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. 2022 Mar 3;41:108016. doi: 10.1016/j.dib.2022.108016

Contribution to Mediterranean medieval dietary studies: Stable carbon and nitrogen isotope data of marine and catadromous fish from Provence (9th–14th CE)

Leïa Mion a,⁎, Tatiana André b, Anne Mailloux b, Myriam Sternberg c, Arturo Morales Muniz d, Eufrasia Rosello-Izquierdo d, Laura Llorente Rodríguez d,e, Estelle Herrscher a
PMCID: PMC8914535  PMID: 35282181

Abstract

Whilst marine resources are one of the pillars of the Mediterranean diet, their mode of acquisition and subsequent consumption by medieval populations in southern France are still not well known. Throughout Europe, bioarchaeological techniques, however, are beginning to reveal hitherto unknown aspects of these practices both dating to the medieval period as well as other periods of history and prehistory. This study involved the stable isotope analysis of five marine and catadromous taxa from three medieval sites in Provence, France: "rue Frédéric Mistral" at Fos-sur-Mer, "le Château" at Hyères and "Couvent des Dominicaines - Parking/Collège Mignet" at Aix-en-Provence. In total, 127 specimens, including Anguilla anguilla, Dicentrarchus labrax, Sparus aurata, Diplodus sargus and Mugilidae were subjected to carbon and nitrogen stable isotope analysis. The study provides a crucial and unprecedented point of reference of the carbon and nitrogen isotopic variability of one of the main dietary resources in the Mediterranean world, fish.

Keywords: Paleodiet, Stable isotope, Medieval, Marine resources

Specifications Table

Subject Archaeology
Specific subject area Stable carbon and nitrogen isotopes analysis of bone collagen
Bioarchaeology
Type of data Table
Figure
How data were acquired Carbon (δ13C) and nitrogen (δ15N) stable isotope measurements were acquired via Elemental Analyser-Isotope Ratio-Mass Spectrometry (EA-IRMS), using a Europa Scientific 20–20 IRMS. Statistical tests were conducted using R version 4.0.4 (2021–02–15).
Data format Raw
Parameters for data collection Vertebrae from five taxa Anguilla anguilla (n = 53), Dicentrarchus labrax (n = 29), Sparus aurata (n = 4), Diplodus sargus (n = 7) and Mugilidae (n = 34) were sampled entirely for collagen extraction (total n = 127). Four samples did not provide enough material for EA-IRMS measurements. The remaining 123 samples were analysed by EA-IRMS at Iso-Analytical Limited (United Kingdom). One in five samples was measured in duplicate to check for analytical reliability when enough material was available (extracted weight >2 mg, n = 23).
Description of data collection Samples were ultrasonicated in MilliQ water for 15 min until clean. Collagen was then extracted following a modified ABA protocol [1].
0.13–1.1 mg of each extracted bone collagen sample were measured by EA-IRMS.
Data source location
 All sampled skeletal collections are kept in the LA3M UMR 7298, MMSH at Aix Marseille University, Aix-en-Provence, France. The collection comes from the medieval archaeological sites of “rue Frédéric Mistral” at Fos-sur-Mer, “le Château” at Hyères and “Couvent des Dominicaines - Parking/Collège Mignet” at Aix-en-Provence, Provence, France.
Data accessibility Repository: IsoArcH (www.isoarch.eu) [2]
Data identification number: 10.48530/isoarch.2021.012
Direct URL: https://doi.isoarch.eu/doi/2021.012
Data is available under the Creative Commons BY-NC-SA 4.0 license.
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Value of the Data

  • •

    This dataset can benefit archaeologists, anthropologists, and zooarchaeologists interested in palaeodietary reconstruction and past fish acquisition practices and palaeoecology.

  • •

    This dataset is useful to reconstruct the consumption and acquisition of marine resources by medieval communities of the Western Mediterranean Basin.

  • •

    The dataset provided can be used to explore the changes of those practices and their affiliated environments during medieval times.

  • •

    This dataset enlightens the interest and the necessity of building archaeologically documented datasets of the isotopic variability of this key dietary resource to better assess its importance in the Mediterranean diet through time.

