A headspace solid-phase microextraction method was developed for the preconcentration and extraction of methyl tert-butyl ether. An ionic-liquid-mediated multiwalled carbon nanotube–poly(dimethylsiloxane) hybrid coating, which was prepared by covalent functionalization ofmultiwalled carbon nanotubes with hydroxyl-terminated poly(dimethylsiloxane) using the sol–gel technique, was used as solid-phase microextraction adsorbent. This innovative fiber exhibited a highly porous surface structure, high thermal stability (at least 320C) and long lifespan (over 210 uses). Potential factors affecting the extraction efficiency were optimized. Under the optimum conditions, the method LOD (S/N = 3) was 0.007 ng/mL and the LOQ (S/N = 10) was 0.03 ng/mL. The calibration curve was linear in the range of 0.03–200 ng/mL. The RSDs for one fiber (repeatability, n = 5) at three different concentrations (0.05, 1, and 150 ng/mL) were 5.1, 4.2, and 4.6% and for the fibers obtained from different batches (reproducibility, n = 3) were 6.5, 5.9, and 6.3%, respectively. The developed method was successfully applied to the determination of methyl tert-butyl ether in different real water samples on three consecutive days. The relative recoveries for the spiked samples with 0.05, 1, and 150 ng/mL were between 94–104%.

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