SnO2 doped MoO3 nanofibers were prepared by wet-chemical method. The nanofiber diameter is ranging from 20 to 100 nm and length of 2–8 μm. The response of SnO2 doped MoO3 nanofibers to CO gas is 2 times higher than MoO3. The chemisorption and the oxidation of CO on the nanofiber surfaces are vital to the sensing performance.