This paper presents the development of a metal oxide semiconductor (MOS) sensor for the detection of volatile organic compounds (VOCs) which are of great importance in many applications involving either control of hazardous chemicals or noninvasive diagnosis. In this study, the sensor is fabricated based on tin dioxide (SnO2) and poly(ethylene oxide) (PEO) using electrospinning. The sensitivity of the proposed sensor is further improved by calcination and gold doping. The gold doping of composite nanofibers is achieved using sputtering, and the calcination is performed using a high-temperature oven. The performance of the sensor with different doping thicknesses and different calcination temperatures is investigated to identify the optimum fabrication parameters resulting in high sensitivity. The optimum calcination temperature and duration are found to be 350 °C and 4 h, respectively and the optimum thickness of the gold dopant is found to be 10 nm. The sensor with the optimum fabrication process is then embedded in a microchannel coated with several metallic and polymeric layers. The performance of the sensor is compared with that of a commercial sensor. The comparison is performed for methanol and a mixture of methanol and tetrahydrocannabinol (THC) which is the primary psychoactive constituent of cannabis. It is shown that the proposed sensor outperforms the commercial sensor when it is embedded inside the channel.