Current approaches to the derivatization of Chemical Weapons Convention-related alcohols for on-site gas chromatographic analysis

Kód výsledku v IS VaVaI

<a href="https://www.isvavai.cz/riv?ss=detail&h=RIV%2F60162694%3AG45__%2F24%3A00560481" target="_blank" >RIV/60162694:G45__/24:00560481 - isvavai.cz</a>

Výsledek na webu

<a href="https://www.mdpi.com/2504-3900/92/1/13" target="_blank" >https://www.mdpi.com/2504-3900/92/1/13</a>

DOI - Digital Object Identifier

<a href="http://dx.doi.org/10.3390/proceedings2023092013" target="_blank" >10.3390/proceedings2023092013</a>

Jazyk výsledku

angličtina

Název v původním jazyce

Current approaches to the derivatization of Chemical Weapons Convention-related alcohols for on-site gas chromatographic analysis

Popis výsledku v původním jazyce

The task of deployable military laboratories is to perform the fast identification of chemical warfare agents (CWAs) and related chemicals in various types of samples in field conditions. Identification is limited by the time and equipment of mobile laboratories. Polar degradation products are commonly derivatized by a procedure using N,O-Bis(trimethylsilyl)trifluoroacetamide (BSTFA) [1,2], which is time-consuming, and the resulting chromatograms often contain a number of artifacts that hinder their identification [3]. This work describes the development and optimization of an alternative trimethylsilylation (TMS) procedure for on-site identification. The goal was to develop a fast and robust method that was efficient without heating, producing clean chromatograms. The analytes were precursors and degradation products of blistering (thiodiglycol, ethyldiethanolamine, methyldiethanolamine, triethanolamine), nerve (N,N-diisopropylamino ethanol), and psychoactive (3-quinuclidinol) CWAs. Ten TMS reagents were compared in terms of their derivatization efficiency. The solvent effect, catalyst addition effect, and the time and temperature of derivatization were studied and optimized. The stability of the derivatives was observed over time, and chromatogram artifacts were monitored. The original recommended and widely used method of derivatizing alcohol for 30 min at 60 °C in acetonitrile using BSTFA was overcome using three optimized procedures with different TMS reagents. They achieved high and stable yields in an acetone environment already at room temperature and a reaction lasting 5 min. Due to the same chemical structure of the resulting compounds (TMS-derivatives), it was possible to use established mass spectral databases. Optimized procedures were applied to environmental (water, sand) and urban (acrylic paint, asphalt-aluminum paint, concrete) samples contaminated with the studied alcohol. The results obtained on a benchtop gas chromatograph were validated afterward on a field device used by the deployable chemical laboratory of the Czech Army following their standard operating procedures for sample preparation. The developed methods are useful for military teams and stationary analytical laboratories whose task is the unambiguous identification of CWAs and related compounds in various samples.

Název v anglickém jazyce

Current approaches to the derivatization of Chemical Weapons Convention-related alcohols for on-site gas chromatographic analysis

Popis výsledku anglicky

The task of deployable military laboratories is to perform the fast identification of chemical warfare agents (CWAs) and related chemicals in various types of samples in field conditions. Identification is limited by the time and equipment of mobile laboratories. Polar degradation products are commonly derivatized by a procedure using N,O-Bis(trimethylsilyl)trifluoroacetamide (BSTFA) [1,2], which is time-consuming, and the resulting chromatograms often contain a number of artifacts that hinder their identification [3]. This work describes the development and optimization of an alternative trimethylsilylation (TMS) procedure for on-site identification. The goal was to develop a fast and robust method that was efficient without heating, producing clean chromatograms. The analytes were precursors and degradation products of blistering (thiodiglycol, ethyldiethanolamine, methyldiethanolamine, triethanolamine), nerve (N,N-diisopropylamino ethanol), and psychoactive (3-quinuclidinol) CWAs. Ten TMS reagents were compared in terms of their derivatization efficiency. The solvent effect, catalyst addition effect, and the time and temperature of derivatization were studied and optimized. The stability of the derivatives was observed over time, and chromatogram artifacts were monitored. The original recommended and widely used method of derivatizing alcohol for 30 min at 60 °C in acetonitrile using BSTFA was overcome using three optimized procedures with different TMS reagents. They achieved high and stable yields in an acetone environment already at room temperature and a reaction lasting 5 min. Due to the same chemical structure of the resulting compounds (TMS-derivatives), it was possible to use established mass spectral databases. Optimized procedures were applied to environmental (water, sand) and urban (acrylic paint, asphalt-aluminum paint, concrete) samples contaminated with the studied alcohol. The results obtained on a benchtop gas chromatograph were validated afterward on a field device used by the deployable chemical laboratory of the Czech Army following their standard operating procedures for sample preparation. The developed methods are useful for military teams and stationary analytical laboratories whose task is the unambiguous identification of CWAs and related compounds in various samples.

Druh

D - Stať ve sborníku

CEP obor

—

OECD FORD obor

10500 - Earth and related environmental sciences

Projekt

—

Návaznosti

I - Institucionalni podpora na dlouhodoby koncepcni rozvoj vyzkumne organizace

Rok uplatnění

2023

Kód důvěrnosti údajů

S - Úplné a pravdivé údaje o projektu nepodléhají ochraně podle zvláštních právních předpisů

Název statě ve sborníku

Proceedings

ISBN

—

ISSN

2504-3900

e-ISSN

2504-3900

Počet stran výsledku

2

Strana od-do

13-14

Název nakladatele

MDPI

Místo vydání

Tallinn, Estonsko

Místo konání akce

Tallinn, Estonsko

Datum konání akce

9. 10. 2023

Typ akce podle státní příslušnosti

WRD - Celosvětová akce

Kód UT WoS článku

—