High performance liquid chromatography with mass spectrometry (HPLC-MS) is a powerful method for characterising modern fats and oils at the molecular level (triacylglycerols). It is a technique that should have great potential for the analysis of archaeological fatty residues. However, its archaeological potential has yet to be systematically evaluated. This paper presents the results of an HPLC-MS study of food residues adsorbed into archaeological ceramics. Experimentally three classes of materials were studied: raw plant and animal foods likely to be available to the prehistoric population of Anatolia (Turkey), the same foods after cooking and archaeological residues from Late Bronze and Early Iron Age (ca 1500–900 BCE) contexts from ceramics excavated at the site of Gordion, Central Turkey. Modern foods were used as a baseline; modern cooked residues provided a measure of the effects of cooking on the same fatty residues. These datasets were then compared to the HPLC-MS results for the archaeological residues. The study found that HPLC-MS does offer important new information, but does not provide a 'magic bullet'. Like established techniques using gas chromatography and mass spectrometry, it is best used in tandem with other techniques in a multi-stranded approach to archaeological residue characterisation and identification.