1. Data Description

The data comprise of elemental and isotope values of 127 vertebrae of marine and catadromous fish specimens (53 Anguilla anguilla, 29 Dicentrarchus labrax, 4 Sparus aurata, 7 Diplodus sargus and 34 Mugilidae). This dataset is the result of a research project (Icht'Isomed2 https://www.univ-amu.fr/fr/public/icthisomed2) which combined an archaeo-ichthyological approach and an analysis of the carbon and nitrogen isotope values of 5 key fish species of three medieval archaeological sites in Provence, South of France. The objective is to reconstruct the environments used for foraging marine resources Table 1. present sample data by specimen, providing site, taxon and sampled bone of the specimens analysed, collagen extraction data (Initial weight of the prepared sample, amount of extracted collagen and associated yield), elemental values (carbon and nitrogen contents expressed in percentage, atomic C/N ratio) and carbon and nitrogen isotope values (δ13C and δ15N) using delta notation (δ) in per mil increments (‰).

Table 1.

Elemental and isotopic data (carbon and nitrogen) of the fish samples analysed with related skeletal and archaeological information. Abbreviations: FOS= “rue Frédéric Mistral”, Fos-sur-Mer, Bouches-du-Rhône, France, HYERES=“le Château”, Hyères, Var, France, AIX=“Couvent des Dominicaines – Parking/Collège Mignet”, Aix-en-Provence, Bouches-du-Rhône, France, VTC= caudal vertebra, VTPC= precaudal vertebra, VTT= thoracic vertebra, UND undetermined vertebra,*samples did not provid enough collagen for EA-IRMS analyses or do not met the minimum thresholds for carbon and nitrogen contents (%C>13% and%N > 5% [10]) or atomic C:N ratio (between 2.9 and 3.6 [11]).

