SUPPLEMENTARY INFORMATION

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1 In the format provided by the authors and unedited. SUPPLEMENTARY INFORMATION VOLUME: 3 ARTICLE NUMBER: Earliest direct evidence of plant processing in prehistoric Saharan pottery Julie Dunne a, Anna Maria Mercuri b, Richard P. Evershed a, Silvia Bruni c and Savino di Lernia d,e a Organic Geochemistry Unit, School of Chemistry, University of Bristol, Cantock s Close, Bristol BS8 1TS, UK b Laboratorio di Palinologia e Paleobotanica, Dipartimento di Scienze della Vita, Università degli Studi di Modena e Reggio Emilia, Viale Caduti in Guerra 127, Modena, Italy c Dipartimento di Chimica, Università degli Studi di Milano, Via C. Golgi 19, Milano, Italy d Dipartimento di Scienze dell Antichità, Sapienza, Università di Roma, Via dei Volsci, Roma, Italy e School of Geography, Archaeology & Environmental Sciences, University of the Witwatersrand, Johannesburg, Private Bag 3, Wits 2050, South Africa NATURE PLANTS DOI: /nplants

2 Supplementary Table 1 Archaeological phase, P/S ratios, n-alkane lipid distributions, stable carbon isotope values, CPI, ACL, weighted mean and Paq values from trimethylsilylated TLEs of potsherds from Takarkori rock shelter and Uan Afuda cave, Tadrart Acacus, Libyan Sahara. The maxima for the n-alkane distributions are highlighted in bold. Sample no. Archaeological period Palmitic/ Stearic ratio C 23 Lipid distribution - abundance Stable carbon isotope values (δ 13 C) C 25 C 27 C 29 C 31 C 33 C 23 C 25 C 27 C 29 C 31 C 33 CPI C23-C33 ACL C23-C33 Weighted mean δ 13 C P aq TAK4 Late Acacus n/d n/d n/d n/d TAK14 Middle Pastoral 1.98 n/d n/d n/d n/d TAK23 Late Acacus 2.56 n/d n/d n/d TAK24 Early Pastoral 5.38 n/d n/d n/d TAK82 Middle Pastoral 2.82 n/d n/d n/d n/d TAK135 Middle Pastoral n/d n/d n/d n/d TAK159 Middle Pastoral n/d n/d n/d n/d TAK479 Middle Pastoral n/d n/d n/d n/d TAK709 Middle Pastoral 2.47 n/d n/d n/d n/d n/d n/d n/d TAK730 Middle Pastoral 4.80 n/d n/d n/d n/d TAK766 Middle Pastoral n/d n/d n/d TAK860 Middle Pastoral 4.00 n/d n/d n/d n/d TAK873 Middle Pastoral 1.98 n/d n/d n/d TAK953 Middle Pastoral n/d n/d n/d TAK1008 Middle Pastoral 2.46 n/d n/d n/d n/d n/d n/d n/d TAK1054 Middle Pastoral n/d n/d n/d TAK1072 Middle Pastoral n/d n/d TAK1531 Middle Pastoral 4.00 n/d n/d n/d n/d UAF A1 Late Acacus 3.67 n/d n/d n/d n/d UAFA3 Late Acacus 3.70 n/d n/d n/d n/d n/d n/d n/d n/d n/d 27.3 n/d 0.89 UAF20 Late Acacus 1.50 n/d n/d n/d n/d UAF45 Late Acacus n/d n/d n/d n/d n/d n/d n/d 26.0 n/d 0.75 UAF46 Late Acacus 4.66 n/d n/d n/d n/d n/d n/d n/d UAF50 Late Acacus 4.23 n/d n/d n/d n/d n/d n/d n/d 26.3 n/d n/d UAF84 Late Acacus n/d n/d n/d n/d n/d n/d n/d 26.9 n/d n/d n/d - not determined, signal intensity too low Late Acacus period years uncalibrated years BP, calbc Early Pastoral years uncalibrated years BP, calbc Middle Pastoral years uncalibrated years BP, calbc 12,13 P/S ratio - relative abundance ratio C16:0/C18:0 fatty acids, values greater than 4 indicate a plant origin CPI - measures the relative abundance of odd over even carbon chain lengths, e.g. CPI values for all plant species have strong odd-chain preferences, with CPI values varying between 1.6 and ACL - weight-averaged number of carbon atoms of the higher plant C25 - C33 s 16 P aq - emergent and non-emergent aquatic macrophyte input, P aq <0.1 corresponds to a terrestrial plant input, P aq to emergent macrophytes and P aq to submerged or floating macrophytes 18 NATURE PLANTS DOI: /nplants

