Three dimensionally honeycomb layered double hydroxides framework as a novel fiber coating for headspace solid-phase microextraction of phenolic compounds

• The three dimensionally honeycomb layered double hydroxides material was used for fabrication of the solid-phase microextraction (SPME) fiber.
• The fiber was evaluated for the extraction of phenolic compounds.
• Different parameters affecting the extraction efficiency were optimized.
• The SPME fiber was applied in polluted river water and water samples.

A new solid phase microextraction (SPME) fiber based on high-temperature three dimensionally honeycomb layered double hydroxide (TDH-LDH) material is presented. The fiber coating can be prepared easily, it is mechanically stable and exhibits relatively high thermal stability. This study shows that three dimensionally honeycomb layered double hydroxide generated porous morphology. The TDH-LDH material was tested for the extraction of some phenolic and polycyclic aromatic hydrocarbon compounds from aqueous sample solutions in combination with gas chromatography–mass spectrometry (GC–MS). The TDH-LDH fiber contains polar groups and its efficiency for non-polar polycyclic aromatic hydrocarbon compounds was lower than phenolic compounds. On the other hand, a high tendency towards the adsorption of polar phenolic compounds was observed for the proposed fiber. The effects of the extraction and desorption parameters including extraction temperature, extraction time, ionic strength, stirring rate, pH and desorption temperature and time have been studied. In optimum conditions, the repeatability for one fiber (n = 5), expressed as relative standard deviation (R.S.D. %), was between 2.8% and 7.1% for the phenolic compounds. The detection limits for the studied phenolic compounds were between 0.02 and 5.8 ng mL−1. The developed method offers the advantage of being simple to use, with shorter analysis time, lower cost of equipment, thermal stability of fiber and high relative recovery in comparison to conventional methods of analysis