Solid phase microextraction with analysis by gas chromatography to determine short term hydrogen cyanide concentrations in a field setting

Smith, Philip A.; Sheely, Michael V.; Kluchinsky, Timothy A.

doi:10.1002/1615-9314(20021001)25:14<917::aid-jssc917>3.0.co;2-f

Cited by 20 publications

(15 citation statements)

References 7 publications

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“…Schneider et al [12] developed a method to screen air and water with SPME followed by laboratory GC/MS analysis for the volatile nerve agent Sarin. Smith et al [13] developed a SPME field sampling method for airborne hydrogen cyanide with laboratory GC analysis and nitrogen-phosphorous detection (NPD). Lakso and Ng [14] compared the use of SPME-GC/NPD with liquid-liquid extraction for detection of the nerve agents sarin, soman, tabun, and Oethyl S-(2-diisopropylaminoethyl) methylphosphonothiolate (VX) in water.…”

Section: Introductionmentioning

confidence: 99%

Solid phase microextraction sampling and gas chromatography/mass spectrometry for field detection of the chemical warfare agent O‐ethyl S‐(2‐diisopropylaminoethyl) methylphosphonothiolate (VX)

Hook

Kimm

Betsinger

et al. 2003

J of Separation Science

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Solid phase microextraction sampling and gas chromatography/mass spectrometry for field detection of the chemical warfare agent O-ethyl S-(2-diisopropylaminoethyl) methylphosphonothiolate (VX)A rapid detection method for the chemical warfare nerve agent VX was developed using SPME and gas chromatography/mass spectrometry (GC/MS). Five commercially available SPME fiber coatings were evaluated to determine the optimal fiber coating and conditions for extraction. The use of silanized vials was found to be necessary to limit interaction of the basic tertiary amine component of VX with the acidic silanols present in standard glass vials. The polydimethylsiloxane (PDMS) fiber was ultimately selected for completion of this work with extractions being performed at 508C. Clothing material was spiked in the laboratory with 1 lL of neat VX, placed in a sealed vial, and taken into the field for SPME sampling, using optimized conditions studied. GC/MS analysis was also completed in the field using van-mounted instrumentation. With sampling and analysis completed in less than 20.0 minutes, detection of VX contamination was relatively rapid, especially considering the quality of the resulting data. The use of SPME also provides increased safety for the field analysis of VX since it does not require the handling of solvents for sample preparation and samples are not handled directly by the analyst.

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Section: Introductionmentioning

confidence: 99%

Solid phase microextraction sampling and gas chromatography/mass spectrometry for field detection of the chemical warfare agent O‐ethyl S‐(2‐diisopropylaminoethyl) methylphosphonothiolate (VX)

Hook

Kimm

Betsinger

et al. 2003

J of Separation Science

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“…There are a number of reports that validate the use of SPME for the analysis of CWAs in air, water, and soil [46 -51]. These studies include the analysis of hydrogen cyanide [46], VX [50,52], sarin [48 -50], soman [50], tabun [50], and mustard [51]. There have also been reports describing the detection of precursor chemicals and degradation products of CWAs using SPME [52][53][54][55].…”

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confidence: 99%

Hand-portable gas chromatograph-toroidal ion trap mass spectrometer (GC-TMS) for detection of hazardous compounds

