Combination of solid phase extraction and in vial solid phase derivatization using a strong anion exchange disk for the determination of nerve agent markers

Subramaniam, Raja; Åstot, Crister; Nilsson, Carl-Axel; Östin, Anders

doi:10.1016/j.chroma.2009.10.017

Cited by 32 publications

(8 citation statements)

References 28 publications

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“…A paper describing an approach combining solid phase extraction followed by solid phase derivatization of various phosphonic acid markers for nerve agents was introduced in 2009 by the Ostin group at the Swedish Defence Research Agency (FOI) [ 67 ]. The report described the use of in vial solid phase derivatization (SPD) of nine phosphonic acids using BSTFA (with 1% trimethylsilyl chloride) followed by analysis by GC-MS.…”

Section: Silylation Methodsmentioning

confidence: 99%

Analysis of Organophosphorus-Based Nerve Agent Degradation Products by Gas Chromatography-Mass Spectrometry (GC-MS): Current Derivatization Reactions in the Analytical Chemist’s Toolbox

Valdez

Leif

2021

Molecules

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The field of gas chromatography-mass spectrometry (GC-MS) in the analysis of chemical warfare agents (CWAs), specifically those involving the organophosphorus-based nerve agents (OPNAs), is a continually evolving and dynamic area of research. The ever-present interest in this field within analytical chemistry is driven by the constant threat posed by these lethal CWAs, highlighted by their use during the Tokyo subway attack in 1995, their deliberate use on civilians in Syria in 2013, and their use in the poisoning of Sergei and Yulia Skripal in Great Britain in 2018 and Alexei Navalny in 2020. These events coupled with their potential for mass destruction only serve to stress the importance of developing methods for their rapid and unambiguous detection. Although the direct detection of OPNAs is possible by GC-MS, in most instances, the analytical chemist must rely on the detection of the products arising from their degradation. To this end, derivatization reactions mainly in the form of silylations and alkylations employing a vast array of reagents have played a pivotal role in the efficient detection of these products that can be used retrospectively to identify the original OPNA.

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Section: Silylation Methodsmentioning

confidence: 99%

Analysis of Organophosphorus-Based Nerve Agent Degradation Products by Gas Chromatography-Mass Spectrometry (GC-MS): Current Derivatization Reactions in the Analytical Chemist’s Toolbox

Valdez

Leif

2021

Molecules

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“…Additional chemicals had also been added to the water sample (e.g. magnesium sulfate, calcium chloride and polyethylene glycol) in order to create a challenging matrix for derivatization processes and/or analyses …”

Section: Methodsmentioning

confidence: 99%

“…However, phosphonic acids are polar and non‐volatile, and therefore must be derivatized prior to GC analysis . Silylation, methylation and pentafluorobenzylation are the most widely used methods for derivatizing APAs. However, derivatization can be problematic since the derivatization process may be water sensitive, the derivatized products may be relatively unstable and purification may be required prior to analysis.…”

Section: Introductionmentioning

confidence: 99%

Structural determination of nerve agent markers using gas chromatography mass spectrometry after derivatization with 3‐pyridyldiazomethane

2013

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Nerve agents are a class of organophosphorous chemicals that are prohibited under the Chemical Weapons Convention. Their degradation products, phosphonic acids, are analyzed as markers of nerve agent contamination and use. Because the phosphonic acids are non-volatile and very polar, their identification by GC-MS requires a derivatization step prior to analysis. Standard derivatization methods for gas-chromatography electron-impact mass-spectrometry analysis give very similar spectra for many alkyl phosphonic acid isomers, which complicates the identification process. We present a new reagent, 3-pyridyldiazomethane, for preparing picolinyl ester derivatives of alkyl methylphosphonic acids facilitating the determination of their structure by enhancing predictable fragmentation of the O-alkyl chain. This fragmentation is directed by the nitrogen nucleus of the pyridyl moiety that abstracts hydrogen from the O-alkyl chain, inducing radical cleavage of the carbon-carbon bonds and thereby causing extensive fragmentation that can be used for detailed structure elucidation of the O-alkyl moiety. The separability of related isomers was tested by comparing the spectra of the picolinyl esters formed from twelve hexyl methylphosphonic acid isomers. Spectral library matches and principal component analysis showed that the picolinyl esters were more effectively separated than the corresponding trimethylsilyl derivatives used in the standard operating procedures. The suggested method will improve the unambiguous structural determination process for phosphonic acids.

