Trace determination of sulphur mustard and related compounds in water by headspace-trap gas chromatography–mass spectrometry

Røen, Bent Tore; Unneberg, Erik; Tørnes, John Aasulf; Lundanes, Elsa

doi:10.1016/j.chroma.2009.12.008

Cited by 25 publications

(22 citation statements)

References 31 publications

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“…The trap is maintained at lower temperature, just above ambient, leading to condensation of the gaseous phase, while water can be removed by purging helium through the trap. Then, the trap is heated and backflushed, leading to desorption of the analytes that enter the chromatographic system [3].…”

Section: Headspace-trap Settingsmentioning

confidence: 99%

“…A DB-624 (30m x 0.25 mm ID x 1.4 µm film thickness) (Agilent, Avondale, PA, USA) analytical column was chosen. The HS transfer line was directly coupled to the analytical column using a butt connector, and was maintained at 150 °C, as recommended by the manufacturer, to avoid condensation on possible cold spots [3]. Helium was used as carrier gas, at constant column inlet pressure of 15 psi.…”

Section: Gc-ms Analysismentioning

confidence: 99%

“…In addition, when dealing with aqueous matrices, water removal prior to GC-MS analysis needs special consideration. The latter was achieved by dry purging the trap between its loading and desorption [3].…”

Section: Trap Settingsmentioning

confidence: 99%

“…Only relatively recently, a new HS technique has been commercialized: HS-trap, encompassing an enhanced static headspace system covering both static and dynamic HS properties. This technique, already successfully applied to determine various volatile compounds in water [3], spirits [4], soil [5], apple juices [6] and plant matrices [7], was evaluated for its possibility to determine gamma-hydroxybutyric acid (GHB), a low molecular weight compound and drug of abuse, in biofluids such as urine, plasma, serum and whole blood. Detection and quantification of GHB in biological matrices is of interest in toxicological cases, since recreational use with limited awareness of the possibility to suddenly fall into a coma has resulted in an increase in GHB intoxications at raves or other dance parties [8,9].…”

Section: Introductionmentioning

confidence: 99%

“…A third advantage is that smaller sample volumes may be analyzed, while still providing enough sensitivity. This is because, when compared to SPME or SPDE, the trap described here allows sampling of a larger headspace fraction, since its adsorptive capacity (having a solid sorbent volume of 160 mm 3 ) is much larger than that of the small fibers or coated capillaries (having volumes of 0.94-5.99 mm 3 ) used in SPME or SPDE [4]. Furthermore, by combining "in-vial" derivatization and HS-trap, the application range can be extended to non-volatile analytes, with a negligible increase in workload [21].…”

Section: Introductionmentioning

confidence: 99%

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Determination of gamma-hydroxybutyric acid in biofluids using a one-step procedure with “in-vial” derivatization and headspace-trap gas chromatography–mass spectrometry

Ingels¹,

Neels²,

Lambert³

et al. 2013

Journal of Chromatography A

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A headspace-trap gas chromatography-mass spectrometry (HS-trap GC-MS) method was developed to determine GHB, a low molecular weight compound and drug of abuse, in various biological fluids. Combining this relatively novel and fully automated headspace technique with "in-vial" methylation of GHB allowed for a straightforward approach. One single method could be used for all biofluids (urine, plasma, serum, whole blood or lyzed blood), requiring only 100 µl of sample. Moreover, our approach involves mere addition of all reagents and sample into one vial. Following optimization of headspace conditions and trap settings, validation was performed. Although sample preparation only consists of the addition of salt and derivatization reagents directly to a 100 µl-sample in a HS-vial, adequate method sensitivity and selectivity was obtained. Calibration curves ranged from 5 to 150 µg/ml GHB for urine, from 2 to 150 µg/ml for plasma, and from 3.5 to 200 µg/ml for whole blood. Acceptable precision and accuracy (<13 % bias and imprecision) was seen for all quality controls (QC's) (LLOQ-level, low, medium, high), including for the supplementary serum-and lyzed blood-based QC's, using calibration curves prepared in plasma or whole blood, respectively. Incurred sample reanalysis demonstrated assay reproducibility, while cross-validation with another GC-MS method demonstrated that our method is a valuable alternative for GHB determination in toxicological samples, with the advantage of requiring only 100 µl and minimal hands-on time, as sample preparation is easy and injection automated. KeywordsGamma-hydroxybutyric acid (GHB), in-vial derivatization, gas chromatography coupled to mass spectrometry (GC-MS), headspace-trap (HS-trap), biological matrices, toxicology 3

