Archaeological and Anthropological Sciences
https://doi.org/10.1007/s12520-023-01771-y
(2023) 15:70
RESEARCH
Molecular evidence for new foodways in the early colonial Caribbean:
organic residue analysis at Isla de Mona, Puerto Rico
Lisa Briggs1 · Jago Cooper2 · Oliver E. Craig3 · Carl Heron4
María Mercedes Martínez Milantchi5 · Alice Samson6
· Alexandre Lucquin3
·
Received: 16 October 2022 / Accepted: 12 April 2023
© The Author(s) 2023
Abstract
Ceramic objects account for over 90% of the cultural material recovered from archaeological sites in the Caribbean. However,
little research has been conducted on molecular evidence for past food production from these same vessels. Forty ceramic
sherds from Isla de Mona have been analysed by GC–MS and GC-C-IRMS in order to address questions surrounding
foodways in the Greater Antilles prior to and post European arrival. We evaluate evidence for dietary changes to illuminate
aspects of cultural exchange between Indigenous populations and the first generations of Spanish colonists. Here, we show
that plant residues are found in a variety of pottery forms, with some evidence for non-ruminant and ruminant fats. The
dearth of marine biomarkers is curious given the volume of fish bones found in archaeological contexts on Isla de Mona and
may offer evidence for spit-roasting, pit-roasting, or the use of a ‘barbacoa’ to cook fish on the island. The ubiquity of plant
residues in a variety of pottery forms may relate to the large-scale cultivation and export of cassava (Manihot esculenta)
from the island. A Spanish olive jar revealed evidence of wine residues, which may constitute the earliest detection of wine
residues in pottery found in the Americas.
Keywords Organic residues · Colonial Caribbean · Pottery, Foodways · Diet · Wine
Introduction
This paper addresses the impact on foodways from the first
decades of interaction between the Indigenous peoples
of the Greater Antilles and European colonists. It is well
known that hunger and food shortages contributed to the
failure of the colonists’ first town at La Isabela. Following
* Lisa Briggs
briggs@cantab.net
1
Cranfield Forensic Institute, Cranfield University, College
Rd, Cranfield, Wharley End, Bedford MK43 0AL, UK
2
Sainsbury Centre, University of East Anglia,
Norfolk Rd, Norwich NR4 7TJ, UK
3
BioArCH, University of York, Environment Building,
Wentworth Way, Heslington YO10 5NG, York, UK
4
Scientific Research Department, The British Museum, Great
Russell Street, London WC1B 3DG, UK
5
Department of Africa, Oceania and Americas, The British
Museum, Great Russell Street, London WC1B 3DG, UK
6
University of Leicester, University Road, Leicester LE1 7RH,
UK
this disaster, arriving Europeans switched to an almost total
dependence on Indigenous food preparation and foodstuffs
revealing much about coloniser processes of adaptation and
extraction (e.g. Deagan and Cruxent 2002; Deagan 1995).
Less is understood about how and when diet and food subsistence strategies changed in later decades and in different
contexts such as under the encomienda system (the Spanish
system of forced labour). To better understand the dynamics
of early colonial encounter, we explore molecular evidence
for dietary changes detectable in ceramic artefacts from Isla
de Mona. Ceramics of Indigenous manufacture are analysed
alongside European ceramic vessels by gas chromatographymass spectrometry (GC–MS) and GC-combustion-isotope
ratio mass spectrometry (GC-C-IRMS) in order to investigate the local diet and food subsistence strategies on Isla
de Mona and how these changed during the early periods
of European colonial presence. This preliminary study will
establish the feasibility of future, large-scale investigations
into the organic residues present in Caribbean ceramic
assemblages. Our research builds on the first GC–MS
studies of ceramics from nearby Hispaniola conducted by
Vanderveen (Vanderveen 2007, 2006) and expands the
scope of such research by including GC-C-IRMS data,
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gradient analysis of the sherds, and an acid butylation
method designed to detect wine residues. Our fundamental
research questions include whether lipids survive in these
vessels, what these lipids can tell us about diet and food
subsistence strategies on Isla de Mona, and to what extent
lipids discovered in Indigenous vessels differ from those
discovered in European ceramics found on the same island.
Isla de Mona
Isla de Mona is a currently uninhabited island in the northern
Caribbean, part of the Puerto Rican archipelago. It is a 50
km2 flat-topped carbonate platform with 90-m cliffs sticking
out of the fast-flowing sea passage between Puerto Rico and
the Dominican Republic, with the island’s centre located at
18.0829° N, 67.8927° W (Fig. 1). Beaches on the south and
west coasts provide some anchorage within fringing coral
reefs which quickly drop off to depths of up to a thousand
metres. Despite being semi-arid at present, with poor soil
development, and no permanent sources of freshwater, it is
not known whether these adverse conditions were similar in
the past. It is known, however, that Isla de Mona attracted
people to it for over 5000 years, in keeping with early patterns of small island use by Indigenous people across the
archipelago (Keegan et al. 2008). As well as for the island’s
abundant seasonal marine and terrestrial resources, people
were drawn underground into its extensive cave systems.
Archaeological research has documented pre-Columbian and
early colonial Indigenous rock art throughout the caves, at
Archaeological and Anthropological Sciences
least two ballcourts in the island’s interior, and a village site
on the west coast (Dávila Dávila 2003; Lace 2013; Rouse
1952; Samson and Cooper 2015). In the sixteenth century,
the Spanish Crown established a royal encomienda or provisioning station on Mona, exploiting Indigenous labour to
supply food and textiles to its burgeoning mining industries
across the region (Samson et al. in press). In later centuries,
the island became a base for pirates and refugees and, much
later, guano miners in the nineteenth century.
Evidence for diet and foodways
in the pre‑Columbian Caribbean
Pottery accounts for around 90% of all pre-Columbian
artefacts (Keegan 2000, p. 135); however, the traditional
focus in archaeology has been on constructing typo-chronologies rather than what it can tell us about diet. Increasingly, scientific techniques are being applied to elucidate
this (Vanderveen 2007, 2006). To date, studies of diet in
the region have used stable isotope analysis of human bone
collagen (Pestle 2010, 2013; Pestle and Colvard 2012),
identification of starch grains through scanning electron
microscopy (Ciofalo et al. 2019, 2018; Pagán-Jiménez and
Mickleburgh 2022), and zooarchaeology through the identification of faunal remains (Keegan 2000; Rainey 1940).
We believe analysis of pottery contents through organic
residue analysis can provide information not obtainable
by these methods.
Fig. 1 Location of Isla de Mona, situated between modern-day Dominican Republic and Puerto Rico
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Stable isotope analysis of skeletal remains from Puerto
Rico has provided insights into shifts in diet in the Indigenous population over time. However, stable isotope analysis of human bone collagen can only illuminate the diet of
the specific individuals under study, relies on the successful
preservation and extraction of human bone collagen (which
can quickly degrade in tropical environments), and cannot
distinguish between the consumption of meat and dairy
products. Pottery, on the other hand, could provide information about productive and communal activities. GC–MS and
GC-C-IRMS analysis of pottery can offer a greater specificity by distinguishing between plant, dairy, marine, and
ruminant versus non-ruminant foodstuffs.
Analysis of starch grains by scanning electron microscopy indicates high levels of Indigenous manioc/cassava
consumption (Ciofalo et al. 2019, 2018; Pagán-Jiménez
and Carlson 2014); however, this analytical method can only
detect the remains of food products with a starchy, granular
structure. Analysis of the lipids trapped in pottery could help
to fill in the gaps left by this type of analysis.
