A metal-organic framework/periodic mesoporous silica (MOF-5@SBA-15) hybrid material has been prepared by using SBA-15 as a matrix. The prepared MOF-5@SBA-15 hybrid material was then deposited on a stainless-steel wire to obtain the fiber for the solid-phase microextraction of phenolic compounds. Modifications in the metal-organic framework structure have proven to improve the extraction performance of MOF/SBA-15 hybrid materials, compared to pure MOF-5 and SBA-15. Optimum conditions include an extraction temperature of 75°C, a desorption temperature of 260°C, and a salt concentration of 20% w/v. The dynamic linear range and limit of detection range from 0.1-500 and from 0.01-3.12 ng/mL, respectively. The repeatability for one fiber (n = 3), expressed as relative standard deviation, is between 4.3 and 9.6%. The method offers the advantage of being simple to use, rapid, and low cost, the thermal stability of the fiber, and high relative recovery (compared to conventional methods) represent additional attractive features.

In this research, a carbon nanotube/layered double hydroxide nanocomposite was synthesized by an in situ growth route by electrostatic force. The prepared carbon nanotube/layered double hydroxide nanocomposite was successfully prepared and deposited on a stainless-steel wire for the fabrication of the solid-phase microextraction fiber. The fiber was evaluated for the extraction of phenolic compounds from water samples. Analytical merits of the method, under optimum conditions (extraction temperature: 75°C, extraction time: 30 min, desorption time: 2 min, desorption temperature 260°C, salt concentration: 10% w/v) are 0.01-300 ng/mL for the linear dynamic range and 0.005-0.08 for the limit of detection. In optimum conditions, the repeatability for one fiber (n = 3), expressed as relative standard deviation, was between 6.5 and 9.9% for the phenolic compounds.

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