LabCode Site Taxon Sampled bone Initial weight (mg) Extracted weight (mg) Yield (mg/g) Weight analysed (mg) Carbon content (%) Nitrogen content (%) C:N δ13C (‰) δ15N (‰)
AIX_F01 AIX Anguilla anguilla VTC 16.11 2.9 180.0 0.92 24.43 9.40 3.03 −9.98 10.64
AIX_F02 AIX Anguilla anguilla VTPC 18.66 3.4 182.2 1.02 16.22 5.63 3.36 −12.79 14.19
AIX_F03* AIX Anguilla anguilla VTPC 23.89 5.2 217.7 0.99 8.59 2.93 3.42 −11.81 10.66
Duplicate values 0.96 8.85 2.99 3.45 −11.81 10.82
AIX_F04 AIX Anguilla anguilla VTPC 11.11 2.2 198.0 0.71 26.61 10.11 3.07 −11.57 11.06
AIX_F05* AIX Anguilla anguilla VTPC 24.52 5.9 240.6 0.96 9.94 3.54 3.27 −11.05 10.98
AIX_F06 AIX Anguilla anguilla VTPC 16.37 3.0 183.2 1.02 30.51 11.75 3.03 −13.53 16.14
AIX_F07* AIX Anguilla anguilla VTPC 12.16 1.7 139.8 0.14 22.84 7.21 3.70 −15.12 14.23
AIX_F08 AIX Anguilla anguilla VTPC 12.26 2.4 195.8 0.56 23.15 9.22 2.93 −9.16 10.71
AIX_F09* AIX Anguilla anguilla UND 3.01 <1 >10
AIX_F10* AIX Mugilidae VTC 80.01 9.3 116.2 1.10 12.11 4.42 3.19 −11.99 9.10
AIX_F11* AIX Mugilidae VTC 52.76 7.0 132.7 0.97 12.77 4.58 3.25 −16.65 13.06
Duplicate values 1.00 12.75 4.54 3.28 −16.55 13.32
AIX_F12* AIX Mugilidae VTC 28.68 8.9 310.4 0.97 6.90 2.33 3.46 −14.77 13.98
Duplicate values 0.96 6.79 2.34 3.39 −14.55 13.90
FOS_F01 FOS Anguilla anguilla VTC 58.40 9.8 167.8 1.06 41.96 15.85 3.09 −10.62 14.15
Duplicate values 0.92 40.11 15.22 3.08 −10.56 14.10
FOS_F02 FOS Anguilla anguilla VTC 15.50 3.0 193.5 1.01 38.76 14.52 3.11 −11.39 16.99
FOS_F03 FOS Anguilla anguilla VTC 26.30 4.2 159.7 1.03 41.96 15.48 3.16 −25.94 9.47
FOS_F04 FOS Anguilla anguilla VTC 33.20 4.4 132.5 0.99 41.77 15.56 3.13 −26.26 10.65
FOS_F05 FOS Anguilla anguilla VTC 51.40 7.4 144.0 0.96 43.56 16.33 3.11 −21.69 9.84
FOS_F06 FOS Anguilla anguilla VTC 72.40 10.6 146.4 0.95 40.58 15.32 3.09 −20.77 11.66
FOS_F07 FOS Anguilla anguilla VTPC 47.60 6.5 136.6 1.00 41.12 15.52 3.09 −9.62 13.41
Duplicate values 1.02 41.57 15.59 3.11 −9.60 13.44
FOS_F08 FOS Anguilla anguilla VTPC 74.30 10.0 134.6 0.97 42.75 15.92 3.13 −9.94 13.48
FOS_F09 FOS Anguilla anguilla VTC 63.00 9.2 146.0 1.10 38.13 14.35 3.10 −9.80 12.99
FOS_F10 FOS Anguilla anguilla VTC 30.80 5.2 168.8 1.01 41.87 15.44 3.16 −9.54 13.24
FOS_F11 FOS Anguilla anguilla VTC 177.90 18.8 105.7 0.97 22.28 8.36 3.11 −21.79 9.07
FOS_F12 FOS Anguilla anguilla VTC 111.60 11.8 105.7 1.04 43.36 16.11 3.14 −9.93 17.32
Duplicate values 1.05 43.39 16.03 3.16 −9.88 17.33
FOS_F13 FOS Anguilla anguilla VTC 68.40 8.0 117.0 1.10 42.48 15.86 3.12 −9.09 16.04
FOS_F14 FOS Anguilla anguilla VTC 18.90 3.7 195.8 1.02 39.17 14.46 3.16 −9.65 12.36
FOS_F15 FOS Anguilla anguilla VTC 109.00 9.5 87.2 1.00 43.81 16.06 3.18 −20.52 10.64
FOS_F16 FOS Anguilla anguilla VTC 134.20 20.1 149.8 0.99 44.84 16.89 3.10 −10.68 15.97
FOS_F17 FOS Anguilla anguilla VTC 59.30 3.9 65.8 1.07 43.02 16.20 3.10 −10.86 15.85
Duplicate values 0.95 41.81 15.85 3.08 −10.82 15.90
FOS_F18 FOS Anguilla anguilla VTC 90.00 1.7 18.9 0.94 37.13 13.85 3.13 −27.74 9.95
FOS_F19 FOS Anguilla anguilla VTC 56.40 6.4 113.5 0.99 43.22 16.28 3.10 −9.10 11.99
FOS_F20 FOS Anguilla anguilla VTPC 12.86 14.8 115.1 0.98 42.39 16.07 3.08 −10.88 13.90