Faunal remains provide important dietary information
on archaeological sites. For example, the site of Coralie on
the island of Grand Turk yielded abundant faunal remains,
and a subsistence shift from the large-scale consumption of
local land crabs to marine molluscs has seen more widely
across the region. This is concomitant with a change in pottery styles from the Saladoid style (c. 500 BCE to 600 CE)
to the Ostionoid style (c. 600–1500 CE) (Keegan 2000, p.
152). Froelich Rainey (1940) perceived this as evidence for
two distinct cultures: a ‘Crab Culture’ and a ‘Shell Culture’,
yet later research has shown these differences are paralleled
in other areas of material culture (Rodríguez-Ramos 2005).
This offers insight into the dynamic nature of food pathways
in the Caribbean, providing a clear illustration that the diet
of Indigenous populations did not remain static, but rather
evolved over time. Given the variety of diets prior to contact with Spanish colonists, our research seeks to understand
what further changes may have occurred in diet and culinary
practices after early interactions with Europeans.
In neighbouring regions, organic residue analysis by
GC–MS has produced significant findings: residue studies
of Native American ceramics from the Midwest, Mississippi River, and the American Bottom regions of continental
North America have revealed molecular evidence for varying levels of maize consumption (Reber and Evershed 2004),
thus contributing to our understanding of agriculture, dietary
practices, and culinary traditions. Two publications characterise the lipids recovered from Indigenous vessels from Hispaniola by GC–MS (Vanderveen 2007, 2006), and none have
been conducted on ceramics from Puerto Rico. Vanderveen
reported evidence for a variety of foodstuffs in the 55 sherds
recovered from seven archaeological sites on Hispaniola,
including ruminants, conifer products, and plant products
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(2006, pp. 121–156), yet without additional analysis by GCC-IRMS, it is difficult to pinpoint a precise source for the
lipids detected. While the Vanderveen studies provided an
important first step in the molecular analysis of Indigenous
pottery from the Greater Antilles, more work is needed in
this area.
At the pre-Columbian and colonial era site of Sardinera
on Isla de Mona, there is faunal evidence that can help us
infer aspects of diet. Our excavations of the sixteenth century
deposits recovered fish and marine molluscs as well as pig
bones (Sus scrofa domesticus). In earlier excavations, Rouse
(1952, p. 368) makes brief mention of native bird, crab, fish,
hutía, iguana, manatee, turtle, and molluscs amongst the
excavated food remains. He also tentatively identified cow
and another imported mammal in upper layers. Food remains
were the most abundant category in Dávila Dávila’s excavations at the same site (2003, p. 139); the majority of which
(60%) were marine molluscs in addition to fish and hutía,
with cow, goat, and pig in the top layer (0–20 cm) (2003, pp.
145–154). The floor of the nearby site of Cueva Campanita,
a collapsed dolina on the cliffs above Sardinera, was covered
in remains of marine molluscs and large mammal bones during our visit in 2016, and Dávila Dávila reported marine
molluscs and remains of cow, goat, and pig on the surface
during earlier surveys (2003, pp. 166–167). Although these
remains could be associated with the long use of this place
into more recent times, Indigenous and sixteenth-century
Spanish pottery is also abundant. In terms of the historic
evidence, Spanish accounts repeatedly emphasise the fertility and food abundance on the island including cassava,
beans, maize, peppers, fruit, and fish, turtles, crabs, and the
best-tasting iguana in the Americas (Cyclura cornuta stejnegeri) (Fernandez de Oviedo y Valdés, 1851, bk. XII, chap.
VII, p.394; book XVI, chap. I, p. 465; Las Casas 1875, p.
XCVIII, 68–69; Wadsworth 1973). Isla de Mona became
a centre for food production and a major exporter of cassava bread in the sixteenth century as one of three Spanish
Crown-controlled supply stations in Puerto Rico producing
food and bedding (hammocks) for pearl and gold-mining
industries (Samson et al. in press).
Materials and methods
Ceramic artefacts
Ceramic artefacts from two archaeological sites on the
island, Playa Sardinera and Cueva Campanita, are analysed
here to better understand what changes may have occurred
in dietary practices and food preparation at colonial sites.
Archaeological evidence suggests that occupation at these
sites ceased after 1560 CE. Forty ceramic artefacts were
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Table 1 Ceramic types analysed, time periods of deposition, number
of samples in each group, and percentage of the total (n = 40)
Category
Time Period
Total
pot
sherds
Chican-Ostionoid
Indigenous undecorated
Buren
European glazed
Olive jar
Green bacin
1300–1560
1300–1560
1300–1560
1494–1560
1494–1560
1494–1560
9
14
3
10
2
2
selected for analysis by GC–MS, consisting of 14 sherds of
Iberian origin, and 26 sherds of Indigenous origin (Table 1).
There are six broad ceramic types represented in this sample set (Table 1, Fig. 2). The 26 Indigenous sherds fall into
three groups: undecorated plain bowls and plates, decorated
bowls and plates of the Chican-Ostionoid series, and buren,
which are flat, ceramic griddles used for cooking a variety
of plants and other foods (Rouse 1992, p. 12). Two of the
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European sherds derive from ‘olive jars’, a large ceramic
amphora used to transport foodstuffs to the Americas on
board ships. While the term olive jar implies that these vessels contained either olives or olive oil, olive jars are likely
to have been multiuse vessels which contained a range of
other liquid commodities such as wine (Goggin 1960). This
supposition is investigated here. Other vessels of European
manufacture found at Isla de Mona and analysed here consist
of thick-walled open forms with an emerald-green glaze on
both the interior and exterior surface and have been identified as green bacin/green lebrillo, which are large (50-cm
diameter), rimmed platters. A number of imported sherds
are covered in a white or brown glaze. Of the 10 glazed
sherds of European manufacture, seven have a whitish/tan
coloured glaze and may belong to the ‘Columbia plain’
ceramic type, but this assignation is tentative due to the
small size of the sherds and poor preservation of the glaze.
The remaining three are of an unidentified European type
with a slightly browner shade of glaze than the other seven.
As the condition of the glazed ceramics is not sufficient for
a secure typological identification, these have been grouped
Fig. 2 Ceramic samples from the six categories of pottery analysed. 1 = Chican-Ostionoid (217), 2 = Indigenous undecorated (231), 3 = buren
(220), 4 = Spanish olive jar (175), 5 = European glazed (227), 6 = green bacin (229). Scale = 5 cm
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together as ‘European glazed’ and are listed as either European white-glaze or European brown-glaze throughout. The
original shape of the glazed vessels is not clear, but they
were most likely plates or shallow bowls (escudillas) given
the distance between the rim and the base (i.e. Fig. 2, sherd
5). The assemblage represents a mixture of individual and
communal food storage (olive jar), food preparation (bacin,
buren, bowls), and food consumption (plates, bowls) forms.
Although there is no historical record for European presence
on the island until 1508, the date ranges for European material in Table 1 reflect the possibility of indirect acquisition
through Indigenous networks.
The relatively small number of samples (26 Indigenous
and 14 European) allows us to draw preliminary interpretations from our GC–MS investigations which can be supplemented in the future in a larger study that incorporates a
greater number of ceramic samples.
residue analysis in archaeology, including the differentiation
between adipose and dairy fats (Evershed et al. 1997, 1994).
Based on the concentration of C16:0 (palmitic acid) and C18:0
(stearic acid) in the extracts, a subset of 25 ceramics were
selected for analysis by GC-C-IRMS. In order to assess the
presence or absence of biomarkers associated with marine
resources, the 25 samples selected for GC-C-IRMS were
also analysed by GC–MS in selected ion monitoring (SIM)
mode and using a temperature programme setup to better
detect and resolve the isoprenoid (i.e. 4,8,12-TMTD, pristanic and two natural diastereomers of phytanic acids) and
the ω-(o-alkylphenyl)alkanoic acids (thereafter referred to as
‘Aqua-SIM’)(Shoda et al. 2017). Detailed information on the
preparation of all samples is provided in the Supplementary
Information.
