Acrylamide has been shown to cause cancer in animal studies. It has also been shown to cause nerve damage in people who have been exposed to very high levels at work. In April 2002 the Swedish National Food Authority reported the presence of elevated levels of acrylamide in certain types of food processed at high temperatures. Since then, acrylamide has been found in a range of cooked and heat-processed foods in many countries including the United States [1]. In order to assess acrylamide risk to humans, food levels need to be measured accurately. This prompts the need for development of analytical methods for acrylamide analysis. The US Food and Drug Administration has published an LC/MS/MS method for acrylamide [2]. Due to the low molecular weight of acrylamide, GC/MS has also been used for its analysis [3, 4]. However, GC/MS requires time-consuming derivatization. Here, we describe a simple and rapid LC/Time-of-flight MS method with accurate mass measurement and “in-source CID” fragmentation for acrylamide analysis.