FOS_F21 FOS Anguilla anguilla VTPC 111.70 15.2 136.1 1.10 44.70 16.83 3.10 −19.58 11.25
FOS_F22 FOS Anguilla anguilla VTPC 49.10 6.3 128.3 1.07 44.32 16.58 3.12 −24.01 12.57
Duplicate values 1.04 43.19 16.12 3.13 −24.05 12.61
FOS_F23 FOS Anguilla anguilla VTPC 60.60 9.8 161.7 0.96 45.87 17.34 3.09 −11.22 11.93
FOS_F24 FOS Anguilla anguilla VTPC 66.50 0.7 10.5 0.54 32.47 12.36 3.07 −9.35 12.39
FOS_F25 FOS Dicentrarchus labrax VTPC 285.00 26.7 93.7 1.00 44.79 17.01 3.07 −9.72 11.54
FOS_F26 FOS Dicentrarchus labrax VTPC 243.90 26.5 108.7 1.10 46.06 17.35 3.10 −9.75 11.46
FOS_F27 FOS Dicentrarchus labrax VTPC 197.30 19.8 100.4 1.08 45.87 17.18 3.12 −9.80 11.45
FOS_F28 FOS Dicentrarchus labrax VTPC 111.80 8.1 72.5 0.95 44.25 16.15 3.20 −11.05 12.58
Duplicate values 0.98 44.56 16.19 3.21 −11.10 12.57
FOS_F29 FOS Dicentrarchus labrax VTPC 165.30 15.9 96.2 1.10 42.08 15.76 3.12 −8.78 11.32
FOS_F30 FOS Dicentrarchus labrax VTPC 239.30 17.1 71.5 0.96 45.09 17.08 3.08 −10.06 13.54
FOS_F31 FOS Dicentrarchus labrax VTC 161.40 26.1 161.7 1.05 49.45 18.48 3.12 −10.19 13.58
FOS_F32 FOS Dicentrarchus labrax VTPC 307.80 30.8 100.1 1.00 32.40 12.17 3.11 −10.75 10.15
FOS_F33 FOS Dicentrarchus labrax VTC 93.80 14.9 158.8 1.10 43.68 15.46 3.30 −11.03 12.39
Duplicate values 0.99 42.84 15.33 3.26 −10.97 12.42
FOS_F34 FOS Dicentrarchus labrax VTC 43.30 6.3 145.5 0.96 40.04 15.29 3.06 −11.67 11.28
FOS_F35 FOS Dicentrarchus labrax VTPC 275.50 26.9 97.6 1.06 42.87 15.37 3.25 −11.54 13.39
FOS_F36 FOS Dicentrarchus labrax VTPC 87.40 9.7 111.0 1.07 38.82 14.67 3.09 −8.74 13.87
FOS_F37 FOS Dicentrarchus labrax VTPC 113.00 11.2 99.1 0.91 41.36 15.43 3.13 −8.80 13.92
FOS_F38 FOS Dicentrarchus labrax VTC 111.60 9.4 84.2 1.00 41.99 15.58 3.14 −13.10 11.28
Duplicate values 1.05 42.07 15.63 3.14 −13.14 11.32
FOS_F39 FOS Dicentrarchus labrax VTC 290.20 36.1 124.4 1.04 35.42 13.14 3.15 −9.52 13.34
FOS_F40 FOS Dicentrarchus labrax VTC 122.60 15.1 123.2 1.00 41.99 15.92 3.08 −13.38 6.55
Duplicate values 0.96 42.93 16.36 3.06 −13.42 6.51
FOS_F41 FOS Dicentrarchus labrax VTC 254.70 32.1 126.0 1.01 43.62 16.54 3.08 −12.57 14.24
FOS_F42 FOS Dicentrarchus labrax VTC 74.10 10.8 145.7 0.91 41.61 15.80 3.07 −9.33 11.36
FOS_F43 FOS Dicentrarchus labrax VTC 200.60 13.1 65.3 0.95 40.94 15.29 3.12 −10.46 10.03
Duplicate values 0.98 39.92 15.09 3.09 −10.52 10.04
FOS_F44 FOS Dicentrarchus labrax VTPC 197.20 23.5 119.2 1.05 41.31 14.91 3.23 −10.49 13.56
FOS_F45 FOS Dicentrarchus labrax VTPC 204.70 9.3 45.4 0.99 39.41 14.25 3.23 −11.99 11.65
FOS_F46 FOS Dicentrarchus labrax VTC 286.60 28.8 100.5 0.91 40.60 15.34 3.09 −10.81 10.35
FOS_F47 FOS Dicentrarchus labrax VTC 132.70 17.3 130.4 0.93 43.43 16.23 3.12 −11.65 13.43
FOS_F48 FOS Dicentrarchus labrax VTC 199.40 24.0 120.4 0.93 41.95 15.82 3.09 −9.95 11.82
Duplicate values 0.95 40.82 15.53 3.07 −9.91 11.82
FOS_F49 FOS Diplodus sargus VTC 26.60 4.3 161.7 0.96 38.96 14.74 3.08 −6.80 9.68
FOS_F50 FOS Diplodus sargus VTC 32.20 4.4 136.6 0.99 39.54 14.85 3.11 −8.32 10.43
FOS_F51 FOS Diplodus sargus VTC 27.20 3.2 117.6 1.08 40.69 15.40 3.08 −7.65 7.83
FOS_F52 FOS Diplodus sargus VTPC 52.70 6.6 125.2 1.05 41.09 15.38 3.12 −6.84 8.82
