Determination of Organophosphate Esters in Water Samples Using Gas Chromatography– Mass Spectrometry (GC–MS) and Magnetic Solid-Phase Extraction (SPE) Based on Multi-Walled Carbon Nanotubes (MWCNTs)

A method based on gas chromatography–mass spectrometry (GC–MS), coupled with magnetic solid-phase extraction (SPE) with multi-walled carbon-nanotube (MWCNT)-coated iron oxide (Fe3O4) as the adsorbent, was developed for analyzing four organophosphate esters in ambient water samples. The magnetic, MWCNT composites were prepared by hydrothermal synthesis and characterized with scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared (FT-IR) spectroscopy, and superconducting quantum interference device magnetometry (SQUID). The extraction and desorption conditions, such as adsorbent dosage, adsorption time, eluent type, and eluent volume, were studied. The adsorbent was used to extract analytes within 50 min. The limit of detection (LOD) was between 0.038–1 μg/L, and the limit of quantitation (LOQ) was between 0.10–3.59 μg/L. The method was applied to analyze organophosphate esters in environmental water samples. A 72.5–89.1% recovery was obtained by analyzing spiked samples with low-, medium-, and high-concentration analytes. The relative standard deviations (RSDs) were less than 10%. This method displayed better sensitivity and accuracy; therefore, it could be successfully used to detect organophosphate esters in environmental water samples.