An efficient, rapid, and inexpensive method for extraction and clean-up of some selected volatile nitrosamines from frankfurter sausages was developed by using superheated water coupled with solid-phase extraction. Because a coextraction of lipid caused a serious problem during the extraction, a subsequent clean-up step using fat-selective Florisil adsorbent with 60% diethyl ether-dichloromethane was then necessary. Various factors affecting superheated water extraction, such as flow rate, extraction temperature, dynamic time, and static time were optimized by using a full factorial design with three replicates. The optimal extraction temperature was 140 degrees C with dynamic and static time of 10 and 5 min, respectively, and a flow rate of 1.0 mL/min. Separation and quantification of nitrosamines were carried out using GC-FID and GC-MS in selected ion monitoring mode. Direct application of this method to frankfurter samples allowed overall recoveries of N-nitrosamines in the range of 81-106% with < 10% RSD, and the detection limit of the coupling method ranged between 0.47-1.48 ng nitrosamines injected.