Atomic emission detection for the quantitation of trimethylsilyl derivatives of chemical-warfare-agent related compounds in environmental samples

Creasy, William R.; Rodríguez, Alex A.; Stuff, John R.; Warren, Robert W.

doi:10.1016/0021-9673(95)00451-r

Cited by 72 publications

(19 citation statements)

References 16 publications

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“…This can be achieved by solvent extraction [7], co-distillation [21], various solid phase extraction techniques [22,23,27,28] or by phase transfer processes [24]. In this work, isolation by anion exchange SPE was evaluated but found to require excessive time for concentrating the eluate (aqueous sodium bromide) containing the acids to dryness.…”

Section: Sample Preparationmentioning

confidence: 99%

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The trace analysis of alkyl alkylphosphonic acids in urine using gas chromatography–ion trap negative ion tandem mass spectrometry

Riches

Morton

Read

et al. 2005

Journal of Chromatography B

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Section: Sample Preparationmentioning

confidence: 99%

“…These include extraction of the non-ionised acid on hydrophobic cartridges [22] or capture of the ionised acid on anion exchange cartridges [23,27,28]. An alternative to selective extraction is to remove extraneous materials from urine, e.g.…”

Section: Sample Preparationmentioning

confidence: 99%

The trace analysis of alkyl alkylphosphonic acids in urine using gas chromatography–ion trap negative ion tandem mass spectrometry

Riches

Morton

Read

et al. 2005

Journal of Chromatography B

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“…Moreover, some neutral compounds, such as carbohydrates, which contain hydroxide groups competed against the phosphonates in the silylation reaction and suppressed the TBDMS derivatization. 28,31) Several investigations on cleanup of nerve gas hydrolysis products using solid phase extraction (SPE) have been reported, 23,25,[32][33][34] and some drawbacks were found such as low recoveries of RMPAs and MPA and insufficient information about SPE procedures. We attempted some types of SPE including strong cation-exchanger, 28) anionexchanger and reversed-phase 31,35) followed by TBDMS derivatization.…”

Section: Fig 4 Effects Of Alkaline Earth Metals On the Detection Yimentioning

confidence: 99%

Laboratory Identification of the Nerve Gas Hydrolysis Products Alkyl Methylphosphonic Acids and Methylphosphonic Acid, by Gas Chromatography-mass Spectrometry after <i>tert</i>-Butyldimethylsilylation

Kanamori-Kataoka

Seto

2008

JOURNAL OF HEALTH SCIENCE

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Alkyl methylphosphonic acids (RMPAs) and methylphosphonic acid (MPA), both nerve gas hydrolysis products, can be identified by gas chromatography-mass spectrometry (GC-MS). We adopted tertbutyldimethylsilylation (TBDMS) as a derivatization technique for the identification of these products by GC-MS. We found that it was difficult to detect RMPAs and MPA from evidence specimens such as soils and body fluids, and ascertained several causes for this. The first is the interference from the TBDMS derivatization. It was determined that the TBDMS derivatization of RMPAs and MPA was suppressed in the presence of divalent metal cations such as calcium and magnesium ions, as well as some neutral compounds like carbohydrates. A cleanup procedure using a strong anion-exchanger (SAX)-solid phase extraction (SPE) method was optimized to remove the interfering compounds. The second reason that detection was difficult was because of strong matrix adsorption. We elucidated that the aqueous extraction recoveries for all phosphonates were inversely correlated with the phosphate adsorption coefficient in the soil samples. To diminish the adsorption of phosphonates to soils, a method of alkali extraction was adopted. For human serum samples, we adopted acetonitrile or trichloroacetic acid deproteinization which worked to break the binding between the proteins and the phosphonates. The detection yields of RMPAs and MPA from soils and human serum were dramatically increased using these pretreatment procedures combined with extraction and/or SAX-SPE. The method of SAX-SPE was applied to various types of samples, such as seawater, drinks and human urine, and good detection yields of RMPAs and MPA were provided by GC-MS.

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“…In such cases, sample extraction methods are very crucial for selective removal of background to detect CWAs in the presence of complex background material. Solid-phase extraction (SPE) and solid-phase microextraction (SPME) have been extensively used as the sample preparation techniques for the analysis of toxic chemicals present in aqueous samples [10][11][12][13][14][15][16][17][18][19][20][21][22][23][24][25][26]. However, there are no reports of using SPE for the analysis of CWAs present in complex organic backgrounds.…”

Section: Introductionmentioning

confidence: 99%

Trace level detection and identification of chemicals related to the chemical weapons convention from complex organic samples

Reddy

Saradhi

Prabhakar

et al. 2004

Journal of Chromatography A

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Atomic emission detection for the quantitation of trimethylsilyl derivatives of chemical-warfare-agent related compounds in environmental samples

Cited by 72 publications

References 16 publications

The trace analysis of alkyl alkylphosphonic acids in urine using gas chromatography–ion trap negative ion tandem mass spectrometry

The trace analysis of alkyl alkylphosphonic acids in urine using gas chromatography–ion trap negative ion tandem mass spectrometry

Laboratory Identification of the Nerve Gas Hydrolysis Products Alkyl Methylphosphonic Acids and Methylphosphonic Acid, by Gas Chromatography-mass Spectrometry after <i>tert</i>-Butyldimethylsilylation

Trace level detection and identification of chemicals related to the chemical weapons convention from complex organic samples

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