Headspace-trap gas chromatography–mass spectrometry for determination of sulphur mustard and related compounds in soil

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

doi:10.1016/j.chroma.2010.01.088

Cited by 29 publications

(12 citation statements)

References 19 publications

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“…These analytes are then thermally desorbed and sent to the GC column with the flow of carrier gas. This technique is still not widespread despite its having been used since the early 2000s . Until today, very few reports have been published on the application of HS Trap on edible oils.…”

Section: Introductionmentioning

confidence: 99%

Analysis of target volatile compounds related to fishy off‐flavor in heated rapeseed oil: A comparative study of different headspace techniques

Sghaier

Vial

Sassiat

et al. 2015

Euro J Lipid Sci & Tech

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Off‐flavors, characterized by a fishy odor, are emitted during the heating of rapeseed oil in a fryer. In order to study the headspace composition of degraded rapeseed oil, and more specifically the compounds responsible for the fishy odor, four headspace techniques were evaluated: Static headspace (SHS), headspace trap (HS Trap), headspace solid phase microextraction (HS‐SPME), and headspace sorptive extraction (HSSE) coupled to gas chromatography‐mass spectrometry (GC‐MS). The selected model compounds to develop the headspace methods were 1‐penten‐3‐one, 1‐octen‐3‐one, and E,Z‐2,6‐nonadienal as known fishy odor markers. Extraction conditions for the four techniques were optimized and evaluated in terms of repeatability and sensitivity. They were then applied to the analysis of real samples of degraded rapeseed oil. SHS was not suitable for the analysis of odorant volatile compounds because of LOD values lower than those required for a quantitative analysis of the target compounds. Concerning HS‐SPME and HSSE, a discrimination against the more volatile compounds was observed. Finally, HS Trap‐GC‐MS was considered the most appropriate technique for the analysis of the headspace of rapeseed oil in this study with LOD values less than 2 μg/L for the three target compounds. More than 60 compounds were identified by HS Trap‐GC‐MS and two compounds responsible for the fishy odor could be detected. The evolution of the relative areas of these compounds was reported for fresh oil and rapeseed oil degraded by 1, 5, and 10 heating cycles. Practical applications: The characterization of the volatile compounds responsible for the fishy odor is a key industrial issue. Moreover, the developed method with HS‐Trap could be used to quantify several volatile compounds characteristic of the degradation of rapeseed oil, and to evaluate the possible effect of antioxidants on oils. Rapeseed oil is edible oil containing a substantial amount of omega 3, but the heating of this oil leads to the formation of off‐flavors, characterized by a fishy odor. The characterization of these off‐flavors is a key industrial issue, and different headspace techniques can be considered to study the molecules present in the headspace of degraded rapeseed oil.

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Section: Introductionmentioning

confidence: 99%

Analysis of target volatile compounds related to fishy off‐flavor in heated rapeseed oil: A comparative study of different headspace techniques

Sghaier

Vial

Sassiat

et al. 2015

Euro J Lipid Sci & Tech

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“…The reactions of 2-CEES in water, water/acetone, and water/ethanol mixtures have been investigated. [3][4][5][6][7][8] These studies indicate that the reaction mechanism is the same as shown in Figure 1. The first step is the formation of a cyclic sulfonium cation via the intramolecular assistance of the neighboring sulfur; the cyclic sulfonium cation then reacts quickly with water to form 2-hydroethyl ethyl sulfide (2-HEES), or reacts with 2-CEES to form (CH 3 CH 2 )(CH 2 CH 2 Cl)S + (CH 2 CH 2 SCH 2 CH 3 ) product (ECT), or continue to react with the initial product 2-HEES to form (CH 3 CH 2 ) (CH 2 CH 2 OH)S + (CH 2 CH 2 SCH 2 CH 3 ) product (EHT).…”

Section: Introductionmentioning

confidence: 49%

Reaction Products and Process of 2-Chloroethyl Ethyl Sulfide in Microemulsion Media