Analytical methods
Results
GC–MS methods
Lipid recovery rates were high overall, with all sherds
analysed in this study yielding above the minimum 5 ug/g
threshold for interpretable lipid profiles (Evershed 2008;
Heron et al. 1991). Indigenous undecorated vessel 183 had
the lowest concentration of lipids at 14 µg/g, and European
white glazed vessel had the highest at 259 µg/g; however,
both Indigenous and European vessels are amongst the
top three highest and lowest lipid concentrations. No clear
pattern has emerged in terms of lipid concentration and
vessel type.
There is little evidence for contamination in these samples, with two exceptions. The first is the presence of diethyltoluamide detected in sample 216. This compound, also
known as DEET, is the active ingredient in many insect
repellents and likely derives from post-excavation handling.
The second possible indication of contamination is the presence of even-numbered n-alkanes. The presence of even
numbered n-alkanes dominating over odd has been interpreted as contamination from petroleum products (Freeman
and Pancost 2014; Whelton et al. 2018) or possibly the result
of thermal alteration of organic matter present in the deposition environment (Bondetti et al. 2020; March et al. 2014;
Suryanarayan et al. 2021; Wang et al. 2017).
A wide variety of compounds were detected in the samples analysed. The most abundant are a broad range of free
fatty acids, including both saturated (FA) and unsaturated
(UFA), and of a wide range of carbon lengths from short
to long-chain fatty acids (LCFA) and very-long-chain fatty
acids (VLCFA). Additional compounds detected include
dicarboxylic acids (diacids), hydroxy fatty acids, phytosterols, fatty alcohols, and n-alkanes. Characteristic chromatograms for the six ceramic types analysed here are shown
in Fig. 3.
In an effort to detect a wide range of compounds, all sherds
were extracted at least twice with two different methods
of extraction. This included the acidified methanol extraction method which utilises methanol and sulphuric acid to
aggressively target lipids in low concentrations and by solvent extraction using dichloromethane and methanol (2:1)
designed to preserve larger molecules such as triacylglycerols. These were prepared and performed according to established protocols (Correa-Ascencio and Evershed 2014; Drieu
et al. 2021; Dudd and Evershed 1998; Stern et al. 2000). A
test was conducted on a subset of four sherds in order to
assess levels of environmental input into the ceramics. This
consisted of obtaining and separately extracted five successive layers from the interior of the four vessels to evaluate
qualitative/quantitative differences in the lipid extracted
according to a previously published protocol (Stern et al.
2000). In order to assess the presence of wine biomarkers, we
investigated a subset of seven samples with a third extraction
method using an acid butylation protocol designed to detect
tartaric acid and malic acid (Drieu et al. 2021; Garnier and
Valamoti 2016). Detailed information on the preparation of
all samples for GCMS analysis is provided in the Supplementary Information.
GC‑C‑IRMS methods
In addition to GC–MS analysis, 25 samples have been analysed by GC-C-IRMS. This technique, first introduced in
the 1990s, has made it possible to access stable isotope
information from individual biomarker molecules, making
further information available in the application of organic
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Fig. 3 Characteristic chromatograms for the six ceramic types analysed in this study consisting of Spanish olive jars, Chican-Ostionoid, Indigenous undecorated, green bacin, European glazed, and buren
Lipid profiles
Lipid biomarker analysis by GC–MS has shown the residues
from these vessels fall into at least four, and possibly more,
broad categories (Table 2). Identifying ‘lipid profiles’ allows
us to demonstrate overarching patterns amongst ceramic
samples, which demonstrate similar molecular results (e.g.
13
Dunne et al. 2022a, b). An example of each lipid profile is
shown in Fig. 4. A table detailing the main results found for
each individual sample, their pottery type, lipid profile, lipid
concentrations, and ẟ13C values found in the GC-C-IRMS
analysis are presented in Table 3.
The lipid profiles have been assigned in order of specificity (Table 2). Broadly, Lipid Profile 1 could be considered
Archaeological and Anthropological Sciences
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Table 2 Overview of lipid profiles detected by acidified methanol extraction, with main molecules and compound classes detected, origin of
ceramics, ceramic types in each lipid profile, and number of samples assigned to each group
Lipid profile
Main molecules
Origins
Vessel types in this profile
Interpretation
Number
of samples
assigned
1
C18, C16, LCFA (C14–C20),
VLCFA (C21–C32)
Indigenous and European
Plant and animal products
n = 12
2
C16, C18, High UFAs (C18:1, Indigenous and European
C16:1, C22:1)
Plant (possible Brassica)
and animal products
n = 10
3
C16, C18,odd-numbered
alkanes, diacids, hydroxy
fatty acids
C16, C18, diterpenoids
Chican-Ostionoid, green
bacin, white glazed,
undecorated, buren
Chican-Ostionoid, green
bacin, white glazed,
brown glazed, undecorated, buren
Chican-Ostionoid, green
bacin, brown glazed,
undecorated, buren
Olive jars
Plant products
n = 16
4
Indigenous and European
European
the most generic as the compounds found in this group are
present in a wide variety of foodstuffs. Lipid Profile 2 features unsaturated fatty acids in high abundance, including
erucic acid (C22:1). Lipid Profile 3 contains long-chain dicarboxylic fatty acids, hydroxy fatty acids, and odd-numbered
n-alkanes. Lipid Profile 4 contains a suite of diterpenoids,
with a clear source attributable to conifer products from the
Pinaceae family.
‘Lipid Profile 1’ is dominated by common fatty acids
found in virtually all foodstuffs: palmitic acid (C16:0) and
stearic acid (C18:0), with additional peaks assigned to a series
of long-chain fatty acids (LCFA) between 14 and 20 carbon
atoms, and very long-chain fatty acids (VLCFA) between
21 and 32 carbon atoms. Twelve out of the 40 sherds fall
into this category which accounts for 30% of the samples
analysed and includes both Indigenous and European sherds
(Table 3). While this profile could be indicative of degraded
animal fats (Dudd et al. 1998; Whelton et al. 2018), experimental analysis on modern animals fats and plant oils has
shown that with such ubiquitous compounds, it is difficult
to distinguish between lipids derived from animals and
those derived from plants (Steele et al. 2010). The VLCFA
observed in these samples is likely derived from plant waxes.
‘Lipid Profile 2’ contains multiple examples of unsaturated fatty acids (UFAs) in high levels: primarily oleic acid
(C18:1), palmitoleic acid (C16:1) and erucic acid (C22:1), with
some samples in this profile also containing margaroleic
acid (C17:1), linoleic acid (C18:2), and gadoleic acid (C20:1).
Oleic acid is also present in high abundance in these samples. Oleic acid accounts for between 56 and 86% of fresh
olive oil (Colombini and Modugno 2009, p. 7); however, this
UFA is also present in other fats and oils and is a constituent of modern hand creams and cosmetics (Whelton et al.
2021) and could be a sign of contamination. Some samples
in this category contain even-numbered n-alkanes (samples
Conifer products and wine
residues
n=2
216, 218, and 220), which may be indicative of contamination from petroleum products. Two of the samples in this
profile also contain phytosterols: European white-glazed
227 contains campesterol and sitosterol, while European
green bacin 229 contains sitosterol. Both of these phytosterols have an unambiguous origin in plants (Colombini
and Modugno 2009, p. 54). Vegetable oils contain a greater
amount of UFAs than animals fats and are therefore more
prone to oxidation and polymerisation (Colombini and
Modugno 2009, p. 100). As such, these results are somewhat
unexpected given the propensity for unsaturated fatty acids
to degrade in archaeological ceramics. The preservation of
higher concentration of UFAs in these samples may be due
to the relatively recent age of the samples (when compared
to ceramics commonly investigated by organic residue analysis) or a very high level of UFAs present in the pottery prior
to deposition. A third possibility is that these samples contained food products with high levels of antioxidants which
may have contributed to the preservation of UFAs. Erucic
acid (C22:1) is present in all samples of this group and has
been identified as an indicator of plants from the Brassica
family (Colombini and Modugno 2009, p. 7) although this
compound is also found in a much wider range of plants.