3 Supplementary Table 2 Archaeological phase, lipid concentration (µg g-1), total lipid in extract (µg) and δ 13 C16:0 values from trimethylsilylated TLEs of potsherds from Takarkori rock shelter and Uan Afuda cave, Tadrart Acacus, Libyan Sahara. Lipid concentration (µg g -1 ) Total lipid in extract (µg) δ 13 C 16:0 Sample no. Archaeological period UAFA1 Late Acacus UAFA2 Late Acacus UAFA3 Late Acacus UAF20 Late Acacus UAF39 Late Acacus UAF45 Late Acacus UAF46 Late Acacus UAF47 Late Acacus UAF48 Late Acacus UAF50 Late Acacus UAF84 Late Acacus UAF85 Late Acacus UAF102 Late Acacus UAF127 Late Acacus UAF153 Late Acacus UAF158 Late Acacus UAF168 Late Acacus UAF169 Late Acacus TAK4 Late Acacus TAK5 Late Acacus TAK23 Late Acacus TAK33 Late Acacus TAK13 Early Pastoral TAK24 Early Pastoral TAK2 Middle Pastoral TAK7 Middle Pastoral TAK12 Middle Pastoral TAK14 Middle Pastoral TAK17 Middle Pastoral TAK38 Middle Pastoral TAK42 Middle Pastoral TAK47 Middle Pastoral TAK82 Middle Pastoral TAK128 Middle Pastoral TAK135 Middle Pastoral TAK159 Middle Pastoral TAK188 Middle Pastoral TAK475 Middle Pastoral TAK479 Middle Pastoral TAK709 Middle Pastoral TAK730 Middle Pastoral NATURE PLANTS DOI: /nplants

4 TAK732 Middle Pastoral TAK766 Middle Pastoral TAK813 Middle Pastoral TAK860 Middle Pastoral TAK873 Middle Pastoral TAK897 Middle Pastoral TAK927 Middle Pastoral TAK939 Middle Pastoral TAK953 Middle Pastoral TAK989 Middle Pastoral TAK1008 Middle Pastoral TAK1054 Middle Pastoral TAK1058 Middle Pastoral TAK1072 Middle Pastoral TAK1531 Middle Pastoral NATURE PLANTS DOI: /nplants

5 Supplementary Figure 1 Map of the Tadrart Acacus massif (SW Libya) with location of studied sites, Takarkori rock shelter and Uan Afuda cave ( The Archaeological Mission in the Sahara, Sapienza University of Rome) NATURE PLANTS DOI: /nplants

6 Supplementary Figure 2 (a) view of the cave of Uan Afuda, central Tadrart Acacus (SW Libya), (b) the site stratigraphy consists of Late Pleistocene reddish aeolian sands at the base and the later Early Holocene sequence comprises brownish sediments rich in organic matter, (c) close view of structures including fireplaces from Late Acacus layers, radiocarbon dated to 7500 calbc. ( The Archaeological Mission in the Sahara, Sapienza University of Rome) NATURE PLANTS DOI: /nplants

7 Supplementary Figure 3 (a) view of Takarkori rock shelter, southern Tadrart Acacus (SW Libya), (b) Middle Pastoral layers during excavation, (c) detail of plants remains and Barbary sheep coprolites from Late Acacus 2 stone structure, radiocarbon dated to ca calbc ( The Archaeological Mission in the Sahara, Sapienza University of Rome) NATURE PLANTS DOI: /nplants

8 Supplementary Figure 4 Analysed potsherds from Uan Afuda cave. These originate from Late Acacus hunter-gatherer occupation levels, dated between approximately 8300 and 7300 calbc ( The Archaeological Mission in the Sahara, Sapienza University of Rome) NATURE PLANTS DOI: /nplants

9 Supplementary Figure 5 Analysed potsherds from Takarkori rock shelter grouped by archaeological phases from Late Acacus to Late Pastoral periods ( calbc). ( The Archaeological Mission in the Sahara, Sapienza University of Rome) NATURE PLANTS DOI: /nplants

10 Supplementary Figure 6 The pollen diagrams from the two archaeological sites (top: Uan Afuda; bottom: Takarkori), showing selected taxa. Pollen records demonstrate that wet environments with hygrophilous trees (Tamarix, Ficus), limno-telmatophytes (Typha, Juncus cf.) and aquatics (Lemna, Potamogeton) were locally spread in the Tadrart Acacus Mountains, in the Central Sahara, during the Early and Middle Holocene. Meanwhile, desert communities with Acacia and Cheno-Amaranthaceae were less spread than in the current dry phase. High values of Poaceae pollen and Artemisia are evidence of human transport (and use) of plants into these cave (top) and rock shelter (bottom) sites 6 NATURE PLANTS DOI: /nplants

11 Equation 1 Paq ratio 18 This formula is used to determine the extent of aquatic plant input to lake sediments through expressing the relative proportion of mid-chain length (C23, C25) to long-chain (C29, C31) n- alkane homologues 18. A Paq<0.1 corresponds to a terrestrial plant input, Paq to emergent macrophytes and Paq to submerged or floating macrophytes. P aaaa = (C 23 + C 25 )/(C 23 + C 25 + C 29 + C 31 ) NATURE PLANTS DOI: /nplants

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