Elastomers are one of the raw materials involved in the production of the gum base for chewing gum manufacturing. Gum bases generally consist among others of an elastomer to improve base component compatibility, to modify elasticity and to softens the chewing [1]. Synthetic elastomers such as polyisobutylene, isobutylene-isoprene copolymers, styrene-butadiene copolymers, polyisoprene, and combinations thereof are typically used for gum base production. The current legislation on gum bases limits some residual monomers in raw materials [2] thus requiring their quantitation in quality control. The recognition of these compounds is easy but their quantitation is often complex because of the solid state and the “plasticity” of the elastomers. Several sample preparation and quantification methods of residual monomers and to qualify elastomers were tested in view of quality control analysis [3,4]. This method describe a validated HS-GC/MS method enabling to quantify isobutylene, isoprene and hexane in all investigated raw materials with a good intermediate precision depending on the elastomers, RSD% ranging between 0.49 and 20.88%, and with LOD and LOQ in the ppb range.