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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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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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Publication details

The article was received on 23 Sep 2017, accepted on 27 Oct 2017 and first published on 30 Oct 2017


Article type: Paper
DOI: 10.1039/C7AY02275A
Citation: Anal. Methods, 2017, Advance Article
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    Combined headspace single-drop microextraction and solid-phase microextraction for the determination of phenols as their methyl ethers by gas chromatography-mass spectrometry

    A. Jain, S. Soni, K. Reddy-Noone, A. K. K. V. Pillai and K. K. Verma, Anal. Methods, 2017, Advance Article , DOI: 10.1039/C7AY02275A

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