Nine of the 10 samples assigned to this group contain additional compounds indicative of plants, including diacids and
hydroxy fatty acids.
‘Lipid Profile 3’ comprises samples with either odd-numbered n-alkanes, long-chain dicarboxylic acids, 2-hydroxy
fatty acids, or in many cases a combination of these compounds. These three classes of compounds are diagnostic for
plant-derived foodstuffs. Plant sphingolipids, for example,
are mostly composed of 2-hydroxy fatty acids (Ukawa et al.
2022), and these compounds are widely present in the samples in Lipid Profile 3. Plant waxes such as Candelilla wax
are produced by leaves of various Euphorbia species which
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Fig. 4 Examples of Lipid Profiles 1–4 shown by chromatograms characteristic of each group
are native to the Americas and are present on Isla de Mona
today and contain a mixture of odd-numbered n-alkanes
with 29–31 carbon atoms (Colombini and Modugno 2009,
p. 99). Four samples in this category display such odd-numbered n-alkanes, all of Indigenous origin. The two classes
of fatty acids, dicarboxylic acids (also known as diacids),
and hydroxy fatty acids are common degradation products
of other foodstuffs, particularly plant-derived lipids. Diacids
can be formed through the uptake of oxygen at the double
bond sites on the carbon chain of unsaturated fatty acids
(Colombini and Modugno 2009, p. 308). Mono- and polyunsaturated fatty acids (present in plant oils and marine oils)
are particularly labile and prone to oxidation and thermal
alterations that can produce hydroxy, dihydroxy, dicarboxylic
13
fatty acids, and ⍵-(o-alkylphenyl)alkanoic acids (APAAs)
(Bondetti et al. 2020; Cramp and Evershed 2013; Whelton
et al. 2021). There is some overlap between ‘Lipid Profile 2’
and ‘Lipid Profile 3’ as 9 out of 10 samples in Lipid Profile 2
contain both high levels of unsaturated fatty acids and dicarboxylic acids and hydroxy fatty acids. Lipid Profile 3 lacks
the high levels of UFAs found in Lipid Profile 2; however,
this may be due to partial oxidation or thermal degradation
of the unsaturated fatty acids in question.
‘Lipid Profile 4’ comprises sherds with a suite of diterpenoids detected, in addition to the palmitic acid (C16:0), and
stearic acid (C18:0) present in every sample. Diterpenoids are
resinous compounds primarily found in conifers of the Pinaceae
family (Heron and Pollard 1988; Pollard and Heron 1996). The
Lipid concentration
ug/g
δ13C C16:0 δ13C C18:0 Δ13C(C18:0-C16:0) Lipid profile Assignation
LCFA (x) and/ or
diacids present (o)
175
176
177
178
179
180
181
182
183
184
185
200
201
209
210
211
212
213
214
215
216
217
218
219
220
221
222
223
224
225
226
227
228
229
Cueva Campanita
Cueva Campanita
Cueva Campanita
Playa Sardinera
Playa Sardinera
Playa Sardinera
Playa Sardinera
Playa Sardinera
Playa Sardinera
Playa Sardinera
Playa Sardinera
Playa Sardinera
Playa Sardinera
Playa Sardinera
Playa Sardinera
Playa Sardinera
Playa Sardinera
Playa Sardinera
Playa Sardinera
Playa Sardinera
Playa Sardinera
Playa Sardinera
Playa Sardinera
Playa Sardinera
Playa Sardinera
Playa Sardinera
Playa Sardinera
Playa Sardinera
Playa Sardinera
Playa Sardinera
Playa Sardinera
Playa Sardinera
Playa Sardinera
Playa Sardinera
Olive jar
Green bacin
Undecorated
Chican-Ostionoid
Undecorated
Chican-Ostionoid
Undecorated
Chican-Ostionoid
Undecorated
Undecorated
Olive jar
Chican-Ostionoid
Green basin
White glazed
Chican-Ostionoid
White glazed
White glazed
Chican-Ostionoid
Undecorated
Chican-Ostionoid
White glazed
Chican-Ostionoid
White glazed
Green basin
Buren
Chican-Ostionoid
Chican-Ostionoid
White glazed
Buren
White glazed
Brown glazed
White glazed
Undecorated
Green basin
27.73
15.27
136.15
44.63
53.77
22.70
29.53
14.27
14.13
28.97
30.94
214.35
73.68
27.90
56.78
134.63
67.33
36.54
42.40
46.05
37.27
64.84
259.27
63.07
45.18
30.22
34.43
31.87
24.51
43.29
29.81
50.80
21.95
34.98
-27.71
− 21.82
− 19.40
− 23.70
− 27.09
− 24.52
− 29.41
− 29.29
− 29.29
− 28.87
− 28.04
− 27.60
− 27.05
− 28.59
− 29.06
− 27.11
− 24.94
− 26.48
− 27.07
x
x
x
x
x
x
x
x
xo
x
x
x
x
x
x
xo
x
xo
x
xo
x
xo
xo
x
xo
xo
xo
x
xo
x
xo
x
xo
x
European
European
Indigenous
Indigenous
Indigenous
Indigenous
Indigenous
Indigenous
Indigenous
Indigenous
European
Indigenous
European
European
Indigenous
European
European
Indigenous
Indigenous
Indigenous
European
Indigenous
European
European
Indigenous
Indigenous
Indigenous
European
Indigenous
European
European
European
Indigenous
European
− 28.30
− 22.39
− 20.20
− 23.26
− 28.43
− 24.77
− 29.80
− 29.56
− 29.14
− 29.35
− 28.36
− 28.64
− 28.56
− 29.10
− 29.76
− 26.85
− 25.97
− 27.35
− 28.06
− 0.59
− 0.58
− 0.80
0.44
− 1.34
− 0.26
− 0.38
− 0.27
0.15
− 0.49
− 0.32
− 1.04
− 1.51
− 0.51
− 0.71
0.27
− 1.04
− 0.87
− 0.99
4
1
3
1
3
1
3
3
3
1
4
1
3
1
1
2
1
3
1
2
2
3
2
3
2
3
3
2
3
1
3
2
3
2
Wine and conifer products
Plant + degraded animal fats
Plant
Plant + degraded animal fats
Plant
Plant + degraded animal fats
Plant
Plant
Plant
Plant + degraded animal fats
Wine and conifer products
Plant + degraded animal fats
Plant
Plant + degraded animal fats
Plant + degraded animal fats
Plant (possible Brassica)
Plant + degraded animal fats
Plant
Plant + degraded animal fats
Plant (possible Brassica)
Plant (possible Brassica)
Plant
Plant (possible Brassica)
Plant
Plant (possible Brassica)
Plant
Plant
Plant (possible Brassica)
Plant
Plant + degraded animal fats
Plant
Plant (possible Brassica)
Plant
Plant (possible Brassica)
70
Ceramic type
Page 9 of 19
Site
(2023) 15:70
13
Sample number Origin
Archaeological and Anthropological Sciences
Table 3 Sample number, origin of sample (Indigenous of European), site on Isle de Mona, ceramic type, lipid concentration, ẟ13C and Δ13C, lipid profile, assignation, and the presence or
absence of LCFA and/or diacids.
