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The present study was conducted to synthesise a carbon nanotube/layered double hydroxide nanocomposite by an in situ growth route via electrostatic force. The fabricated carbon nanotube/layered double hydroxide nanocomposite was successful in deposition on a stainless-steel wire for the preparation of the solid-phase microextraction fibre. The produced fibers are enduring with high suitability being chemically and thermally stable capable of coupling to GC and GC/MS. The important extraction parameters including extraction temperature, extraction time, sample mass and added water were simultaneously optimised using an optimisation approach. I comparison to hydrodistillation (HD), headspace single drop micro-extraction) HS-SPME (is advantageous regarding little sample level, time-efficiency, convenience and low cost.