A hollow fiber-liquid phase microextraction coupled with gas chromatography method has been developed for the determination of carcinogenic nitrosodiethylamine and nitrosodipropylamine in several food samples. In this method, a small amount of toluene as the acceptor phase was introduced to fill-up the channel of a polypropylene hollow fiber using a microsyringe while the hollow fiber was immersed in an aqueous donor solution. After extraction, the acceptor phase was withdrawn and injected for gas chromatographic analysis. Parameters that affect the extraction efficiency were studied including the organic solvent, length of fiber, volume of acceptor and extraction time. The limits of detection for nitrosodiethylamine and nitrosodipropylamine were 330 µg L–1 and 20 µg L –1 respectively. This method was applied successfully for the determination of nitrosodiethylamine and nitrosodipropylamine in sausage, corned meat, fresh meat, and salted egg.