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Gas chromatography (GC) is regarded as an essential separation method for the analysis of volatile compounds, and a wide variety of polymeric liquid-phases have been developed as the stationary phase. 1,2 Various deactivation and polymer-coating processes have been also proposed for the preparation of GC columns with good separation performance and stability. [3][4][5][6] In contrast to the successful applications and subsequent commercialization of these polymer-coated columns, such as wall-coated, support-coated and pellicular-coated, the reports for the fibrous polymer-packed stationary phases, however, have been limited, except for characterizing the surface of the fibers in inverse GC (IGC). 7,8 In general, the surface characteristics of the fiber have been analyzed with IGC technique by injecting the standard samples into a fiber-packed column and measuring the elution behavior. This characterization method is based on the observation of the specific interactions between the surface of the fibers and the standard solutes injected as the probes. Consequently, it is quite natural that a synthetic fiber can be employed as a separation medium in GC, if the fiber possesses both the thermal stability for the operation at an elevated temperature and the resistance to the gaseous chemical species through the column during the separation.In terms of the use of fibrous stationary phase in liquid phase separation methods, several applications have been reported. Kiso et al. introduced fibrous cellulose acetate (CA) stationary phase for the separation of alcohols 9 and polycyclic aromatic hydrocarbons (PAHs) 10 in microcolumn LC, and Jinno et al.reported the application of CA phase in capillary electrochromatography (CEC). 11,12 Recently, the possibility of the several synthetic fibers as the stationary phase in CEC 13 was also demonstrated. Although the separation efficiency of those columns was still not comparable with those of conventional particle-packed columns such as octadecylsilica (ODS) phase, and moreover, there were several limitations on the mobile phase composition and the packing density, still it has been clearly shown that the packed filaments could play the role as a stationary phase. Saito et al. have also reported the successful applications of fibrous polymeric material as an extraction medium for novel miniaturized sample preparations specially designed for the on-line coupling to microcolumn liquid phase separation methods. 14-22 On the basis of the above successful applications of fibrous materials as the stationary phase and the extraction medium, fiber-packed fused-silica capillaries have been introduced in our previous study for the separation of volatile compounds in GC. 23In this work, polymer coating onto the packed-filaments in a capillary was investigated using several conventional polymeric materials as the liquid-phase for capillary GC columns. As the fibrous material, Zylon ® [poly(p-phenylene-2,6-benzobisoxazole)] fiber ( Fig. 1) was employed, taking into account the heat resistance...