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“…A large number of publications reported on the detection and analysis of chemical and biological warfare agents (CBWAs) using chromatographic methods coupled to mass spectrometry, − including the analysis of capsicum extracts from self-defense devices, carbon nanotube sensors, , direct analysis in real time (DART) coupled to MS, aninon exchange SPE, and nanopore sensing . Light isotopes were investigated for the analysis of wood safety matches and to determine geographic provenance of marijuana plants, and lead isotopes were analyzed to distinguish between legal and counterfeit tobacco cigarettes .…”

Section: Forensic Examination Of Trace Evidencementioning

confidence: 99%

Forensic Science

2011

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Analytical ChemistryREVIEW worth noting that conference proceedings are available online for important meetings in this field including the International Symposium on Human Identification (aka the "Promega meeting") (http://www.promega.com/geneticidproc/) and the International Society of Forensic Genetics (ISFG) (http://www. isfg.org) meetings. Volume 13 of Progress in Forensic Genetics, which contains the proceedings of the ISFG meeting held in Buenos Aires, Argentina, in September 2009, includes 250 brief articles covering current research on all aspects of forensic DNA typing. 2 Short tandem repeat (STR) typing of autosomal markers with fluorescence-based detection is now almost universally used in forensic DNA laboratories worldwide. 3 Reduced-size STR, or miniSTR, assays are being developed for improved recovery of information from badly damaged DNA templates. Low level DNA and samples containing mixtures continue to present challenges for forensic analysts. A large portion of the literature involves reporting STR allele frequencies from various populations. However, limited space in this review prevents a summary or description of the many population studies performed in 2009 and 2010.Single nucleotide polymorphisms (SNPs) continue to be explored as potential supplements to STR markers already in use but will probably not replace STRs in the near future. Information on uniparental lineage markers from the Y-chromosome and mitochondrial DNA continues to accumulate in the literature. These lineage markers are also widely used for human evolutionary studies and genetic genealogy. The availability of commercial kits for Y-STR amplification has enabled more widespread usage of these important male-specific markers in forensic DNA laboratories. A number of X-chromosome STRs are also being investigated. Nonhuman DNA plays a useful role in many forensic investigations. Tests have been developed for plant and animal DNA testing to associate victims or suspects to crime scenes.National DNA databases collectively house millions of STR profiles around the world. With the demonstrated success of linking previous offenders to unsolved crimes they have committed, new legislation is expanding the number of samples that will be going into DNA databases of the future. In December 2010, the United States exceeded 9.5 million DNA profiles in the National DNA Index System of the FBI Laboratory's Combined DNA Index System (CODIS). The United Kingdom has over four million STR profiles in their national DNA database, which represents a significant portion of their active criminal population.Automation of laboratory techniques and data interpretation with expert systems has become increasingly important with the large numbers of DNA samples that need to be examined. Forensic DNA testing also aids missing persons investigations and identification of mass disaster victims albeit with some extra issues unique to kinship and parentage analysis. At the end of the forensic DNA analysis section, we also list relevant papers on interpretat...

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Combination of solid phase extraction and in vial solid phase derivatization using a strong anion exchange disk for the determination of nerve agent markers

Cited by 32 publications

References 28 publications

Analysis of Organophosphorus-Based Nerve Agent Degradation Products by Gas Chromatography-Mass Spectrometry (GC-MS): Current Derivatization Reactions in the Analytical Chemist’s Toolbox

Analysis of Organophosphorus-Based Nerve Agent Degradation Products by Gas Chromatography-Mass Spectrometry (GC-MS): Current Derivatization Reactions in the Analytical Chemist’s Toolbox

Structural determination of nerve agent markers using gas chromatography mass spectrometry after derivatization with 3‐pyridyldiazomethane

Forensic Science

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