Lei

Shen

et al. 2014

Phosphorus, Sulfur, and Silicon and the Related Elements

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GRAPHICAL ABSTRACTCl S +H 2 O S OH S S Cl S S OH S Cl H S OH S Cl +H 2 O _ ECT EHT 2-CEES 2-HEES Abstract The reaction of 2-chloroethyl ethyl sulfide was investigated in several oil-in-water microemulsions. The reaction products were identified by GC/MS, NMR, and LC/MS, and the reaction process was monitored by measuring peak height of reaction products and 2-chloroethyl ethyl sulfide with time by 1 H NMR spectroscopy. The result showed that 2-chloroethyl ethyl sulfide degraded to 2-hydroxyethyl ethyl sulfide, cyclic sulfonium ion, open chain sulfonium chloro ion and sulfonium hydroxyl ion, and the reaction proceeded via a cyclic sulfonium ion intermediate. Based on the NMR results, a pseudoternary model was established for the reaction process of 2-chloroethyl ethyl sulfide in microemulsion.

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“…TDG may be oxidized to thiodiglycol sulfoxide (TDGO) and, more slowly, to thiodiglycol sulfone (TDGOO) . HD and its degradation products TDG, TDGO, and TDGOO are surprisingly rarely found in the sediment and water samples from the dumpsites , whereas the cyclic compounds are quite frequently found in the real samples from the dumpsites . The analysis of HD degradation products indicates the presence and leakage of HD from the corroded shells.…”

Section: Introductionmentioning

confidence: 99%

“…Røen et al. have developed methods for the trace determination of cyclic HD degradation compounds in soil and water samples using headspace‐trap in combination with GC‐MS. The cyclic sulfur compounds 1,4‐thioxane, 1,3‐dithiolane, and 1,4‐dithiane could be detected at 0.2–0.7 ng/g in soil samples and at 0.1 ng/mL in water samples.…”

Section: Introductionmentioning

confidence: 99%

Development and comparison of HPLC and MEKC methods for the analysis of cyclic sulfur mustard degradation products

2017

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In this study, novel, fast, and simple methods based on RP-HPLC and MEKC with DAD are developed and validated for the qualitative and quantitative determination of five cyclic sulfur mustard (HD) degradation products (1,4-thioxane, 1,3-dithiolane, 1,4-dithiane, 1,2,5-trithiepane, and 1,4,5-oxadithiepane) in water samples. The HPLC method employs a C18 column and an isocratic water-ACN (55:45, v/v) mobile phase. This method enables separation of all five cyclic compounds within 8 min. With the CE method, the baseline separation of five compounds was achieved in less than 11 min by applying a simple BGE composed of a 10 mM borate buffer and 90 mM SDS (pH 9.15). Both methods showed good linear correlation (R > 0.9904). The detection limits were in the range of 0.08-0.1 μM for the HPLC method and 10-20 μM for MEKC. The precision tests resulted in RSDs for migration times and peak areas less than 0.9 and 5.5%, respectively, for the HPLC method, and less than 1.1 and 7.7% for the MEKC method, respectively. The developed methods were successfully applied to the analysis of five cyclic HD degradation products in water samples. With the HPLC method, the LODs were lowered using the SPE for sample purification and concentration.

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Headspace-trap gas chromatography–mass spectrometry for determination of sulphur mustard and related compounds in soil

Cited by 29 publications

References 19 publications

Analysis of target volatile compounds related to fishy off‐flavor in heated rapeseed oil: A comparative study of different headspace techniques

Analysis of target volatile compounds related to fishy off‐flavor in heated rapeseed oil: A comparative study of different headspace techniques

Reaction Products and Process of 2-Chloroethyl Ethyl Sulfide in Microemulsion Media

Development and comparison of HPLC and MEKC methods for the analysis of cyclic sulfur mustard degradation products

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