Gas chromatography-mass spectrometry combined method for determining three traces of monohalohydroxybenzonitrile in river water

A technology of monohalogenated hydroxybenzonitrile and gas chromatography, which is applied in the directions of measuring devices, instruments, scientific instruments, etc., can solve the problems of lack of detection standards and practical methods, etc.

Active Publication Date: 2019-01-15
丁立平 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to overcome the deficiency that there are no detection standards and practical methods for the three kinds of trace monohalogenated hydroxybenzonitriles in the existing river water, the technical problem to be solved by the present invention is to provide a kind of rapid adsorption based on a novel adsorbent in a dispersed solid phase extraction mode, A gas chromatography-mass spectrometry method suitable for the detection of three trace amounts of monohalogenated hydroxybenzonitriles in river water

Method used

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  • Gas chromatography-mass spectrometry combined method for determining three traces of monohalohydroxybenzonitrile in river water
  • Gas chromatography-mass spectrometry combined method for determining three traces of monohalohydroxybenzonitrile in river water
  • Gas chromatography-mass spectrometry combined method for determining three traces of monohalohydroxybenzonitrile in river water

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Effect test

Embodiment 1

[0079] The present embodiment 1 adopts Minjiang River water as the sample matrix to carry out the standard addition recovery experiment to verify the feasibility of the method of the present invention, according to the following steps to process:

[0080] Minjiang water was taken from the tap water intake of the Taijiang section of Fuzhou. After sampling, it was refrigerated and stored at 4°C. When used, it was filtered and the pH value was adjusted to the range of 6.5-7.5 with sodium hydroxide solution.

[0081] 1. Adsorption of compounds:

[0082] In a 500mL separating funnel, add 200mL water samples to each of them, take 5.00mL of the above-mentioned 10.0μg / L, 20.0μg / L and 200.0μg / L standard solutions respectively, and prepare three-level six-parallel spiked samples , add 0.40g benzenesulfonate-magnesium aluminum type hydrotalcite roasting product adsorbent to each funnel afterwards, vibrate for 15min to make the adsorbent adsorb;

[0083] 2. Desorption of compounds:

[0...

Embodiment 2

[0093]The present embodiment 2 adopts Longjiang water as the sample matrix to carry out the standard addition recovery experiment to verify the feasibility of the method of the present invention, and process according to the following steps:

[0094] Longjiang water was taken from the tap water intake of Yinxi Township, Longjiang, Fuqing. After sampling, it was refrigerated and stored at 4°C. When used, it was filtered and the pH value was adjusted to a range of 6.5-7.5 with sodium hydroxide solution.

[0095] 1. Adsorption of compounds:

[0096] In a 500mL separating funnel, add 200mL water samples to each of them, take 5.00mL of the above-mentioned 10.0μg / L, 20.0μg / L and 200.0μg / L standard solutions respectively, and prepare three-level six-parallel spiked samples , add 0.40g benzenesulfonate-magnesium aluminum type hydrotalcite roasting product adsorbent to each funnel afterwards, vibrate for 15min to make the adsorbent adsorb;

[0097] 2. Desorption of compounds:

[0098...

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Abstract

The invention relates to a method for analyzing and detecting trace harmful substances, in particular to a gas chromatography-mass spectrometry combined method for determining trace amounts of 3-fluoro-4-hydroxybenzonitrile, 3-chloro-5-hydroxybenzonitrile and 5-bromo-2-hydroxybenzonitrile in river water. In view of the current lack of standards and methods for the detection of three target compounds in river water, the practical detection method step developed by the invention comprises: enriching the target compounds in drinking water with a novel benzenesulfonate-magnesium aluminum hydrotalcite calcined product adsorbent, achieving complete elution of the target with a hydrochloric acid dissolved adsorbent, eficiently extracting compounds with low doses of organic solvents, and after derivatization, quickly analyzing and measuring by gas chromatography-mass spectrometry combined method. The novel adsorbent used in the method adopts the method of dispersive solid phase extraction to achieve rapid and efficient adsorption of the target. The acid desorption adsorbent can achieve complete desorption of the target. The use of only a small amount of organic solvent extraction has significant safety, environmental benefits and economic advantages.

Description

technical field [0001] The invention relates to a method for analyzing and detecting harmful trace substances, in particular to a method for determining trace amounts of 3-fluoro-4-hydroxybenzonitrile, 3-chloro-5-hydroxybenzonitrile and 5-bromo-2-hydroxybenzonitrile in river water Gas chromatography-mass spectrometry of benzonitrile. Background technique [0002] Hydroxybenzonitrile compounds are an important chemical product and an important intermediate commonly used in the preparation of pesticides, spices and liquid crystal materials, of which 3-fluoro-4-hydroxybenzonitrile, 3-chloro-5-hydroxybenzonitrile And 5-bromo-2-hydroxybenzonitrile are three structurally similar, important halogenated hydroxybenzonitrile compounds. Although there is no animal toxicity research data on these three compounds, the halogens in their structures and the benzene ring structures that are easy to accumulate in animals all indicate that they may be potentially harmful to animals and humans...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/02G01N30/72
CPCG01N30/02G01N30/06G01N30/72G01N2030/062
Inventor 丁立平张睿黄菁菁郑铃姜晖郑香平陈志涛郑麟毅蔡春平
Owner 丁立平
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