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Section: Headspace-trap Settingsmentioning

confidence: 99%

Section: Gc-ms Analysismentioning

confidence: 99%

Section: Trap Settingsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 3 more Smart Citations

Determination of gamma-hydroxybutyric acid in biofluids using a one-step procedure with “in-vial” derivatization and headspace-trap gas chromatography–mass spectrometry

Ingels¹,

Neels²,

Lambert³

et al. 2013

Journal of Chromatography A

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Gas Chromatography in Screening of Chemicals Related to the Chemical Weapons Convention

Kostiainen

2016

Encyclopedia of Analytical Chemistry

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Various gas chromatographic methods, which are useful for the screening of chemical weapons convention (CWC)‐related chemicals, are described in this article. The choice of columns, detectors, and injection techniques, crucial to the optimization of gas chromatography (GC) as a routine screening tool, is discussed. In addition, various screening and identification methods are described. The use of retention indices (RI) method allowing the identification without the need for an authentic chemical is described in detail. RIs are used as identification method also together with electron impact mass spectrometry (EIMS) in on‐site analysis method established by Organization for Prohibition of Chemical Weapons (OPCW).

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Current Awareness in Drug Testing and Analysis

2010

Drug Testing and Analysis

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J Forensic Sci 2010 55 (2) 451 Paradigm shift for the alcohol breath testThe alcohol breath test (ABT) has been used for quantification of ethyl alcohol in individuals suspected of driving under the influence for more than 50 years. In this time, there has been little change in the concepts underlying this single breath test. The old model, which assumes that end-exhaled breath alcohol concentration is closely related to alveolar air alcohol concentration, is no longer acceptable. This paper reviews experimental research and mathematical modeling which has evaluated the pulmonary exchange processes for ethyl alcohol. Studies have shown that alcohol exchanges dynamically with the airway tissue both during inspiration and expiration. The airway tissue interaction makes it impossible to deliver air with alveolar alcohol concentration to the mouth. It is concluded that the ABT is dependent on physiological factors that need to be assessed for accurate testing Jackson G, Arver S, Banks I, Stecher VJ// London Bridge Hosp, 27 Tooley St, Emblem House, London SE1 2PR, England Int J Clin Pract 2010 64 (4) 497 Counterfeit phosphodiesterase type 5 inhibitors pose significant safety risks Counterfeit drugs are inherently dangerous and a growing problem; counterfeiters are becoming increasingly sophisticated. Growth of the counterfeit medication market is attributable in part to phosphodiesterase type 5 inhibitor (PDE5i) medications for erectile dysfunction (ED). Millions of counterfeit PDE5is are seized yearly and account for the bulk of all counterfeit pharmaceutical product seizures. It has been estimated that up to 2.5 million men in Europe are exposed to illicit sildenafil, suggesting that there may be as many illegal as legal users of sildenafil. Analysis of the contents of counterfeit PDE5is shows inconsistent doses of active pharmaceutical ingredients (from 0% to > 200% of labelled dose), contaminants (including talcum powder, commercial paint and printer ink) and alternative ingredients that are potentially hazardous. In one analysis, only 10.1% of samples were within 10% of the labelled tablet strength. Estimates place the proportion of counterfeit medications sold over the Internet from 44% to 90%. Of men who purchase prescription-only medication for ED without a prescription, 67% do so using the Internet. Counterfeit PDE5is pose direct and indirect risks to health, including circumvention of the healthcare system. More than 30% of men reported no healthcare interaction when purchasing ED medications. Because > 65% actually had ED, these men missed an opportunity for evaluation of comorbidities (e.g. diabetes and hypertension). Globally, increased obstacles for counterfeiters are necessary to combat pharmaceutical counterfeiting, including fines and penalties. The worldwide nature of the counterfeit problem requires proper coordination between countries to ensure adequate enforcement. Locally, physicians who treat ED need to inform patients of the dangers of ordering PDE5is via the Internet

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Trace determination of sulphur mustard and related compounds in water by headspace-trap gas chromatography–mass spectrometry

Cited by 25 publications

References 31 publications

Determination of gamma-hydroxybutyric acid in biofluids using a one-step procedure with “in-vial” derivatization and headspace-trap gas chromatography–mass spectrometry

Determination of gamma-hydroxybutyric acid in biofluids using a one-step procedure with “in-vial” derivatization and headspace-trap gas chromatography–mass spectrometry

Gas Chromatography in Screening of Chemicals Related to the Chemical Weapons Convention

Current Awareness in Drug Testing and Analysis

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