Multicapillary columns (MCCs) for gas chromatography make it possible to perform high-speed analysis of the mixtures of gaseous and volatile substances at a relatively large amount of the loaded sample. The study was performed using PLOT MCCs for gas-solid chromatography (GSC) with different stationary phases (SP) based on alumina, silica and poly-(1-trimethylsilyl-1-propyne) (PTMSP) polymer as well as porous polymers divinylbenzene-styrene (DVB-St), divinylbenzene-vinylimidazole (DVB-VIm) and divinylbenzene-ethylene glycol dimethacrylate (DVB-EGD). These MCCs have the efficiency of 4000–10000 theoretical plates per meter (TP/m) and at a column length of 25–30 cm can separate within 10–20 s multicomponent mixtures of substances belonging to different classes of chemical compounds. The sample amount not overloading the column is 0.03–1 μg and depends on the features of a porous layer. Examples of separations on some of the studied columns are considered.