The transition to food production in Africa follows a different trajectory to that of the European Neolithic, where, rather than the adoption of farming, pastoralism became an established and widespread way of life, long before the domestication of plants. In the early 'Green ' Holocene, hunter-gatherers lived semi-sedentary lifestyles, becoming more mobile as drying conditions commenced. Domesticated cattle, sheep and goat appeared in north Africa by the middle Holocene and faunal remains and rock art suggests that cattle played a significant role in the lives and ideology of prehistoric people in Neolithic north Africa. However, to date, no direct evidence exists that prehistoric Holocene groups were exploiting secondary products. Furthermore, archaeological and archaeobotanical evidence from sites across Holocene north Africa suggests that the gathering and processing of wild plants was a significant component in the subsistence strategies of both the early hunter-gatherers and the later pastoralists in the region. This thesis reports the results of the first organic residue analyses, using lipid biomarker and stable isotope approaches, of ceramics originating from Holocene north Africa. The pottery constitutes some of the earliest, technologically advanced ceramics in the world and thus this research provides a unique opportunity to investigate diet and subsistence strategies for the human groups living in Holocene north Africa. Lipid extracts of 443 potsherds were · analysed by gas chromatography (GC), GC-mass spectrometry (GC-MS) and GC-combustion isotope ratio-MS. The pottery was sampled from archaeological sites in three distinct regions in north Africa, selected for their contrasting pastoral trajectories, with the aim of investigating the potential of organic residues analyses of preserved food residues to identify the spatiotemporal extent of the exploitation of domesticates for their dairy and carcass products, and also further elucidate diet and subsistence practices, particularly the exploitation of plants. The three areas included (1) Mediterranean north Africa including the Maghreb, (2) The Nile Valley and the adjacent dry hinterlands and (3) Saharan Africa from west of the Nile to West Africa. The exploitation of domesticates for their carcass and dairy products, in the 5th millennium BC, was identified for the first time based on the 813C and ~l3C values of preserved fatty acids using a new reference database for modern animal fats. These results also reveal that the animals giving rise to these fats subsisted on a wide range of different forages composed of C3 plants, varying combinations of C3 and C4, to diets comprising primarily C4 plants, suggesting that the ecosystems existing across the span of the early to middle Holocene in north Africa were extremely varied. This demonstrates that 8l3C values of lipids from ceramics provide a valuable environmental proxy, through vegetation driven signatures (C3 versus C4), and thus can be used to determine spatiotemporal variations in vegetation and humidity. The remarkable preservation of diagnostic plant lipid biomarkers, notably long-chain fatty acids (C20 to C2S) and n-alkanes (C23 to C33) in organic residues from sites in the Libyan Sahara and at Kadero, Sudan, has enabled identification of the earliest processing of plants in ceramic vessels. Carbon number distributions and 8l3C values indicate that in the Libyan Sahara, vessels were likely used to process edible water plants, wild cereals and emergent macrophytes. These signals persist in residues from the Early Acacus to the Middle Pastoral, suggesting that aquatic plants were exploited by both hunter-gatherers and mobile pastoralists. High frequencies of organic residues dominated by palmitic acid, and low in stearic acid, also suggest the processing of oil seeds in the vessels.