A novel catalyst preparation for NO reduction by CH4 has been conducted using a glow discharge plasma treatment followed by calcinations thermally. Such plasma prepared Pt/NaZSM-5 catalyst exhibits a high dispersion of metal active species. A remarkable improvement in the activity and stability, compared to the catalysts prepared conventionally, has been achieved. Especially, an excellent low temperature activity over the plasma-treated Pt/NaZSM-5 catalyst has been obtained. For example, the conventional 0.1 wt% Pt/NaZSM-5 catalyst shows no activity at temperatures below 673 K, while at 673 K, the NO conversion to nitrogen reaches 61.3% over the plasma-treated 0.1 wt% Pt/NaZSM-5 catalyst. The initiated temperature for the plasma-treated 0.1 wt% Pt/NaZSM-5 catalyst can be as low as 548 K.