New approach on the alkylthiol determination in water by<i>in situ</i>derivatization SPME followed by GC-ECD/NPD analysis

Salgado-Petinal, Carmen; Alzaga, Roberto; Garcı́a-Jares, Carmen; Llompart, Marı́a; Bayona, Josep M.

doi:10.1080/03067310500107195

Cited by 7 publications

(6 citation statements)

References 12 publications

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“…There are several organic compounds suitable to react with an SH group forming a stable derivative, but most of these reagents require the presence of organic media, as they would be hydrolyzed when they are used directly in aqueous solution. Previous experience with the 2,4-dinitrofluorobenzene showed it to be a suitable derivatization reagent for alkanethiols in distilled water, but some inconvenience appeared when it was used to form the corresponding alkanethiol derivatives in complex aqueous samples . In the present work, the NEM feasibility as a proper derivatization reagent of alkanethiols and dihydrogen sulfide in water samples (Figure ) and the ability of SPME to extract the derivatives from the aqueous media were evaluated.…”

Section: Resultsmentioning

confidence: 94%

“…Previous experience with the 2,4-dinitrofluorobenzene showed it to be a suitable derivatization reagent for alkanethiols in distilled water, but some inconvenience appeared when it was used to form the corresponding alkanethiol derivatives in complex aqueous samples. 22 In the present work, the NEM feasibility as a proper derivatization reagent of alkanethiols and dihydrogen sulfide in water samples (Figure 1) and the ability of SPME to extract the derivatives from the aqueous media were evaluated. The in-fiber derivatization was also tested, but no successful results using this derivatization procedure were obtained.…”

Section: Resultsmentioning

confidence: 99%

“…Consequently, the newly developed methodology improves the one developed previously by using 2,4-dinitrofluorobenzene as derivatization reagent since it suffered from matrix effects in aqueous complex matrixes. 22 Application of the Developed Method to Different Aqueous Samples. Several aqueous samples collected from different sewage treatment plants, were analyzed by applying the developed analytical methodology.…”

Section: Resultsmentioning

confidence: 99%

“…In fact, a matrix effect appeared when environmental matrixes were analyzed and dihydrogen sulfide could not be analyzed. 22 It is important to notice that the derivatization efficiency is dependent on both the choice and the concentration of the derivatization reagent, as well as the matrix conditions. 21 Maleimides are a well-known chemical class widely used to react with, protect, block, or simply label the SH groups on proteins or other molecules.…”

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confidence: 99%

“…In a previous study, we employed the 2,4-dinitrofluorobenzene as derivatization reagent, obtaining a suitable methodology limited to noncomplex aqueous matrixes. In fact, a matrix effect appeared when environmental matrixes were analyzed and dihydrogen sulfide could not be analyzed . It is important to notice that the derivatization efficiency is dependent on both the choice and the concentration of the derivatization reagent, as well as the matrix conditions .…”

mentioning

confidence: 99%

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Low Part per Trillion Determination of Reactive Alkanethiols in Wastewater by in Situ Derivatization-Solid-Phase Microextraction Followed by GC/MS

et al. 2005

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A solid-phase microextraction (SPME) procedure for the simultaneous determination of volatile alkanethiols (i.e., methane-, ethane-, propanethiol) and dihydrogen sulfide in aqueous samples as stable thioethers followed by GC/MS determination was developed. Accordingly, N-ethylmaleimide as derivatization reagent in the aqueous phase was used for the first time, improving the analyte stability and method sensitivity in comparison to the determination of free forms. Thus, pH of the aqueous medium, reaction time, and derivatization reagent concentration have been evaluated, and the main parameters affecting the SPME process (i.e., coating selection, extraction mode and time profile, extraction and desorption temperatures) optimized. At the selected derivatization and extraction conditions, the proposed method provided no matrix effect either in the derivatization reaction or in the microextraction steps. RSD values were lower than 11% and LODs from 0.74 to 5.2 ng L(-1). The developed procedure was successfully applied to different water and wastewater samples, where dihydrogen sulfide and some of the target alkanethiols were identified at low-microgram per liter concentrations.

