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基于巯基化衍生的气相色谱-质谱法测定有机相及水相中氯化氰

Cyanogen chloride (ClCN) has been widely used in industrial production. ClCN is also listed in the Schedule of the Chemical Weapons Convention (CWC). The use of traditional colorimetric analysis or gas chromatography for the detection of ClCN has been characterized by low efficiency and poor sensiti...

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Autores principales: LI, Xiaosen, WU, Jina, XIA, Junmei, YUAN, Ling, YANG, Yang
Formato: Online Artículo Texto
Lenguaje:English
Publicado: Editorial board of Chinese Journal of Chromatography 2021
Materias:
Acceso en línea:https://www.ncbi.nlm.nih.gov/pmc/articles/PMC9404212/
https://www.ncbi.nlm.nih.gov/pubmed/34212592
http://dx.doi.org/10.3724/SP.J.1123.2020.12004
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author LI, Xiaosen
WU, Jina
XIA, Junmei
YUAN, Ling
YANG, Yang
author_facet LI, Xiaosen
WU, Jina
XIA, Junmei
YUAN, Ling
YANG, Yang
author_sort LI, Xiaosen
collection PubMed
description Cyanogen chloride (ClCN) has been widely used in industrial production. ClCN is also listed in the Schedule of the Chemical Weapons Convention (CWC). The use of traditional colorimetric analysis or gas chromatography for the detection of ClCN has been characterized by low efficiency and poor sensitivity. In this study, a method was established for the qualitative analysis and quantitative detection of ClCN in organic and water matrices by gas chromatography-mass spectrometry (GC-MS) based on thiol derivatization. 1-Butylthiol was selected as the optimal derivatization reagent. The optimal temperature for thiol derivatization in the organic matrices was 40 ℃ and the reaction time was 10 min. The pH for derivatization was approximately 9. The ClCN in the organic matrices was directly analyzed by GC-MS after derivatization. The conditions of ClCN derivatization in the water matrices were the same as those in the organic matrices. After the derivatization of ClCN, headspace-solid phase microextraction (HS-SPME) was employed during sample preparation for water matrices. Different temperatures for HS-SPME were explored, and the optimal temperature was found to be 55 ℃. The product of thiol derivatization was confirmed as butyl thiocyanate. The main fragmentation patterns and mass spectrometric cleavage pathway were investigated by GC-MS/MS. The quantitative determination of ClCN in organic and water matrices was conducted via the internal standard and external standard methods, respectively. ClCN showed good linearity in the corresponding ranges in the organic and water matrices. The correlation coefficients for both matrices were greater than 0.99. The linearities of ClCN in the organic and water matrices were in the range of 20-2000 μg/L and 20-1200 μg/L, respectively. An organic sample and water samples from different substrates were selected to verify the accuracy and precision of the method at three spiked levels. The average spiked recoveries of ClCN in the organic sample and water samples were 87.3%-98.8% and 97.6%-102.2%, respectively. The corresponding relative standard deviations (RSDs, n=6) were 2.1%-4.7% and 2.8%-4.2%. The derivatization method established in this study showed good reaction specificity. The method was successfully applied in the analysis of samples obtained from the Organisation for the Prohibition of Chemical Weapons (OPCW). The method established in this study for the detection of ClCN showed high sensitivity and precision, and could aid in the analysis and detection of ClCN in the environment.
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spelling pubmed-94042122022-09-14 基于巯基化衍生的气相色谱-质谱法测定有机相及水相中氯化氰 LI, Xiaosen WU, Jina XIA, Junmei YUAN, Ling YANG, Yang Se Pu Articles Cyanogen chloride (ClCN) has been widely used in industrial production. ClCN is also listed in the Schedule of the Chemical Weapons Convention (CWC). The use of traditional colorimetric analysis or gas chromatography for the detection of ClCN has been characterized by low efficiency and poor sensitivity. In this study, a method was established for the qualitative analysis and quantitative detection of ClCN in organic and water matrices by gas chromatography-mass spectrometry (GC-MS) based on thiol derivatization. 1-Butylthiol was selected as the optimal derivatization reagent. The optimal temperature for thiol derivatization in the organic matrices was 40 ℃ and the reaction time was 10 min. The pH for derivatization was approximately 9. The ClCN in the organic matrices was directly analyzed by GC-MS after derivatization. The conditions of ClCN derivatization in the water matrices were the same as those in the organic matrices. After the derivatization of ClCN, headspace-solid phase microextraction (HS-SPME) was employed during sample preparation for water matrices. Different temperatures for HS-SPME were explored, and the optimal temperature was found to be 55 ℃. The product of thiol derivatization was confirmed as butyl thiocyanate. The main fragmentation patterns and mass spectrometric cleavage pathway were investigated by GC-MS/MS. The quantitative determination of ClCN in organic and water matrices was conducted via the internal standard and external standard methods, respectively. ClCN showed good linearity in the corresponding ranges in the organic and water matrices. The correlation coefficients for both matrices were greater than 0.99. The linearities of ClCN in the organic and water matrices were in the range of 20-2000 μg/L and 20-1200 μg/L, respectively. An organic sample and water samples from different substrates were selected to verify the accuracy and precision of the method at three spiked levels. The average spiked recoveries of ClCN in the organic sample and water samples were 87.3%-98.8% and 97.6%-102.2%, respectively. The corresponding relative standard deviations (RSDs, n=6) were 2.1%-4.7% and 2.8%-4.2%. The derivatization method established in this study showed good reaction specificity. The method was successfully applied in the analysis of samples obtained from the Organisation for the Prohibition of Chemical Weapons (OPCW). The method established in this study for the detection of ClCN showed high sensitivity and precision, and could aid in the analysis and detection of ClCN in the environment. Editorial board of Chinese Journal of Chromatography 2021-08-08 /pmc/articles/PMC9404212/ /pubmed/34212592 http://dx.doi.org/10.3724/SP.J.1123.2020.12004 Text en https://creativecommons.org/licenses/by/4.0/本文是开放获取文章,遵循CC BY 4.0协议 https://creativecommons.org/licenses/by/4.0/This is an open access article distributed under the terms of the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original author and source are credited.
spellingShingle Articles
LI, Xiaosen
WU, Jina
XIA, Junmei
YUAN, Ling
YANG, Yang
基于巯基化衍生的气相色谱-质谱法测定有机相及水相中氯化氰
title 基于巯基化衍生的气相色谱-质谱法测定有机相及水相中氯化氰
title_full 基于巯基化衍生的气相色谱-质谱法测定有机相及水相中氯化氰
title_fullStr 基于巯基化衍生的气相色谱-质谱法测定有机相及水相中氯化氰
title_full_unstemmed 基于巯基化衍生的气相色谱-质谱法测定有机相及水相中氯化氰
title_short 基于巯基化衍生的气相色谱-质谱法测定有机相及水相中氯化氰
title_sort 基于巯基化衍生的气相色谱-质谱法测定有机相及水相中氯化氰
topic Articles
url https://www.ncbi.nlm.nih.gov/pmc/articles/PMC9404212/
https://www.ncbi.nlm.nih.gov/pubmed/34212592
http://dx.doi.org/10.3724/SP.J.1123.2020.12004
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