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Analysis method of more than 9 nitrosamine compounds in water

A technology of nitrosamines and analysis methods, which is applied in the field of environmental detection and analysis, can solve the problems of false positives of nitrosamines, accurate analysis of difficult N-nitrosamine compounds, etc., and achieve the effect of reducing the volume of water samples

Inactive Publication Date: 2019-09-27
NAT RESERACH CENT OF GEOANALYSIS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are only 4 kinds of N-nitrosamine compounds used for detection. When more types of N-nitrosamine compounds are involved, it is difficult to analyze each of them accurately.
[0005] Most of the detection methods of N-nitrosamines in water reported at present are analyzed and detected by gas chromatography-mass spectrometry and high-performance liquid chromatography, but gas chromatography-mass spectrometry is easy to produce false positive results for the detection of nitrosamines in water

Method used

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  • Analysis method of more than 9 nitrosamine compounds in water
  • Analysis method of more than 9 nitrosamine compounds in water
  • Analysis method of more than 9 nitrosamine compounds in water

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0110] Example 1 Comparison of Extraction Needles

[0111] In this embodiment, different types of fiber-coated extraction needles were selected, and tests were carried out according to the above-mentioned "sample and method used in the embodiment". In this embodiment, the concentrations of standard samples containing NDMA, NMEA, NDEA, NDPA, NDBA, NPIP, NPYR, NMOR and NDPhA compounds in the water samples to be tested are all 1 μg / L.

[0112] Choose 5 different types of fiber coatings, choose 7μmPDMS (polydimethylsiloxane), 100μmPDMS (polydimethylsiloxane), 85μmPA (polyacrylate), 65μmPDMS / DVB (polydimethylsiloxane) Alkane / divinylbenzene), 75μmCAR / PDMS (carbon molecular sieve / polydimethylsiloxane) different types of fiber coatings, and compare the extraction efficiency of nitrosamines.

[0113] 20mL of the water sample to be tested is extracted for each test corresponding to the extraction target, and detected by gas chromatography coupled with mass spectrometry:

[0114] The e...

Embodiment 2

[0115] The comparison of embodiment 2 extraction modes

[0116] In this example, the headspace extraction method was tested according to the above-mentioned "sample and method used in the example", and the headspace extraction method was replaced by the immersion extraction method for comparison. The immersion extraction method is to directly immerse the extraction needle into the sample to be tested The extraction is carried out in the sample, and the headspace extraction method is to suspend the extraction needle above the sample to be tested, and extract without direct contact with the sample to be tested. The concentrations of NDMA, NMEA, NDEA, NDPA, NDBA, NPIP, NPYR, NMOR and NDPhA compound standard samples in the water samples to be tested in this embodiment are all 5 μg / L.

[0117] The organic matter in enriched water was extracted by immersion extraction method and headspace extraction method respectively. The experimental results are as follows: figure 2 As shown, t...

Embodiment 3

[0118] The comparison of embodiment 3 extraction temperature

[0119] The present embodiment adopts different water bath temperatures, and has carried out test according to above-mentioned " embodiment uses sample and method ". In this embodiment, the concentrations of NDMA, NMEA, NDEA, NDPA, NDBA, NPIP, NPYR, NMOR and NDPhA compound standard samples in the water samples to be tested are all 1 μg / L.

[0120] Under the temperature condition of 0-100°C, the headspace extraction method was used to extract the organic matter in the enriched water. The experimental results are as follows: image 3 As shown, the peak area in the figure refers to the chromatographic peak area of ​​the corresponding compound in the chromatogram. It can be seen from the figure that although the distribution coefficient of the analytes in the headspace is larger when the extraction temperature is 0°C, the overall concentration of the headspace compounds is lower at lower temperatures. When the tempera...

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Abstract

The invention relates to an analysis method for detecting more than 9 nitrosamine compounds in water. The nitrosamine compounds comprise N-nitrosodimethylamine, N-Nitroso-ethyl methylamine, N-Nitrosodiethylamine, N-nitrosodipropylamine, N-nitrosodibutylamine, N-nitrosopyrrolidine, N-nitrosopiperidine, N-nitrosomorpholine and N-nitrosodiphenylamine. The analysis method comprises the following steps of: extracting a water sample to be detected by adopting solid phase micro-extraction; and determining the nitrosamine compounds by adopting a gas chromatography tandem mass spectrometry (GC-MS / MS). The method provided by the invention achieves rapid, convenient and sensitive determination of the content of various nitrosamine compounds in the water sample, and has the advantages of the high analysis efficiency and the better popularization prospect.

Description

technical field [0001] The invention belongs to the field of environmental detection and analysis, in particular to an analysis method for trace nitrosamine compounds in water. Background technique [0002] Nitrosoamines are a class of compounds highly mutagenic and carcinogenic to humans, including N-nitrosodimethylamine (NDMA), N-nitrosodiethylamine (NDEA) , N-nitrosomethylethylamine (NMEA), N-nitrosopyrrolidine (NPYR), N-nitrosomorpholine (NMOR), N-nitrosopiperidine (NPIP), N-nitroso Nitrodi-n-propylamine (NDPA) and N-nitrosodi-n-butylamine (NDBA) are listed by the International Agency for Research on Cancer (IARC) as possible carcinogens for humans, and N-nitrosodiphenylamine (NDPhA) can induce Bladder cancer in mice. In recent years, people have detected the presence of nitrosamine compounds in water, which has aroused people's attention to a series of issues such as the content, distribution, source and harm of nitrosamines in water. focus on. At present, the analys...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/062
Inventor 黄毅李程石喆元饶竹田芹刘晨
Owner NAT RESERACH CENT OF GEOANALYSIS
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