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Section: Resultsmentioning

confidence: 94%

Section: Resultsmentioning

confidence: 99%

Section: Resultsmentioning

confidence: 99%

mentioning

confidence: 99%

mentioning

confidence: 99%

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Low Part per Trillion Determination of Reactive Alkanethiols in Wastewater by in Situ Derivatization-Solid-Phase Microextraction Followed by GC/MS

et al. 2005

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Selective preconcentration of volatile mercaptans in small SPE cartridges: Quantitative determination of trace odor‐active polyfunctional mercaptans in wine

Mateo-Vivaracho

Cacho

Ferreira

2009

J of Separation Science

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A general procedure for the selective preconcentration and purification of mercaptans has been developed. Mercaptans are strongly retained in a small (20 mg) SPE cartridge containing p-hydroxymercurybenzoate. The cartridge can then be rinsed with relatively high volumes of polar (water/methanol mixtures) and non-polar (pentane or pentane/ ether mixtures) rinsing solutions to remove nearly all volatile compounds lacking a thiol functionality. Retained analytes are further eluted with a small volume of an organic solvent containing 1,4-dithioerythritol. Some basic aspects of the strategy, such as the retention of p-hydroxymercurybenzoate in the sorbent and its stability versus different rinsing and eluting systems, have been studied in depth. Light sulfur compounds contained in water or wine, including mercaptans such as methanethiol or thioethers, such as diethyl sulfide, can be quantitatively extracted, although only mercaptans can be quantitatively recovered if a polar rinsing is applied. The strategy has been applied to the GC-MS quantitative determination of some trace polyfunctional mercaptans that are key aromas in wine, such as 2-methyl-3-furanthiol, 2-furfurylthiol, 4-mercapto-4-methyl-2-pentanone, 3-mercaptohexyl acetate or 3-mercaptohexanol. The developed method reaches detection limits in the ng/L range and has a satisfactory analytical behavior, being quite simple and fast.

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Strategies for the microextraction of polar organic contaminants in water samples

Quintana

Rodrı́guez

2006

Anal Bioanal Chem

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In this paper the most recent developments in the microextraction of polar analytes from aqueous environmental samples are critically reviewed. The particularities of different microextraction approaches, mainly solid-phase microextraction (SPME), stir-bar-sorptive extraction (SBSE), and liquid-phase microextraction (LPME), and their suitability for use in combination with chromatographic or electrically driven separation techniques for determination of polar species are discussed. The compatibility of microextraction techniques, especially SPME, with different derivatisation strategies enabling GC determination of polar analytes and improving their extractability is revised. In addition to the use of derivatisation reactions, the possibility of enhancing the yield of solid-phase microextraction methods for polar analytes by using new coatings and/or larger amounts of sorbent is also considered. Finally, attention is also focussed on describing the versatility of LPME in its different possible formats and its ability to improve selectivity in the extraction of polar analytes with acid-base properties by using separation membranes and buffer solutions, instead of organic solvents, as the acceptor solution.

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New approach on the alkylthiol determination in water byin situderivatization SPME followed by GC-ECD/NPD analysis

Cited by 7 publications

References 12 publications

Low Part per Trillion Determination of Reactive Alkanethiols in Wastewater by in Situ Derivatization-Solid-Phase Microextraction Followed by GC/MS

Low Part per Trillion Determination of Reactive Alkanethiols in Wastewater by in Situ Derivatization-Solid-Phase Microextraction Followed by GC/MS

Selective preconcentration of volatile mercaptans in small SPE cartridges: Quantitative determination of trace odor‐active polyfunctional mercaptans in wine

Strategies for the microextraction of polar organic contaminants in water samples

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