FOS_F53 FOS Diplodus sargus VTPC 27.20 3.7 136.0 0.99 38.54 14.54 3.09 −9.44 12.56
FOS_F54 FOS Diplodus sargus VTPC 122.90 15.0 122.1 0.95 42.51 16.16 3.07 −6.59 9.15
FOS_F55 FOS Diplodus sargus VTC 38.50 7.3 189.6 1.10 30.08 11.43 3.07 −6.41 8.66
Duplicate values 0.98 30.87 11.72 3.07 −6.36 8.71
FOS_F56 FOS Mugilidae VTPC 311.50 21.7 69.7 0.91 40.85 15.14 3.15 −15.93 6.59
Duplicate values 1.01 42.15 15.57 3.16 −15.99 6.60
FOS_F57 FOS Mugilidae VTPC 247.40 20.8 84.1 1.08 42.07 15.63 3.14 −11.35 8.39
FOS_F58 FOS Mugilidae VTPC 179.90 17.5 97.3 1.07 43.86 16.55 3.09 −8.72 9.88
FOS_F59 FOS Mugilidae VTC 190.70 19.1 100.2 0.99 43.06 15.55 3.23 −5.87 7.90
FOS_F60 FOS Mugilidae VTC 190.10 13.4 70.5 1.00 41.91 15.70 3.11 −22.46 9.06
FOS_F61 FOS Mugilidae VTC 206.40 18.9 91.6 0.97 42.10 15.51 3.17 −12.96 12.82
Duplicate values 0.95 41.73 15.39 3.16 −12.94 12.84
FOS_F62 FOS Mugilidae VTC 353.70 27.5 77.7 1.05 41.96 15.36 3.19 −6.60 9.14
FOS_F63 FOS Mugilidae VTPC 196.80 19.0 96.5 1.08 43.78 16.54 3.09 −9.88 11.45
FOS_F64 FOS Mugilidae VTPC 197.40 11.0 55.7 1.03 39.07 14.60 3.12 −10.52 11.23
FOS_F65 FOS Mugilidae VTC 110.00 9.4 85.5 1.05 42.87 15.87 3.15 −19.19 12.99
FOS_F66 FOS Mugilidae VTPC 303.80 35.7 117.5 1.03 44.75 16.48 3.17 −13.64 9.56
Duplicate values 1.03 45.09 16.55 3.18 −13.58 9.55
FOS_F67 FOS Mugilidae VTPC 227.60 18.4 80.8 0.95 42.11 15.55 3.16 −12.55 12.69
FOS_F68 FOS Mugilidae VTPC 195.40 25.5 130.5 0.96 33.46 12.50 3.12 −6.54 9.18
FOS_F69 FOS Mugilidae VTPC 362.40 29.3 80.8 1.01 43.75 15.55 3.28 −6.01 7.85
FOS_F70 FOS Mugilidae VTPC 182.70 15.0 82.1 0.95 42.99 15.92 3.15 −6.45 9.01
FOS_F71 FOS Mugilidae VTC 84.10 9.8 116.5 1.05 42.08 14.80 3.32 −6.73 6.95
Duplicate values 0.99 42.94 15.47 3.24 −6.69 6.97
FOS_F72 FOS Mugilidae VTC 89.80 10.1 112.5 1.03 38.82 14.08 3.22 −6.97 6.99
FOS_F73 FOS Mugilidae VTC 162.40 9.3 57.3 0.93 39.50 14.61 3.15 −13.86 8.07
FOS_F74 FOS Mugilidae VTC 212.70 23.4 110.0 1.05 44.59 16.48 3.16 −10.29 11.02
FOS_F75 FOS Sparus aurata VTC 44.40 6.6 148.6 1.02 36.34 13.75 3.08 −6.59 8.78
FOS_F76 FOS Sparus aurata VTC 86.20 10.4 120.6 1.00 41.50 15.51 3.12 −12.00 14.50
Duplicate values 1.03 41.97 15.72 3.11 −12.10 14.52
FOS_F77 FOS Sparus aurata VTPC 277.40 35.1 126.5 0.97 39.83 15.14 3.07 −8.65 10.13
FOS_F78 FOS Sparus aurata VTC 164.20 14.1 85.9 1.10 43.48 16.13 3.14 −7.22 9.86
Hy_F01 HYERES Anguilla anguilla VTC 12.40 1.3 104.8 0.30 25.60 9.34 3.20 −15.43 8.02
Hy_F02 HYERES Anguilla anguilla VTC 10.20 2.4 235.3 0.97 34.63 12.92 3.13 −11.41 11.43
Hy_F03 HYERES Dicentrarchus labrax VTPC 33.80 7.1 210.1 0.97 15.53 5.72 3.17 −13.01 7.26
Duplicate values 1.09 15.12 5.46 3.23 −12.95 7.06
Hy_F04 HYERES Dicentrarchus labrax VTC 18.10 2.8 154.7 0.95 37.55 13.78 3.18 −12.82 7.13
Hy_F05 HYERES Dicentrarchus labrax VTC 18.90 2.7 142.9 0.93 35.22 12.76 3.22 −15.13 11.51
Hy_F06 HYERES Dicentrarchus labrax VTC 13.20 1.9 143.9 0.83 35.71 12.92 3.23 −12.96 6.00
Hy_F07 HYERES Mugilidae VTPC 22.40 5.2 232.1 1.03 21.85 8.04 3.17 −12.33 11.74
Duplicate values 0.98 22.15 8.09 3.20 −12.38 11.79
Hy_F08 HYERES Mugilidae VTC 12.10 1.8 148.8 0.98 36.91 13.32 3.23 −12.24 9.64
Hy_F09 HYERES Mugilidae VTPC 19.10 2.4 125.7 1.01 35.22 12.76 3.22 −12.53 6.98