Plant + degraded animal fats
Plant (possible Brassica)
Plant
Plant (possible Brassica)
Plant + degraded animal fats
Plant
1
2
3
2
1
3
− 1.58
− 0.23
− 1.86
− 0.69
− 28.18
− 30.04
− 27.83
− 30.17
− 26.60
− 29.81
− 25.97
− 29.47
24.94
22.53
71.51
44.08
35.30
32.69
Buren
Undecorated
Chican-Ostionoid
Undecorated
Undecorated
Undecorated
Playa Sardinera
Playa Sardinera
Playa Sardinera
Playa Sardinera
Playa Sardinera
Playa Sardinera
Indigenous
Indigenous
Indigenous
Indigenous
Indigenous
Indigenous
230
231
232
233
234
235
δ13C C16:0 δ13C C18:0 Δ13C(C18:0-C16:0) Lipid profile Assignation
Lipid concentration
ug/g
Ceramic type
Site
Sample number Origin
Table 3 (continued)
13
x
x
xo
xo
x
x
Page 10 of 19
LCFA (x) and/ or
diacids present (o)
70
Archaeological and Anthropological Sciences
(2023) 15:70
terpenoids detected consist of unaltered diterpenoids including
levopimaric acid and isopimaric acid, as well as diterpenoids
that have been oxidised or degraded including dehydroabietic
acid, 7-oxo-dehydroabietic acid, and finally the molecule retene
which is a heating marker which can be indicative of pitch and
tar production through the distillation of resinous woods (Connan and Nissenbaum 2003; Heron and Pollard 1988; Pollard
and Heron 1996). The two samples in this category are the only
two unglazed ‘olive jars’ included in this data set, indicating that
both vessels had a resinous lining derived from conifer products.
Acid butylation
A subset of seven samples was selected for extraction by acid
butylation/boron trifluoride. This method is designed to detect
fruit acids including tartaric acid and malic acid, two acids
found in grape-based products such as wine (Garnier and Valamoti 2016). Recent analysis of control samples has shown that
while a variety of fruits contain tartaric acid and malic acid, it
is only in ripened grape products, including wine, and tamarind that a minimum threshold of 35% tartaric acid to malic
acid is expressed (Drieu et al. 2021). We calculated the ratio
of tartaric acid to malic acid for the seven samples extracted
by this method, and results are presented in Fig. 5.
The results show that sample 175, a Spanish olive jar, contains levels of tartaric acid that indicate a past content of wine.
This result is consistent with the suite of diterpenoids also
found in this samples, as many wine vessels were lined with
conifer products in the past in order to more effectively seal
the permeable sides of the vessel and contribute antimicrobial
properties to the wine (Briggs et al. 2022; Drieu et al. 2021;
Heron and Pollard 1988; Pecci et al. 2017, 2013; Pollard and
Heron 1996). Tamarind products can also impart a similar
ratio of tartaric acid to malic acid in ceramic vessels (Drieu
et al. 2021, p. 5); however, tamarind was not present in this
region during this time period, having been transported to
Mexico and Central America for the first time later in the
sixteenth century by Spanish and Portuguese colonists from
tropical regions of Africa (Tamale et al. 1995).
Five additional samples (European white glazed 225,
European white glazed 227, European green bacin 229,
Indigenous undecorated 177, European white glazed 223)
yielded low levels of tartaric acid and a lower ratio of tartaric acid to malic acid, possibly indicating a past content
of another type of fruit. No tartaric acid was detected in the
Indigenous undecorated vessel 234.
Detection of biomarkers associated with aquatic
products
Further GC–MS analysis was undertaken on 25 of the 40
sherds included in this study in order to assess the presence
or absence of biomarkers indicative of marine or freshwater
Archaeological and Anthropological Sciences
(2023) 15:70
Page 11 of 19
70
Fig. 5 Ratio of tartaric acid to
malic acid found for seven samples selected for acid butylation.
Blue dotted line at 35% is the
minimum threshold for wine
products (Drieu et al., 2020)
fish resources. These biomarkers include isoprenoid fatty
acids and ⍵-(o-alkylphenyl)alkanoic acids (APAAs) with
a carbon chain > 20, which are formed through the heating of the polyunsaturated fatty acids (PUFAs) found in
marine resources (Bondetti et al. 2020; Cramp and Evershed
2014). APAAs with a carbon chain length of < 20 are created through the heating of foods that contain UFAs, such
as vegetable oils, and terrestrial adipose fats (Bondetti et al.
2021; Evershed 2008; Heron and Evershed 1993). In order to
further assess the presence of isoprenoid alkanoic acids, the
ratio of two naturally occurring diastereomers of phytanic
acid, 3S,7R,11R,15-phytanic acid (SRR) and 3R,7R,11R,15phytanic acid (RRR), were calculated, with a ratio of SRR%
over 75.5% indicative of aquatic oil (Lucquin et al. 2016;
Schröder and Vetter 2010; Shoda et al. 2017). While phytanic acid is found in both aquatic and ruminant animals, a
higher SRR/RRR ratio (SRR%) is characteristic of lipids
derived from aquatic organisms (Shoda et al. 2017, p. 169).
Six of the 25 samples analysed revealed an SRR% above
the 75.5% threshold for aquatic oils: five are of Indigenous
origin (samples 178, 184, 213, 229, and 233), and the sixth
is a sherd of European manufacture thought to belong to the
Colombian plain type (sample 216). The sherds of Indigenous origin include both decorated and undecorated vessels. Eleven of the 25 samples revealed traces of ⍵-(o-alkylphenyl)octadecanoic acid (APAA C18), yet none revealed
APAAs with a carbon chain length of < 20. We also determined whether or not APAAs with a carbon chain length
of < 20 would be detectible by these methods by establishing the limit of detectability and found that if present, these
larger chain length APAAs should be detected, meaning that
the APAA C18 detected was not based on random results or
machine noise. APAA C18 is readily created from the heating
of a wide variety of foodstuffs including vegetable oils and
terrestrial adipose tissues; this identification is of limited
diagnostic value in archaeological material (Bondetti et al.
2020, p. 595). Further information can be gathered by the
distribution of the APAA C18 isomers. Two samples have a
high E/H (< 4) consistent with a plant rather than aquatic
origin (Bondetti et al. 2020).
GC‑C‑IRMS
GC-C-IRMS analyses were carried out on 25 of the 40
sherds included in this study to determine the ẟ13C values for
the major fatty acids, C16:0 (palmitic acid) and C18:0 (stearic
acid), and assess the potential sources of the lipids extracted
through use of the Δ13C proxy. The ẟ13C values of palmitic
and stearic fatty acids reflect their dietary and biosynthetic
origin, which allows plant/non-ruminant, ruminant adipose
and ruminant dairy fats to be distinguished (Copley et al.
2003; Dunne et al. 2012). The stable carbon isotope data for
methyl stearate and methyl palmitate are shown in Fig. 6,
and the individual values found for each of the 25 analysed
samples were shown in Table 3.
As demonstrated in Fig. 6, most of the Isla de Mona
ceramics fall within a relatively tight cluster. Four samples
trend towards values associated with either C4 plants or
aquatic resources (from − 25.0 towards − 15.0); all four of
these data points are extracts of Indigenous sherds and are
circled in Fig. 6. The range between − 1.00 and 4.00 has
been interpreted as indicating plant products or non-ruminant fats (Dunne et al. 2022a, b, p. 267), − 1.00 to − 3.30
indicating ruminant adipose fats, and below − 3.30 indicating ruminant dairy fats (Mukherjee et al. 2008, p. 2068).
These values are based on reference samples from a number of regions including South Asia, Europe, and Egypt
(Dunne et al. 2012; Dunne et al. 2022a, b; Mukherjee et al.
