Abstract: The multifunctional riot control agent composed of 2-methyl-2-propanethiol, diethyl sulfide and 2-chlorobenzylidene malononitrile were analysed qualitatively by gas chromatography in hyphenation with mass spectrometry. Complete separation of the analytes was achieved and assoting of the chromatographic peaks was affirmed. 2-Methyl-2-propanethiol in multifunctional riot control agent was determined by gas chromatography using syringe dispensing method in preparation of gas standards. Linear relationship between values of peak height and mass concentration of 2-methyl-2-propanethiol was kept in the range of 5-1 000 μg·L^-1. Detection limit (3S/N) of 5 μg·L^-1 was found when 1 mL of the sample was introduced. Values of recovery obtained by standard addition method were in the range of 97.2%-105%. By replicate introduction of a same sample, RSD (n=6) was 3.2%.