Hy_F10 HYERES Mugilidae VTPC 45.30 4.1 90.5 1.09 40.07 14.90 3.14 −12.35 13.02
Hy_F11 HYERES Mugilidae VTPC 10.00 1.2 120.0 0.41 31.86 11.54 3.22 −12.68 6.90
Hy_F12* HYERES Mugilidae VTPC 25.70 5.1 198.4 1.10 8.03 2.57 3.65 −18.49 8.26
Duplicate values 1.03 7.45 2.42 3.60 −18.37 8.19
Hy_F13 HYERES Mugilidae VTC 19.30 2.6 134.7 1.09 37.43 13.85 3.15 −11.11 8.74
Hy_F14 HYERES Mugilidae VTPC 92.50 8.6 93.0 0.98 38.63 14.31 3.15 −14.60 14.90
Hy_F15 HYERES Anguilla anguilla VTC 7.80 1.3 166.7 0.49 34.66 12.47 3.24 −10.29 14.16
Hy_F16 HYERES Anguilla anguilla VTC 6.80 1.6 235.3 0.38 34.19 12.21 3.27 −18.34 10.10
Hy_F17 HYERES Anguilla anguilla VTPC 7.00 1.6 228.6 0.28 30.07 10.07 3.49 −12.61 12.85
Hy_F18 HYERES Anguilla anguilla VTT 7.50 2.2 293.3 0.57 36.35 12.79 3.32 −13.90 14.09
Hy_F19 HYERES Anguilla anguilla VTC 7.70 1.4 181.8 0.75 33.63 11.72 3.35 −13.31 13.94
Hy_F20 HYERES Anguilla anguilla VTC 5.50 1.4 254.5 0.24 28.01 9.48 3.45 −16.53 12.62
Hy_F21 HYERES Anguilla anguilla VTC 5.00 1.4 280.0 0.52 27.25 9.17 3.47 −13.64 12.14
Hy_F22 HYERES Dicentrarchus labrax VTC 6.80 1.6 235.3 0.66 31.52 11.41 3.22 −12.70 8.25
Hy_F23 HYERES Mugilidae VTPC 6.30 1.2 190.5 0.50 27.33 9.38 3.40 −12.87 8.70
Hy_F24 HYERES Mugilidae VTPC 6.10 1.1 180.3 0.36 28.47 10.00 3.32 −13.22 7.16
Hy_F25 HYERES Anguilla anguilla VTC 3.80 1.3 342.1 0.31 28.17 9.83 3.34 −15.61 13.98
Hy_F26 HYERES Anguilla anguilla VTC 4.10 1.2 292.7 0.24 29.56 9.86 3.50 −11.31 8.95
Hy_F27* HYERES Anguilla anguilla VTC 4.10 0.5 122.0 0.44 30.60 9.41 3.79 −13.59 11.68
Hy_F28* HYERES Anguilla anguilla VTC 3.00 <1 >10
Hy_F29 HYERES Anguilla anguilla VTC 3.50 0.5 142.9 0.30 26.39 9.15 3.37 −10.20 12.90
Hy_F30* HYERES Anguilla anguilla VTT 2.40 0.7 291.7 0.15 26.60 11.59 2.68 −14.06 6.33
Hy_F31* HYERES Anguilla anguilla VTC 20.00 <1 >10
Hy_F32* HYERES Anguilla anguilla VTC 7.00 <1 >10
Hy_F33* HYERES Anguilla anguilla VTC 5.10 1.0 196.1 0.14 28.71 9.07 3.69 −15.50 11.16
Hy_F34* HYERES Anguilla anguilla VTC 4.70 1.0 212.8 0.18 26.01 8.39 3.62 −13.87 11.85
Hy_F35* HYERES Anguilla anguilla VTC 4.30 1.0 232.6 0.15 18.89 5.60 3.94 −12.54 11.32
Hy_F36* HYERES Mugilidae VTPC 4.30 0.9 209.3 0.13 25.43 7.58 3.91 −14.04 7.03
Hy_F37* HYERES Mugilidae UND 3.10 0.7 225.8 0.16 22.23 6.58 3.94 −13.81 7.42
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The samples come from three sites located along the Mediterranean seashore of Provence in South-East France: “rue Frédéric Mistral” at Fos-sur-Mer (Bouches-du-Rhône, France), “le Château” at Hyères (Var, France) and “Couvent des Dominicaines - Parking/Collège Mignet” at Aix-en-Provence (Bouches-du-Rhône, France) (Fig. 1). The samples from “le Château” at Hyères come from a dump layer dated between the end of the 8th and the middle of the 10th century AD [3]. The ones from the " rue Frédéric Mistral" habitat site in Fos-sur-Mer are from occupation levels dated between the 10th and the end of the 14th centuries AD [4]. The samples from “Couvent des Dominicaines - Parking/Collège Mignet” at Aix-en-Provence originate from a deposit pit used for consumption wastes and dated from the early 14th century AD [5].

