Determination of 1,4-dioxane in water samples using freeze-assisted liquid–liquid extraction and gas chromatography-mass spectrometry with select reaction monitoring

In this study, we developed an analytical method for the determination of 1,4-dioxane in aqueous solutions using freeze-assisted liquid–liquid extraction, also known as frozen microextraction, and gas chromatography with triple quadrupole mass spectrometry with select reaction monitoring. The method is capable of quantifying 1,4-dioxane across a broad range of concentrations (1-10 000 μg/L) relevant to contaminated sites, with an instrument detection limit and method detection limit experimentally verified as 2.1 and 2.2 μg/L, respectively. In contrast to methods with similar detection limits that require 50 to 500 mL volume of sample, our method uses only 200 μL of sample. The method presented here facilitates field and laboratory applications where small sample volumes and high precision are required and could be extended to other strongly water-soluble GC-amenable analytes.