Contreras

Murray

Tolley³

et al. 2008

J. Am. Soc. Mass Spectrom.

239

156

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A novel gas chromatograph-mass spectrometer (GC-MS) based on a miniature toroidal ion trap mass analyzer (TMS) and a low thermal mass GC is described. The TMS system has an effective mass/charge (m/z) range of 50-442 with mass resolution at full-width half-maximum (FWHM) of 0.55 at m/z 91 and 0.80 at m/z 222. A solid-phase microextraction (SPME) fiber mounted in a simple syringe-style holder is used for sample collection and introduction into a specially designed low thermal mass GC injection port. This portable GC-TMS system weighs <13 kg (28 lb), including batteries and helium carrier gas cartridge, and is totally self-contained within dimensions of 47 X 36 X 18 em (18.5 X 14 X 7 in.). System start-up takes about 3 min and sample analysis with library matching typically takes about 5 min, including time for column cool-down. Peak power consumption during sample analysis is about 80 W. Battery power and helium supply cartridges allow 50 and 100 consecutive analyses, respectively. Both can be easily replaced. An on-board library of target analytes is used to provide detection and identification of chemical compounds based on their characteristic retention times and mass spectra. The GC-TMS can detect 200 pg of methyl salicylate on-column. n-Butylbenzene and naphthalene can be detected at a concentration of 100 ppt in water from solid-phase microextraction (SPME) analysis of the headspace. The GC-TMS system has been designed to easily make measurements in a variety of complex and harsh environments. and toxic industrial chemicals (TICs), is a concern, the ability to rapidly detect and accurately identify such chemicals in harsh environments is of great utility. There is a need for field-portable, selective, and sensitive detectors for military and emergency first-responder operations and for on-site environmental contamination measurement, to mention only a couple of key applications. The development of fieldportable devices directed toward fast, on-site analysis is one of the most active research areas in analytical chemistry.Currently, several approaches for detection of CWAs and TICs are utilized by military personnel, first responders, and environmental scientists. They include dye solubility (detection paper), enzymatic reaction,

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“…A large number of biomedical SPME applications have been reported,26–28 including our methods for determining several xenobiotics in different biological fluids 29–31. Some HS‐SPME methods have also been published for measuring CN in human whole blood20, 32 or in air33 after its conversion into HCN.…”

mentioning

confidence: 99%

An improved method for cyanide determination in blood using solid‐phase microextraction and gas chromatography/mass spectrometry

Frison

Zancanaro

Favretto

et al. 2006

Rapid Comm Mass Spectrometry

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A new method is described for the qualitative and quantitative analysis of cyanide, a very short-acting and powerful toxic agent, in human whole blood. It involves the conversion of cyanide into hydrogen cyanide and its subsequent headspace solid-phase microextraction (HS-SPME) and detection by gas chromatography/mass spectrometry (GC/MS) in selected ion monitoring (SIM) mode. Optimizing the conditions for the GC/MS (type of column, injection conditions, temperature program) and SPME (choice of SPME fiber, effect of salts, adsorption and desorption times, adsorption temperature) led to the choice of a 75-microm carboxen/polydimethylsiloxane SPME fiber, with D3-acetonitrile as internal standard, and a capillary GC column with a polar stationary phase. Method validation was carried out in terms of linearity, precision and accuracy in both aqueous solutions and blood. The limit of detection (LOD) and limit of quantitation (LOQ) were determined only in aqueous solutions. The assay is linear over three orders of magnitude (water 0.01-10, blood 0.05-10 microg/mL); and the LOD and LOQ in water were 0.006 and 0.01 microg/mL, respectively. Good intra- and inter-assay precision was obtained, always <8%. The method is simple, fast and sensitive enough for the rapid diagnosis of cyanide intoxication in clinical and forensic toxicology.

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Solid phase microextraction with analysis by gas chromatography to determine short term hydrogen cyanide concentrations in a field setting

Cited by 20 publications

References 7 publications

Solid phase microextraction sampling and gas chromatography/mass spectrometry for field detection of the chemical warfare agent O‐ethyl S‐(2‐diisopropylaminoethyl) methylphosphonothiolate (VX)

Solid phase microextraction sampling and gas chromatography/mass spectrometry for field detection of the chemical warfare agent O‐ethyl S‐(2‐diisopropylaminoethyl) methylphosphonothiolate (VX)

Hand-portable gas chromatograph-toroidal ion trap mass spectrometer (GC-TMS) for detection of hazardous compounds

An improved method for cyanide determination in blood using solid‐phase microextraction and gas chromatography/mass spectrometry

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