Combined headspace single-drop microextraction and solid-phase microextraction for the determination of phenols as their methyl ethers by gas chromatography-mass spectrometry?

Analytical Methods Pub Date: 2017-10-30 DOI: 10.1039/C7AY02275A

Abstract

Combined SDME and SPME worked as an elegant strategy to inject a large sampled mass of analytes into a GC. After headspace SDME of methyl derivatives of phenol, chlorophenols, methylphenols and other substituted phenols into 10 μL of solvent drop (1-butanol), the extract was subjected to headspace SPME (DVB/CAR/PDMS, 30/50 μm, fiber) for convenient transfer of analytes to the fiber and then into the GC. This combination resulted in achieving a high sensitivity of detection for a small volume (0.5–2 mL) of sample. The chromatographic separation of thirteen model phenols (as their methyl ethers) was complete within 10 min. A rectilinear calibration graph was obtained using combined headspace SDME/SPME and GC-MS in the range of 0.001–5 mg L?1, with a correlation coefficient of 0.990–0.999 and an average limit of detection of 20 ng L?1 (range 8–45 ng L?1), which was far better than that obtained by headspace SDME, 90 ng L?1 (range 50–138 ng L?1), or headspace SPME, 55 ng L?1 (range 36–70 ng L?1), when used alone. In spiking experiments on environmental water samples, the RSD of the results was in the range of 4.6–9.4%.

Graphical abstract: Combined headspace single-drop microextraction and solid-phase microextraction for the determination of phenols as their methyl ethers by gas chromatography-mass spectrometry
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