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An inside needle capillary adsorption trap based on polypyrrole/hexagonally ordered mesoporous silica was fabricated and used to extract polycyclic aromatic hydrocarbons. Chemical polymerization was used for synthesizing polypyrrole/hexagonally ordered mesoporous silica. Polypyrrole/hexagonally ordered silica was analyzed by scanning electron microscopy and thermo gravimetric methods. The prepared nanoporous material was immobilized into a stainless steel needle to fabrication of the inside needle capillary adsorption trap device. The inside needle capillary adsorption trap device was applied for the extraction of some polycyclic aromatic hydrocarbons from aqueous samples in combination with gas chromatography-mass spectrometry. A simplex method was used for optimization of factors affecting the extraction efficiency of the method. The detection limits of the method under optimized conditions (extraction time of 15 min at 50 °C, sampling flow rate of 5 mLmin −1 , NaCl 12% w/v) were in the range of 0.001–0.005 ngmL −1 . The relative standard deviations at a concentration level of 1 ngmL −1  were between 3.2% and 10.1% ( n  = 4).

Hexagonal Ordered Mesoporous Silica-Coated by Polypyrrole as a Coating for Inside Needle Capillary Adsorption Trap of Polycyclic Aromatic Hydrocarbons