Solid-phase membrane extraction and gas chromatography-tandem mass spectrometry detection method of organic chlorine compounds in water body

A technology of gas chromatography and tandem mass spectrometry, which is applied in the field of water quality and safety detection, can solve the problems of few researches on organochlorine compounds, easy to be interfered by impurities, and inaccurate characterization, and achieve high sensitivity, good reproducibility, and few operation steps Effect

Active Publication Date: 2017-03-15
MARINE FISHERIES RES INST OF ZHEJIANG
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  • Description
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Problems solved by technology

As a selective and highly sensitive detection instrument, gas chromatography-electron capture detection has high sensitivity and accuracy for the detection of organochlorine compounds, but it is easily interfered by impurities and the qualitative is not accurate enough
In recent years, researchers have carried out studies on the residues and distribution of organochlorine in some estuary areas, but there are not many studies on the residues of trace organochlorine compounds in water bodies

Method used

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  • Solid-phase membrane extraction and gas chromatography-tandem mass spectrometry detection method of organic chlorine compounds in water body
  • Solid-phase membrane extraction and gas chromatography-tandem mass spectrometry detection method of organic chlorine compounds in water body
  • Solid-phase membrane extraction and gas chromatography-tandem mass spectrometry detection method of organic chlorine compounds in water body

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Example 1: Determination of 18 organochlorine compounds in laboratory tap water

[0022] (1)C 18 Cleaning and Activation of Solid Phase Extraction Membranes: C 18 The solid phase extraction membrane was soaked in 5 mL of n-hexane / dichloromethane (1:1) for 3 min in advance, and then activated with 10 mL of methanol and 10 mL of water in turn. 18 Solid phase extraction membrane, let all the solvent flow through the solid phase extraction membrane, during this process, the solid phase extraction membrane cannot be exposed to air;

[0023] (2) Extraction of water samples: filter laboratory tap water samples with a 0.45μm glass fiber membrane in advance, and add the pretreated 1000mL laboratory tap water samples to a container containing C 18 In the glass filter of the solid phase extraction membrane, turn on the vacuum pump, and after the water sample passes through at a flow rate of 10 mL / min, continue to vacuum to remove the residual water in the solid phase extraction ...

Embodiment 2

[0033] Example 2: Determination of 18 Organochlorine Compounds in Seawater of Zhoushan Sea Area

[0034] The method is the same as in Example 1, and the content of 18 kinds of organochlorine substances in the seawater of Zhoushan sea area was measured and all were not detected, and the recovery rate of each organochlorine compound in the seawater of Zhoushan sea area was 85%-115% (see Table 2), Meet the recovery requirements of analytical methods.

Embodiment 3

[0035] Example 3 Determination of 18 kinds of organochlorine compounds in a certain reservoir water

[0036] (1)C 18 Cleaning and Activation of Solid Phase Extraction Membranes: C 18 The solid phase extraction membrane was soaked in 5 mL of n-hexane / dichloromethane (1:1) for 3 min in advance, and then activated with 10 mL of methanol and 10 mL of water in turn. 18 Solid phase extraction membrane, let all the solvent flow through the solid phase extraction membrane, during this process, the solid phase extraction membrane cannot be exposed to air;

[0037] (2) Extraction of water samples: filter a water sample from a certain reservoir with a 0.45μm glass fiber membrane in advance, and add the pretreated 1000mL water sample from a certain reservoir to a container containing C 18 In the glass filter of the solid phase extraction membrane, turn on the vacuum pump, and after the water sample passes through at a flow rate of 10 mL / min, continue to vacuum to remove the residual wat...

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Abstract

The invention discloses a solid-phase membrane extraction and gas chromatography-tandem mass spectrometry detection method of organic chlorine compounds in a water body. A C18 solid-phase extraction membrane is used for achieving enrichment of the organic chlorine compounds in the water body. A gas chromatography-tandem mass spectrometry detection method is used for detection. The method is few in operation step, high in sensitivity and good in reproducibility and can be used for measuring the content of the organic chlorine compounds in the water body.

Description

technical field [0001] The invention relates to the technical field of water quality safety detection, in particular to a solid-phase membrane extraction-gas chromatography tandem mass spectrometry detection method for organochlorine compounds in water. Background technique [0002] 666. DDT is a kind of refractory organochlorine pesticides. It has contact killing, stomach poisoning, fumigation and a certain degree of systemic effect on many pests. The half-life of organochlorine pesticides is about 2 to 20 years. Accumulation in the body and transmission through the food chain pose a serious threat to the ecological environment and human health. Although many countries have already banned and restricted the use, due to the stable chemical properties of DDT and DDT, investigations have found that there are residues in environmental media and human bodies in various regions of the country, and some are even many times higher than the standard. For example, the investigation ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/72
CPCG01N30/02G01N30/06G01N30/72
Inventor 孙秀梅金衍健郝青胡红美钟志郭远明
Owner MARINE FISHERIES RES INST OF ZHEJIANG
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