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Archaeological and Anthropological Sciences
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Fig. 6 Top — scatter plot of
results from the 25 samples analysed by GC-C-IRMS, showing
C16:0 ẟ13C from the C18:0 ẟ13C.
Bottom — plot of Δ13C against
ẟ13C16:0 for the 25 ceramic samples from Isla de Mona selected
for GC-C-IRMS analysis.
Indigenous samples = diamonds.
European samples = squares.
Lipid profiles represented by
colour: Lipid Profile 1 = green,
Lipid Profile 2 = yellow, Lipid
Profile 3 = blue, Lipid Profile
4 = red. Six samples with SRR/
RRR ratio over 75.5%, a possible indication of the presence
of aquatic oils, are circled
2008; Steele et al. 2010; Suryanarayan et al. 2021). However, previous investigations using reference animal fats,
notably porcine fats, show some overlap in the ẟ13C values
of lipids for marine organisms and non-ruminant species
(Whelton et al. 2021, p. 6), making the interpretation of
these samples less clear.
The interpretation of GC-C-IRMS data in vessels that
show a clear plant contribution from their lipid profiles
is complicated by the fact that fatty acids which derive
from plant processing are likely to contribute carbon more
depleted in 13C and could therefore alter the δ13C values
of the C16:0 and C18:0 fatty acids. Plants that utilise the C4
photosynthetic pathway (such as maize or millet) are even
more depleted in carbon and thus fall further along the
13
range show in Fig. 6 which show the value of C4 plants
increases to the right of the graph. Most of the Isla de
Mona ceramics analysed here show a clear plant contribution in their molecular profiles. Therefore, according to
the ‘animal fat proxy’ which discusses how and why plant
products may alter isotopic values (Whelton et al. 2021),
we must interpret our GC-C-IRMS data with caution as
the plant signatures so clearly demonstrated in the GC–MS
data are likely to effect the isotopic values found in our
GC-C-IRMS analysis. However, given the lipid concentrations found in our samples and the GC–MS data which
suggests a plant origin, it could be argued that most of the
vessels were used to process plant or, possibly, a mixture
of animal fats and plant products.
Archaeological and Anthropological Sciences
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Discussion
Lipid preservation, vessel use, and reuse
A variety of compound classes have been identified in our
ceramic samples including saturated and unsaturated fatty
acids, dicarboxylic acids, hydroxy fatty acids, n-alkanes,
terpenoids, phytosterols, and some fatty alcohols. Several
of these compound classes, especially long-chain dicarboxylic acids, hydroxy acids, phytosterols, and terpenoids, either
originate in plants or represent the degradation products of
plant constituents. The similarity amongst these samples
tells us two important things: first it indicates that a variety
of ceramic forms contained plant-based products at some
point, suggesting culinary practices that made use of plantbased products in several different vessel types. Second, the
similarities amongst these samples suggest that the presence
of these molecules is unlikely to be a result of environmental
contamination, given the results of the gradient analysis test
performed on four sherds. The relative homogeneity of lipids
present could also indicate reuse of these vessels for a variety of foodstuffs throughout the lifespan of these ceramics.
Four ‘lipid profiles’ have been identified, and all apart
from Lipid Profile 1 indicate a clear plant contribution. Lipid
Profile 1 is not sufficiently diagnostic to provide a secure
answer as to what these vessels contained in the past. The
fatty acids C18:0 and C16:0 are ubiquitous across a wide range
of foodstuffs. LCFAs are also present in Lipid Profile 1, and
while the combination of these compounds in archaeological ceramics has been interpreted as evidence for degraded
animals fats (Dudd et al. 1998; Whelton et al. 2018), questions have been raised as to how specific this profile is and
whether or not plant oils can be distinguished clearly from
animals fats without additional diagnostic compounds present (Steele et al. 2010). Conversely, the VLCFAs present
in these samples are more likely to derive from plant waxes
than animal fats. Therefore, while there may have been a
contribution from degraded animals fats in this lipid profile,
there is also strong evidence for a plant contribution.
Lipid Profiles 2, 3, and 4 show abundant evidence for a
clear contribution from plant foodstuffs. The high levels of
the UFA oleic acid (C18:1) found in Lipid Profile 2 could be
either be derived from plant oils or could possibly be interpreted as a sign of contamination (Whelton et al. 2021), as
oleic acid is likely to rapidly break down in archaeological
contexts given the propensity for oxidisation and thermal degradation of this compound (Colombini and Modugno 2009).
Similarly, the smaller peaks of erucic acid (C22:1) could offer
evidence of plants from the Brassica family, or oils such as
rapeseed oil (Colombini and Modugno 2009), yet concerns
that this compound can be present as a laboratory contaminant
requires us to interpret it with caution. Some plants from the
Brassica family are native to Isla de Mona, including Cakile
Page 13 of 19
70
lanceolata and Lepidium virginicum (Britton 1915), so the
identification of erucic acid may indicate the cooking and consumption of these native plants. In addition, the 2-hydroxy
fatty acids and long-chain dicarboxylic acids found in Lipid
Profile 2 are further evidence for plant products, as 2-hydroxy
fatty acids are widely present in plant sphingolipids (Ukawa
et al. 2022), while mid- to long-chain dicarboxylic acids are
common oxidations product of erucic and oleic acids, both of
which are found in high abundance in plants (Colombini and
Modugno 2009, p. 8). This strengthens the interpretation of
oleic acid and erucic acid as being derived from the past vessel contents rather than contamination. This is also the case
for Lipid Profile 3, where odd-numbered n-alkanes add to the
evidence from the 2-hydroxy fatty acids and long-chain dicarboxylic acids that there is a plant contribution to the molecular
profile observed. Long-chain α,ω-dicarboxylic acids (diacids)
with a chain length of C16 to C26 are considered diagnostic for
suberin, a compound present in the outer part of underground
plants (Dunne et al. 2022a, b, p. 262). Diacids are especially
prevalent in Lipid Profiles 2 and 3, further attesting to the use
of these ceramics for plant processing and the likely consumption of underground plant organs such as tubers in the local
diet of Isla de Mona.
Results from the GC-C-IRMS indicate a possible contribution from a C4 plant in two samples of Indigenous pottery
(177 and 178). While there is some overlap between C4 and
marine signals, the lack of marine signals from the GC–MS
analysis suggests the processing of a C4 plant in these two
vessels. Maize is perhaps the best known and most widely
studied C4 plant grown by Indigenous populations in the
Americas, with both native and imported varieties playing
an important role in Caribbean diets including in Puerto Rico
(Pagán-Jiménez and Mickleburgh 2022). Maize was amongst
the many crops gown on Isla de Mona in addition to cassava,
beans, peppers, and fruit (Fernandez de Oviedo y Valdés,
1851, bk. XII, chap. VII, p.394; book XVI, chap. I, p. 465;
Las Casas 1875, p. XCVIII, 68–69; Wadsworth 1973). Maize
was an important agricultural product in the Americas, and
the detection of ẟ13C values consistent with C4 plants found
in ceramic vessel can provide further evidence for the consumption and preparation of maize in the Americas (Reber
and Evershed 2004). In addition, plants from the Amaranthus
genus also utilise the C4 photosynthetic pathway, and while
there are examples of Amaranthus native to every continent
except Antarctica, the majority are native to the Americas
(Waselkov et al. 2018). Wild forms of the Amaranthus genus
have been identified on archaeological sites in South America that date from between 5910 and 5270 BCE (Arreguez
et al. 2013), and recent archaeological evidence confirms
that domesticated forms of Amaranthus were consumed in
New Mexico as far back as the twelfth century CE (Turner
et al. 2021). Amaranthus is present on Isla de Mona (Britton
1915, p. 40), so it is possible that a species of Amaranthus
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Page 14 of 19
contributed part of the C4 plant signal identified in these pots,
in addition to the maize cultivated on the island.
