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A gas chromatography-mass spectrometry method for the determination of three trace polyhalogenated phenols in textiles

A technology of halogenated phenol and gas chromatography, which is applied in the field of analysis and detection of harmful trace substances, and achieves the effect of simple operation steps

Active Publication Date: 2021-05-14
丁立平 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In order to overcome the deficiencies of the lack of three trace polyhalogenated phenol detection methods in existing textiles, the technical problem to be solved by the present invention is to provide a rapid adsorption method based on a new adsorbent dispersive solid phase extraction, which is suitable for the three trace polyhalogenated phenols in textiles. Gas Chromatography-Mass Spectrometry for Quantitative Detection of Polyhalogenated Phenols

Method used

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  • A gas chromatography-mass spectrometry method for the determination of three trace polyhalogenated phenols in textiles
  • A gas chromatography-mass spectrometry method for the determination of three trace polyhalogenated phenols in textiles
  • A gas chromatography-mass spectrometry method for the determination of three trace polyhalogenated phenols in textiles

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Effect test

Embodiment 1

[0077] In Example 1, cotton cloth is used as the sample matrix to carry out standard addition recovery experiments to verify the feasibility of the method of the present invention. The cotton cloth comes from the sample submitted for inspection, and is processed according to the following steps:

[0078] (1) Extraction and adsorption of compounds: Cut cotton samples into 0.5cm╳0.5cm size, seal them for storage, weigh 1.00g of samples in 50mL plastic centrifuge tubes with stoppers, and add 5.00mL of them to each For three compound standard solutions of 10.0μg / L, 20.0μg / L and 200.0μg / L, three levels of six-parallel spiked samples were prepared, and then 1.0mL of 0.1% formic acid was added for infiltration, and 20mL of ethyl acetate was added , vortex, ultrasonically extract for 15min, centrifuge, and take the supernatant to another centrifuge tube with a stopper, extract once again, combine the upper layer extract; and add 0.20g of p-aminobenzenesulfonate-magnesium aluminum water...

Embodiment 2

[0087] In Example 2, the cotton and linen blended fabric is used as the sample matrix to carry out the standard recovery experiment to verify the feasibility of the method of the present invention. The cotton fabric comes from the sample submitted for inspection, and is processed according to the following steps:

[0088] (1) Extraction and adsorption of compounds: cut the cotton-linen blended fabric sample into 0.5cm╳0.5cm size, seal it for storage, weigh 1.00g sample each in a 50mL plastic centrifuge tube with stopper, and add 5.00 Three compound standard solutions with mL concentrations of 10.0 μg / L, 20.0 μg / L and 200.0 μg / L were prepared to obtain three-level six-parallel spiked samples, and then 1.0 mL of 0.1% formic acid was added for infiltration, and 20 mL of Ethyl acetate, vortex, ultrasonic extraction for 15min, centrifugation, and take the supernatant to another plugged centrifuge tube, re-extract once, combine the upper layer extract; and add 0.20g of p-aminobenzene...

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Abstract

The invention relates to a method for analyzing and detecting trace harmful substances, in particular to a gas chromatography-chromatographic method for determining trace amounts of 3,5-difluorophenol, 5-chloro-2-fluorophenol and 5-bromo-2-fluorophenol in textiles Mass Spectrometry. The steps of the method include enriching the target compound in the textile with a novel adsorbent p-aminobenzenesulfonate-magnesium-aluminum hydrotalcite, using an acid-dissolved adsorbent to achieve complete elution of the target compound, and efficiently extracting the compound with a small dose of organic solvent. After derivatization, it is quickly analyzed and determined by gas chromatography-mass spectrometry. The new adsorbent adopted in this method adopts the method of dispersed solid phase extraction to realize fast and efficient adsorption of the target substance, which has the advantages of fast and high efficiency; the application of acid-dissolved adsorbent can realize the complete desorption of the target substance; only a small amount of organic solvent is used as The extraction solvent of the target object has the characteristics of simple operation steps compared with the conventional phase transfer derivatization method.

Description

technical field [0001] The invention relates to a method for analyzing and detecting harmful trace substances, in particular to a gas chromatography for determining trace amounts of 3,5-difluorophenol, 5-chloro-2-fluorophenol and 5-bromo-2-fluorophenol in textiles - Mass spectrometry. Background technique [0002] Chlorophenol compounds are commonly used fungicides and preservatives in textiles, and their residues in textiles have also attracted much attention. At present, there are relatively many relevant reports on the detection of chlorinated phenolic compound residues in textiles, mainly focusing on the detection by gas chromatography or gas chromatography-mass spectrometry, and the pretreatment methods mainly focus on the use of organic solvent extraction followed by phase transfer to Alkaline solution and derivatization with acetic anhydride. 3,5-difluorophenol, 5-chloro-2-fluorophenol and 5-bromo-2-fluorophenol are three common chemical products that have also been...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 丁立平蔡春平王丹红郑麟毅张睿姜晖林荆黄菁菁郑铃郑香平陈志涛
Owner 丁立平
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