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Analysis method for simultaneously determining 16 phenolic compounds in water environment

A technology for phenolic compounds and analysis methods, which is applied in the analysis field of simultaneous determination of 16 kinds of phenolic compounds in water environment, can solve the problem that there is no standard for gas chromatography-mass spectrometry analysis methods, and achieves good separation effect and good linearity.

Inactive Publication Date: 2015-01-07
NANJING UNIV
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0004] In China, there is no systematic gas chromatography-mass spectrometry standard for the analysis of various phenolic compounds including monohydric phenols and polyphenols

Method used

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  • Analysis method for simultaneously determining 16 phenolic compounds in water environment
  • Analysis method for simultaneously determining 16 phenolic compounds in water environment
  • Analysis method for simultaneously determining 16 phenolic compounds in water environment

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Embodiment 1 measures the qualitative analysis method of 16 kinds of phenolic compounds in water environment, concrete steps are as follows:

[0030] A. Sample pretreatment

[0031](1) 500mL water sample is filtered through a 0.45μm microporous membrane, and the pH value of the water sample is adjusted to <1.5 with sulfuric acid solution. The water sample used in this example is prepared from 16 kinds of phenolic compound standard liquids and water respectively. , and a blank water sample to which the surrogate 2,4,6-tribromophenol was added for recovery control;

[0032] (2) Activate the solid-phase extraction (SPE) cartridge with 9mL of dichloromethane, 9mL of methanol, and 9mL of dilute hydrochloric acid solution, wherein the volume concentration of dilute hydrochloric acid is 0.5-2%, and the SPE cartridge has a volume of 6mL and a mass of 500mg The commercial finished column of the Poly-Sery HLB SPE Cartridge, which is a modified divinylbenzene polymer column;

[...

Embodiment 2

[0043] Embodiment 2 measures the quantitative analysis method of 16 kinds of phenolic compounds in water environment, concrete steps are as follows:

[0044] Before the quantitative analysis and determination of the 16 phenolic compounds in the water environment, it is first necessary to prepare a standard solution. The preparation method is as follows: add an appropriate volume of phenolic compound standard solution into a 20mL glass tube, and dilute to 8.0mL with acetone, so that the concentration of phenolic compound is 1000μg / L. Then add 100 μL pentafluorobenzyl bromide solution and 100 μL K 2 CO 3 solution, cap the bottle, shake gently, and heat in a water bath at 60°C for 1 hour. After the reaction was completed and cooled to room temperature, it was concentrated to 0.5 mL by swirling nitrogen blowing. Then add 3 mL of n-hexane, continue to vortex and concentrate to 1 mL with nitrogen blowing. Then gradually dilute to 5μg / L, 12.5μg / L, 25μg / L, 50μg / L, 100μg / L, 200μg / L...

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Abstract

The invention discloses an analysis method for simultaneously determining 16 phenolic compounds in water environment, and belongs to the technical field of phenolic compound analysis. According to the invention, solid phase extraction (SPE) is used for preprocessing a water sample, and a gas chromatography and mass spectrum coupling technique method (GC-MS) is used for qualitatively and quantitatively analyzing the 16 phenolic compounds in the water sample. Under the analysis condition optimized by the analysis method, the 16 phenolic compounds in water can be simultaneously determined, a good chromatographic peak can be obtained within 28 minutes, and a good separation effect can be obtained. The linearity of all the objective compounds in the concentration range of 5-1000 <mu>g / L is good, the correlation coefficients are all more than 0.9959, the detection limit achieves 0.04-4.0 <mu>g / L, the relative standard deviation is 0.22-13%, and the labeling recovery rate is 77-112%. The analysis method disclosed by the invention is simple, easy to operate, accurate and reliable, so that the analysis method is suitable for detecting large-scale samples.

Description

technical field [0001] The invention relates to the field of analysis of phenolic compounds, in particular to an analysis method for simultaneously measuring 16 kinds of phenolic compounds in water environment. Background technique [0002] Phenolic compounds refer to compounds in which the hydrogen atoms on the benzene ring in aromatic hydrocarbons are replaced by hydroxyl groups. Natural water generally does not contain phenols, but water polluted by industrial wastewater may contain phenols, so its main sources include coking plants, pharmaceutical plants, textile mills, gas plants, petrochemical plants, and synthetic phenol industries. Chlorophenols and nitrophenols in surface waters may also come from seepage of degradation products of various chlorophenolic acid herbicides and organophosphate insecticides in soil. Phenolic compounds are highly toxic substances that are difficult to degrade, can remain in the soil for a long time, and have carcinogenic, teratogenic, an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 鲜啟鸣陈洁霞韦恩泽孙成
Owner NANJING UNIV
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