The diterpenoids identified in the ceramics in Lipid Profile
4 have an unquestionable plant origin, as these compounds are
only synthesised by conifers, most likely from the Pinaceae
family. Conifers have not been identified in early studies of
vegetation on Isla de Mona (Britton 1915), which suggests
that these two vessels, both of the ‘olive jar’ ceramic type,
were lined with a resin, pitch/tar prior to their arrival on Isla
de Mona. While the term ‘olive jar’ appears to indicate a past
content of olives or olive oil, studies of Spanish shipping documents have shown that this vessel type was also used to transport wine, water, honey, beans, chickpeas, capers, almonds,
dates, pitch, and gun powder (Avery 1997, p. 89). Olive jar
175 contains levels of tartaric acid that indicate this vessel contained wine. This vessel was recovered from Cueva Campanita,
where sixteenth-century material culture including a small
bronze bell has been recorded and interpreted as evidence for
Indigenous Catholic practices (Dávila Dávila 2003, p. 167 and
Fig. 16). The archaeological context raises the intriguing possibility that this vessel contained wine used in religious rites.
Olive jar 175 is of a shape consistent with the ‘Early’ style of
olive jars as defined by Goggin, which were produced between
1500 and 1580 CE (1960; James 1988, p. 44). Given the age
of this olive jar, we suggest that the molecular evidence for
wine in this vessel would constitute the oldest wine residues
discovered in the Americas to date.
Comparison with faunal remains
Results from GC-C-IRMS indicate a past content that
includes plant products/non-ruminant adipose fats, with a
minority of samples falling within the range traditional associated with ruminant adipose tissues. There is also a possible
contribution from C4 plants in at least two samples of Indigenous pottery (177 and 178). The values obtained through this
analysis show a relatively tight cluster, with the only clear
differentiation being the two Indigenous vessels enriched in
C13. As there are no large ruminants native to the Greater
Antilles, ruminant values in Indigenous pots may indicate
that they used these exotic animals in their local cuisine. In
addition, faunal remains from sixteenth-century excavated
contexts in Isla de Mona include cow, pig, and goat. Mixtures of products, either by intentional mixing or reuse of pottery vessels, complicates the interpretation of GC-C-IRMS
results; a mixture of ruminant adipose fats and C3 plant products can produce ∆13C values similar to non-ruminant fats
(Hendy et al. 2018). In some instances, these values have
been demonstrated in ceramics where non-ruminant fats
were mixed with C4 plant products such as maize. Such a
mixture is certainly possible for these samples. Furthermore,
we would expect not only pig, but also manatee, turtle, and
iguana to fall within the ‘plant/non-ruminant adipose’ range
13
Archaeological and Anthropological Sciences
(2023) 15:70
yet would be less fatty than pig. The faunal remains of these
animals are widely present on Isla de Mona, so it remains a
possibility that relatively lipid-poor non-ruminants such as
these were processed in some of our samples. However, without reference material to test, it is difficult to establish what
∆13C values would be present in the tissues of these animals.
It should also be noted evidence for plant processing in
archaeological ceramics is difficult to detect, although several
studies have achieved this (Dunne et al. 2021, 2016; Dunne et al.
2022a, b). The reason for this is simple: the lipid concentration
of plant oils in edible plant material exists in relatively low proportions when compared to the lipid concentrations found in
fat-rich meats (Charters et al. 1997; Evershed 2008). This would
cause the signal from animal fats to ‘swamp’ the plant signal
in archaeological ceramics in which plant and animal products
had been mixed. This makes the possible identification of plant
processing noteworthy. Our abundant evidence for plant processing in the Isla de Mona ceramics appears to suggest that plant
products were frequently processed within these vessels.
There is ample evidence that fish were consumed at Isla de
Mona based on the numerous fish bones and marine mollusc
shells recovered from the site. However, there is only limited
evidence for aquatic biomarkers in either the Indigenous vessels or the European vessels. The identification of marine fats
is well established in Eurasian pottery assemblages (both using
lipid biomarker and compound-specific isotope analysis). Only
a handful of our 40 samples (n = 6) revealed evidence for aquatic
oils through GC–MS, and the isotope data either demonstrates
a C4 contribution or traces of aquatic oils. Given the limited
evidence for aquatic oils from GC–MS data, including the lack
of C20 APAAs, it appears that these vessels may not have been
used to process the fish consumed at the site. Rather fish may
have been cooked using a different preparation method. These
methods may have included spit roasting, pit roasting, or use of
a ‘barbeque’ which is derived from the original Indigenous word
‘barbacoa’ meaning a raised wooden grate on which to smoke
food above a fire. Lipids derived from marine-based foodstuffs
are often difficult to detect in archaeological pottery as they are
high in polyunsaturated fats, and unsaturated fatty acids rarely
survive in their unaltered state in archaeological ceramics as they
are particularly susceptible to oxidation during burial and during
the use of the vessel prior to deposition (Evershed et al. 1992).
The divergence between what residues we have detected in
the ceramics and the faunal remains that provide direct evidence for fish consumption are curious, but not without precedent. A recent study conducted on Mesolithic and Neolithic
pottery from a site located on the bank of the White Nile in
Sudan sought to understand a similar archaeological data set:
ample evidence for the consumption of fish was found at the
site, yet little to no evidence was found for aquatic biomarkers in the ceramics (Dunne et al. 2022a, b). The authors concluded that fish was likely cooked using a different method,
while the ceramics were specialised vessels used to prepare
Archaeological and Anthropological Sciences
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sedges, wild grasses, and leafy plants (Dunne et al. 2022a, b,
p. 255). Here, we see a similar phenomenon in that we have
detected abundant evidence for plant oils and residues in both
European and Indigenous vessels, yet very limited molecular
evidence for the many fish which were clearly consumed on
this island based on the many fish bones recovered during
archaeological excavations.
The GC-C-IRMS data appears to support the results we
obtained by GC–MS, in that most of our samples fall within
the region of plant/non-ruminant adipose fats found for the
Δ13C. The interpretation of our GC-C-IRMS data is hindered
by a lack of reference material for this region. The recovery
of manatee and turtle bones at Isla de Mona suggests that
these animals formed part of the diet. Yet, there is currently
insufficient data surrounding the isotope values of the lipids
found in the tissues of these animals. If we contrast this with
the known isotope values for ruminants, non-ruminants,
and dairy fats from Europe, the Middle East, and Africa, it
becomes apparent how much work is still required to gain a
clearer picture of foodways in the early colonial Caribbean.
Cassava production
There is abundant evidence of plant products found in the samples from Isla de Mona. The similarities in molecular profiles
across a majority of vessel forms raises the possibility of the
repurposing of local and imported wares to process plant foods.
Cassava (Manihot esculenta) is known to have been grown and
processed on Isla de Mona, and the intensification of particularly cassava bread production for export in the first half of the
sixteenth century may account for the presence of the plant
profiles. Cleaning and grating the tubers, removing the juices,
grinding the flour, and baking bread are a multi-stage process
requiring a range of tools, containers, and cooking wares.
Spanish colonists were incredibly reliant on local Indigenous foodstuffs, which had to be provided by law to labourers
and enslaved workers (Alegría, 1990, p. 121). The historically
documented intensification of cassava flour and cassava bread
production in the first half of the sixteenth century on Isla de
Mona may have required an expedient use of all available vessels by Indigenous labourers, including novel imported forms.