Fig. 1.

Fig 1

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Location of the three sites in southern France.

The quality of the extracted collagen was measured according to their collagen yield (higher than 10 mg/g [9]), their carbon and nitrogen contents (%C > 13% and%N > 5% [10]) and their atomic C:N ratio (between 2.9 and 3.6 [11]). All samples met the minimum thresholds for collagen yield but 4 did not yield enough material to allowed EA analysis. 9 samples had atomic C:N outside the accepted values and 5 more did not reach the minimum amount of carbon and nitrogen contents. In total 109 samples (86%) met the thresholds for collagen preservation. 50 of them (39%) have carbon and nitrogen contents in collagen higher than 30 and 11%, respectively and C:N ratio lower than 3.2, more restrictive criteria pointed out by van Klinken and Guiry & Szpak for very good collagen conservation [9,12]. There is no strong correlation between the isotopic signatures of the remaining 109 samples and their yield (Spearman tests, S = 262,024, p = 0.34 rho −0.09 for C; S = 210,146, p = 0.18 rho 0.13 for N), their atomic C:N (S = 310,344, p = 0.001 rho −0.29 for C; S = 264,148, p = 0.30 rho −0.10 for N), their carbon contents (S = 197,040, p = 0.06 rho 0.18 for C; S = 200,611, p = 0.08 rho 0.17 for N) and their nitrogen content (S = 199,024, p = 0.07 rho 0.17 for C; S = 194,772, p = 0.04 rho 0.19 for N). A significant alteration of the isotopic information for the remaining samples can therefore be ruled out [11]. In total, 109 samples are then exploitable for isotopic interpretation. Isotopic data of those samples are summarized by site and taxa in Table 2. A scatterplot of δ13C and δ15N data according to site and taxa is presented in Fig. 2.

Table 2.

Summary of the isotopic data (carbon and nitrogen) of the fish samples analysed by taxa and site.

δ13C (‰)
 δ15N (‰)
Site Datation Taxon n Min Max Mean±SD Min Max Mean±SD
Fos-sur-Mer rue Frédéric Mistral 10–14th Anguilla anguilla 24 −27.7 −9.1 −15.0 ± 6.7 9.1 17.3 12.8 ± 2.4
Dicentrarchus labrax 24 −13.4 −8.7 −10.6 ± 1.3 6.6 14.2 12.0 ± 1.7
Diplodus sargus 7 −9.4 −6.4 −7.4 ± 1.1 7.8 12.6 9.6 ± 1.5
Mugilidae 19 −22.5 −5.9 −10.9 ± 4.7 6.6 13.0 9.5 ± 2.0
Sparus aurata 4 −12.0 −6.6 −8.6 ± 2.4 8.8 14.5 10.8 ± 2.5
Hyères le Château 8–10th Anguilla anguilla 12 −18.3 −10.2 −13.5 ± 2.6 8.0 14.2 12.1 ± 2.1
Dicentrarchus labrax 5 −15.1 −12.7 −13.3 ± 1.0 6.0 11.5 8.0 ± 2.1
Mugilidae 9 −14.6 −11.1 −12.7 ± 0.9 6.9 14.9 9.8 ± 2.9
Aix-en-Provence Couvent des Dominicaines - Parking/Collège Mignet 14th Anguilla anguilla 5 −13.5 −9.2 −11.4 ± 1.8 10.6 16.1 12.5 ± 2.5
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Fig. 2.

Fig 2

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δ13C and δ15N values obtained from the fish remains analysed in this study. The data have been disaggregated according to species and site.

2. Experimental Design, Materials and Methods

Prior to the extraction of collagen, the collected bone remains were subjected to a standard procedure: codified taxonomic nominations and standardised measurements were carried out with the help of the referential collections of the LA3M and CCJ osteological platforms [6], [7], [8], [14], [15], [16], [17], [18]. Every vertebra sampled was then photographed using a 2D-3D digital microscope Hirox™.

