Journal
ANALYTICAL CHEMISTRY
Volume 77, Issue 18, Pages 6012-6018Publisher
AMER CHEMICAL SOC
DOI: 10.1021/ac050685r
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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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