This marks a shift from traditional subsistence production to
a colonial export industry in which a variety of imported and
local vessels were given over to this task. So far archaeological
investigations have not revealed colonial-era locally produced
ceramics in forms specifically related to cassava processing,
and this is an avenue for future research. However, until unique
biomarkers for cassava can be determined chemically and identified in archaeological ceramics, we can only point to this as a
likely source of the plant signals detected in our samples. Future
research focus is directed to species specific correlations using
detailed reference collection materials gathered on island and
more targeted multi-method characterisation techniques.
Page 15 of 19
70
Conclusions
The excavations at Isla de Mona yielded ceramic artefacts
of both Indigenous and European manufacture from the
early colonial period providing us with a unique opportunity to explore the dietary and subsistence practices present
on an island at the heart of the Caribbean. This pilot study
has shown that ample lipids are preserved in both Indigenous
and European ceramics recovered from Isla de Mona. Notably, the divergence between the zooarchaeological evidence
from excavations on the island (which suggests an extensive
exploitation of marine resources) and the biomolecular evidence from our ceramic samples (which strongly indicates the
processing and cooking of plant-based foodstuffs) offers an
intriguing insight into the culinary practices on Isla de Mona.
Put simply, it appears there was more than one way to cook a
fish. While Eurasian pottery from colder climates has yielded
ample molecular evidence for the processing and cooking of
fish products, our research suggests that at Isla de Mona, fish
were prepared in another manner, such as on the ‘barbacoa’.
Numerous contemporary sources discuss the use of a ‘barbacoa’ to cook and smoke fish. As a ‘barbacoa’ was a large
raised wooden grate, the remains of this cooking apparatus are
unlikely to survive in the archaeological record, and the use of
a ‘barbacoa’ would help to explain the discrepancy between the
faunal evidence for fish consumption and the lack of marine
residues in these pots. The formation of APAAs requires not
only the presence of fish products in pots but requires that heat
be applied to the fish oils as they are prepared in the ceramic
vessel. In culinary traditions that favour a hot fish-stew over a
barbecued fish fillet, one is far more likely to detect APAAs in
ceramic vessels. In a scenario where fish were prepared on a
barbecue and perhaps even served in these very ceramic vessels, APAAs would be unlikely to form or be preserved within
the ceramic matrix of these vessels as heat would not have
been applied to the vessel while it contained fish. This offers
an interesting insight into culinary exchange on the island: it
appears traditional foodways were maintained even after an
influx of European colonialists arrived on the island with their
glazed ceramics and olive jars.
The lack of evidence for dairy products in our samples
further suggests that European colonialists quickly came
to adopt and rely on Indigenous culinary traditions. Even
though goat and cow bones have been found in archaeological contexts on the island, we see no evidence for dairy fats
in our samples. It seems more likely that these animals were
slaughtered for their meat, or if dairying activities did occur
on the island, the resulting products were not contained in the
selection of pots we have analysed here. While dairy products have long been a staple of European culinary traditions,
this does not appear to be the case on Isla de Mona if the 40
ceramics analysed here are representative of local culinary
practices. If dairying was absent at Isla de Mona, despite the
13
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Page 16 of 19
presence of goats and cows, this may offer further evidence
for the continuation of Indigenous culinary traditions in the
face of European colonialism and the importation of European ceramic vessels. In the future, a larger study incorporating a greater number of ceramics can help to provide a more
comprehensive assessment of this early interaction between
Indigenous and European subsistence strategies.
The molecular evidence suggests that rather than relying on
European-style fish stews and dairy products, the inhabitants
of Isla de Mona largely used their ceramic wares to process
plant-based food items. The detection of diacids, hydroxy
fatty acids, phytosterols, and diterpenoids are indicative of
either C3 or C4 plants, while two indigenous ceramics seem
to have contained plant products derived from an arid-adapted
C4 plant, such as maize or Amaranthus. Every class of ceramic
analysed yielded clear evidence for leafy green plant products,
except for the two Spanish olive jars included in this study.
The molecular evidence from two Spanish olive jars
included in this study suggests that some European culinary
traditions persisted. The detection of wine residues in olive
jar 175 is significant for two reasons: first, it is the earliest
molecular evidence for wine in the Americas yet detected,
and second, the discovery of Spanish olive jar 175 inside a
cave, near a bell thought to have been used in religious rites,
raises the intriguing possibility that imported wine was being
consumed on the island. Whether consumed by Europeans or
members of the Indigenous population, this is direct evidence
for the importation of European wine to a tiny island in the
Caribbean shortly after the arrival of Spanish colonialists.
These preliminary interpretations drawn from our small
sample set of 40 sherds have demonstrated the potential
for a full-scale study of Indigenous and European ceramics
from this region. With additional research on a larger assemblage, it will be possible to assess over-arching patterns in
diet and culinary practices on Isla de Mona in the period
directly following Spanish colonialism in the Caribbean.
Supplementary information The online version contains supplementary material available at https://doi.org/10.1007/s12520-023-01771-y.
Acknowledgements This work was made possible through collaboration with the Departamento de Recursos Naturales y Ambientales
de Puerto Rico (DRNA) and the Instituto de Cultura Puertorriqueña
(ICP), and we thank these entities for their assistance and support.
We wish to thank the Wellcome Trust for financial support (Grant
ref: 097365/Z/11/Z) and National Geographic Society for helping to
fund the excavations on Isla de Mona. We thank Anthony Simpson at
the British Museum for assistance with the figures in this article and
Francesco de Palmas at the British Museum for maintaining the analytical instruments. We thank Helen Talbot at the BioArCH laboratories
at the University of York for assistance in maintaining the analytical
instruments. We also thank the two anonymous peer reviewers whose
helpful suggestions and comments greatly improved this manuscript.
Author contribution LB conceived the research design, conducted data
analysis, investigated and interpreted data, wrote the main text of the
manuscript, reviewed and edited the manuscript, and prepared all figures
13
Archaeological and Anthropological Sciences
(2023) 15:70
and illustrations. JC conceived the research design, supplied samples for
analysis, and reviewed and edited the manuscript. OEC investigated and
interpreted data and reviewed and edited the manuscript. CH conceived
of research design, supervised investigation and interpretation of data,
and reviewed and edited the manuscript. AL conducted data analysis,
investigated and interpreted data, and reviewed and edited the manuscript. MM supplied excavation data and reviewed and edited the manuscript. AS conceived the research design, supplied samples for analysis,
wrote sections of main text of the manuscript, and reviewed and edited
the manuscript. All authors read and approved the final manuscript.
Funding This research was funded by the Wellcome Trust Grant ref:
097365/Z/11/Z.
Data availability For further information, go to—https://www.sprin
gernature.com/gp/authors/research-data-policy/data-availability-state
ments/12330880 All original scientific data from this research is available to all and can be accessed here: Link to access: https://docs.google.
com/spreadsheets/d/1MvVpBVpdrC0ZT5K1mbEfUr1hNC2gvSstYK
zZrmul26Q/edit?usp=sharing
Code availability Not applicable.
Declarations
Competing interests The authors declare no competing interests.
Ethics approval Not applicable.
Consent to participate Not applicable.
Consent for publication All authors consent for this work to be published.
Conflict of interest The authors declare no competing interests.
Open Access This article is licensed under a Creative Commons Attribution 4.0 International License, which permits use, sharing, adaptation, distribution and reproduction in any medium or format, as long
as you give appropriate credit to the original author(s) and the source,
provide a link to the Creative Commons licence, and indicate if changes
were made. The images or other third party material in this article are
included in the article's Creative Commons licence, unless indicated
otherwise in a credit line to the material. If material is not included in
the article's Creative Commons licence and your intended use is not
permitted by statutory regulation or exceeds the permitted use, you will
need to obtain permission directly from the copyright holder. To view a
copy of this licence, visit http://creativecommons.org/licenses/by/4.0/.
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