Collagen extraction was performed at UMR 7269 LAMPEA (France), following a modified ABA method that acknowledges the fragility of the material [1]. Fish vertebrae were kept complete and first washed using successive bath of MilliQ water in an ultrasonic tank until the liquid remained clear. Samples were then demineralised at ca. 4 °C in 12 ml of either 0.1 M (samples weighing less than 100 mg) or 0.5 M HCl (samples weighing more than 100 mg) depending upon the weight of the sample. Solution was changed daily until bones were fully demineralised. Once demineralised, the samples were rinsed five times with MilliQ water. Demineralised bones were then placed in a 0.125 M NaOH solution at room temperature for successive 30 min sessions (until solution stopped changing colour). The samples were finally rinsed 5 times with MilliQ water and then gelatinised in a pH3 solution (10–3 M HCl) at 75°C for 48 h. The resultant soluble collagen was filtered with Ezee filters™, frozen, and subsequently freeze-dryed.

After being weighed into tin capsules (between 0.13 and 1.1 mg), collagen samples were analysed by EA-IRMS on a Europa Scientific Elemental analyser coupled with a Europa Scientific 20-20 continuous flow isotope ratio Mass Spectrometer at Iso-Analytical Limited (United Kingdom). The analysis was conducted in a batch process by which a reference is analysed followed by several samples and then another reference. One in five samples were measured in duplicate when enough material was available to check analytical reliability.

The reference material used for δ13C and δ15N analysis was IA-R068 (soy protein, δ13CV-PDB = −25.22 ‰, δ15NAIR = +0.99 ‰). IA-R068, IA-R038 (L-alanine, δ13CV-PDB = −24.99 ‰, δ15NAIR = −0.65 ‰), IA-R069 (tuna protein, δ13CV-PDB = −18.88 ‰, δ15NAIR = +11.60 ‰) and a mixture of IAEA-C7 (oxalic acid, δ13CV-PDB = -+14.48 ‰) and IA-R046 (ammonium sulphate, δ15NAIR = +22.04 ‰) were run as quality control check samples during analysis. IA-R068, IA-R038 and IA-R069 are calibrated against and traceable to IAEA-CH-6 (sucrose, δ13CV-PDB = −10.449 ‰) and IAEA-N-1 (ammonium sulphate, δ15NAIR = +0.40 ‰). IA-R046 is calibrated against and traceable to IAEA-N-1. IAEA-C7, IAEA-CH-6 and IAEA-N-1 are inter-laboratory comparison standards distributed by the International Atomic Energy Agency, Vienna (Austria).

Following recommendations by Szpak et al [13]., based on repeated measurements of calibration standards, check standards, and sample replicates, precision was determined to be ± 0.07 ‰, ± 0.06 ‰ and ± 0.06 ‰ for δ13C and δ15N, respectively. Based on the difference between the observed and known δ values of the check standards and the long-term standard deviations of these check standards, accuracy or systematic error was determined to be ± 0.17 and ± 0.12 for δ13C and δ15N, respectively. The total analytical uncertainties were estimated to be ± 0.17 for δ13C, ± 0.13 for δ15N.

Ethics Statement

Not applicable.

CRediT authorship contribution statement

Leïa Mion: Conceptualization, Formal analysis, Investigation, Methodology, Writing – original draft, Writing – review & editing. Tatiana André: Conceptualization, Data curation, Investigation, Writing – review & editing. Anne Mailloux: Conceptualization, Funding acquisition, Supervision, Writing – review & editing. Myriam Sternberg: Conceptualization, Funding acquisition, Supervision, Writing – review & editing. Arturo Morales Muniz: Conceptualization, Writing – review & editing. Eufrasia Rosello-Izquierdo: Conceptualization, Writing – review & editing. Laura Llorente Rodríguez: Writing – review & editing. Estelle Herrscher: Conceptualization, Funding acquisition, Methodology, Supervision, Writing – review & editing.

Declaration of Competing Interest

The authors declare that they have no known competing financial interests or personal relationships that have or could be perceived to have influenced the data reported in this article.

Acknowledgments

The project leading to this publication has received funding from Excellence Initiative of Aix-Marseille University - A*MIDEX, a French "Investissements d'Avenir" programme - Institute for Mediterranean Archaeology ARKAIA (AMX-19-IET-003-projet AMORCE 2020 Icht'IsoMed2). Ongoing research of A. Morales Muniz, E. Rosello-Izquierdo, L. Llorente Rodríguez, L. Mion and T. André is now being sponsored by Grant number: PID2020–118662GB-100 of the Spanish Ministry of Science and Innovation. We thank D. Ollivier, N. Nin, L. Nanthavongdouangsy, J.P. Lagrue and F. Marty for access to the archaeological collections. S. Chevallier and M. Farese for their help concerning the photographic record and collagen extraction. Finally, we thank the three anonymous reviewers for their suggestions and corrections.

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