In the paper the method of producing of complex nanopowder materials and barrier structures on their basis by means of pulse laser reactive evaporation of metal targets is offered. It enables to effectively produce nanopowders with mean geometrical diameter up to 5-10 nm and specific surface more than 80-190 m2/g at productivity up to 50 g/h. The carried out researches of photoluminescent properties of nanopowder materials ZnO and TiO2 (after laser anneling including) with the purpose of studying the opportunity of creation on their base a gas sensor. The influence of adsorption of molecular gases O2, H2, N2, and CO on change of intensity of photoluminescence of nanopowder ZnO is investigated. On the basis of the carried out researchers the method for detection, recognition and estimation of gas concentration in the analyzed enviroment is proposed. With the purpose of increasing the selectivity of the method it is offered to analyze the radical-recombination luminescence, which spectral characteristics are determined by the given superficial condition of granules of nanopowder and chemical structure of the analyzed gas.