250°C; splitless injection 1L. Helium (purity>99.999%) was used as the carrier gas with a flow rate of 1.0 mL / min (constant flow mode).

[0028] (3) Mass spectromet...

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 21 kinds of organochlorine pesticide standard substances are the same as in Example 1;

[0031] (2) Secondary mass spectrometry (MS 2 ) Conditions: 21 kinds of OCPs standard substances of 1000pg / μL concentration were used in this embodiment

[0032] Operation under the chromatographic and mass spectrometry conditions in (1) obtains the corresponding primary mass spectrum (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 characteristic ion peak with the highest abundance [M] + As the precursor ion in the MS / MS condition, the default parameter value of MEE is set to 0.3, the EV parameter value is set to 1.5V, and the two most abundant fragment ions in the fragm...

Embodiment 3

[0036] Embodiment 3: (optimize the secondary mass spectrometry condition: the optimization of MEE parameter)

[0037] (1) The concentration, chromatographic conditions, and mass spectrometry conditions of 21 kinds of organochlorine pesticide standard substances are the same as in Example 1:

[0038] (2) Secondary mass spectrometry (MS 2 ) conditions: refer to Example 2 (2) for the selection of parent ions and product ions of 21 organochlorine pesticide target compounds. Set the parameter value of MEE (maximum resonance energy) to 0.225, the parameter range of EV (dissociation voltage) from 0.25 to 3.5V with an interval of 0.25V, a total of 14 parameters, select 2 product ions as quantitative ions, and obtain The corresponding peak area for each compound;

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Abstract

The invention provides a method for detecting organochlorine pesticides in the atmosphere by means of gas chromatography-ion trap tandem mass spectrometry , which comprises the following steps: collecting samples, extracting samples, purifying and concentrating samples, and detecting the samples by chromatography-ion trap mass spectrometry. The invention enjoys higher selectivity and sensitivity than the prior detection methods of the target compounds through optimization of gas chromatography and tandem mass spectrometry conditional parameters. The invention adopts the selection response monitoring techniques (SRM) of gas chromatography / ion trap tandem mass spectrometry (GC / ITMS) to remove the disadvantage that the selectivity and sensitivity of trace amount OCPs in complex background matrix of the prior detectors can not be achieved at the same time. The invention has the advantages of low detecting cost, and accurate and reliable positioning, thus presenting very obvious superiority over the traditional detection devices GC / ECD, GC / LRMS and GC / HRMS.

Description

technical field [0001] The invention relates to a rapid quantitative detection method for trace-level organochlorine pesticides in the atmospheric environment, specifically, it is a selected reaction monitoring (selected reaction monitoring) using gas chromatography-ion trap mass spectrometry (ion trap mass spectrometry, ITMS). SRM) technology realizes the method of rapid quantitative detection of 21 kinds of organochlorine pesticide target compounds in gas and solid atmospheric samples. Background technique [0002] Organochlorine pesticides (Organochlorine Pesticides, OCPs), as an important agricultural insecticide for human beings, are a class of persistent organic pollutants (Persistent Organic Pollutants, POPs) with the widest application range and the longest use time. Half a century ago, scientists discovered that these compounds have stable chemical properties, are not easy to degrade in the environment, and are fat-soluble and can be enriched and amplified along the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88G01N30/06G01N30/72
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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