Absorbed Residue Evidence for Prehistoric Datura Use in the American Southeast and Western Mexico

Abstract

Absorbed residue studies have been used in subsistence research for decades. Only more recently have the chemical methods employed been used to explore the consumption of ritual concoctions such as those including cacao, yaupon holly, and alcohol. In this article we use mass spectrometry to identify Datura residues in prehistoric contexts from western Mexico and the American Southeast. Datura is a genus of flowering plants that contain hallucinogenic alkaloids. Their use in both regions is known historically and still continues today. This study sampled 55 pottery vessels and 18 shell vessels using both a traditional burr method and a water-based sonicator sampling method. Datura residues were found in 13 pottery vessels and 14 shell vessels using both sampling approaches. These results demonstrate that it is possible to identify Datura residue in pottery and shell vessels and that the use of Datura extends back into prehistory in both regions. The form and decoration of pottery vessels with Datura residues show correlations with specific motifs and themes. Historically, shell vessels were used in the Southeast for the consumption of another ritual beverage, called the Black Drink. The presence of Datura shows that those vessels were used for other kinds of beverages as well.

Full text

Absorbed Residue Evidence
for Prehistoric Datura Use in
the American Southeast and
Western Mexico
Adam King, Terry G. Powis, Kong F. Cheong, Bobi Deere, Robert B. Pickering,
Eric Singleton, and Nilesh W. Gaikwad
Scholars have been studying absorbed residues for
many years looking for evidence of ancient food-
related cultural practices (Barnard and Eerkens 2007;
Evershed et al. 1990; Evershed et al. 1992). This is
ABSTRACT
Absorbed residue studies have been used in subsistence research for decades. Only more recently have the chemical methods employed
been used to explore the consumption of ritual concoctions such as those including cacao, yaupon holly, and alcohol. In this article we
use mass spectrometry to identify Datura residues in prehistoric contexts from western Mexico and the American Southeast. Datura is a
genus of flowering plants that contain hallucinogenic alkaloids. Their use in both regions is known historically and still continues today.
This study sampled 55 pottery vessels and 18 shell vessels using both a traditional burr method and a water-based sonicator sampling
method. Datura residues were found in 13 pottery vessels and 14 shell vessels using both sampling approaches. These results
demonstrate that it is possible to identify Datura residue in pottery and shell vessels and that the use of Datura extends back into
prehistory in both regions. The form and decoration of pottery vessels with Datura residues show correlations with specific motifs and
themes. Historically, shell vessels were used in the Southeast for the consumption of another ritual beverage, called the Black Drink. The
presence of Datura shows that those vessels were used for other kinds of beverages as well.
Los estudios de residuos absorbidos han sido utilizado en la investigación de la subsistencia durante décadas. Sólo más recientemente
se han utilizado los métodos químicos empleados en estos estudios para explorar el consumo de brebajes rituales tales como los que
incluyen cacao, acebo de Yaupon, y alcohol. En este trabajo se utiliza la espectrometría de masas para identificar los residuos de Datura
en contextos prehistóricos del oeste de México y el sureste de Estados Unidos. Datura es un género de plantas florecientes que contiene
alcaloides alucinógenos. Su uso en ambas regiones es documentado históricamente y continúa en el presente. Para este estudio se
analizaron muestras de 55 vasijas de cerámica y 18 vasijas de concha utilizando tanto el método tradicional de rebaba como el método
de muestreo en baño de sonicación con agua. Residuos de Datura fueron encontrados en 13 vasijas de cerámica y 14 vasijas de concha
utilizando los dos sistemas de muestreo. Estos resultados demuestran que es posible identificar los residuos de Datura en vasijas de
cerámica y concha y que el uso de Datura se remonta a la prehistoria en ambas regiones. La forma y decoración de las vasijas de
cerámica con restos de Datura muestran correlaciones con motivos y temas específicos. Históricamente, se utilizaron vasijas de concha
en el Sureste para el consumo de otra bebida ritual, llamada la Bebida Negra. La presencia de Datura muestra que las vasijas se utilizaron
también para otras bebidas.
especially the case in the archaeological search for
evidence of subsistence changes associated with
the origins of agriculture, seasonal variation, or envi-
ronmental shifts (for example, Copley et al. 2003;
Advances in Archaeological Practice 6(4), 2018, pp. 312–327
Copyright 2018 © Society for American Archaeology
DOI:10.1017/aap.2018.30
312

Absorbed Residue Evidence for Prehistoric Datura Use in the American Southeast and Western Mexico
Dudd et al. 1999; Reber and Evershed 2004). More
recently, absorbed residues have become a tool in
identifying the use of nonfood substances made
from plants such as cacao (Theobroma cacao; Hall
et al. 1990; Hurst et al. 2002; Powis et al. 2002; Zarrillo
et al. 2018) and yaupon holly (Ilex vomitoria;Crown
et al. 2012; King et al. 2017), as well as fermented
beverages such as wine (McGovern et al. 2013) and
pulque (Correa-Ascencio et al. 2014). These studies
give us a means for nding the remains of ritual bev-
erages, exploring associated material culture, and
understanding their contexts of use. This, in turn,
makes possible the exploration of issues relating to
medicine traditions, ritual practices, elite culture,
and how these were adopted, changed, and moved
across cultural boundaries.
In this essay we apply mass spectrometry to the identication of
residues of Datura in late prehistoric shell and pottery vessels
from western Mexico and the southeastern United States. Datura
is a genus of owering plants that contain hallucinogenic alka-
loids that are still in use by native peoples in the region today.
The use of Datura before the coming of Europeans has been con-
rmed by direct archaeological evidence and indirectly through
iconography and early historical texts. However, identifying its
use through absorbed residue studies has not been accom-
plished until now. Using liquid chromatography mass spectrome-
try, we have identied a key Datura alkaloid (atropine) in samples
collected from 14 shell cups and 7 pottery vessels found in Mis-
sissippian and Caddoan Mississippian (AD 1000–1600) contexts in
Arkansas and Oklahoma, as well as in an additional 6 pottery ves-
sels recovered from precolumbian contexts in West Mexico. Our
results go beyond simply demonstrating that Datura residues can
be identied. They also reveal correlations between the presence
of Datura and particular vessel forms and modes of decoration.
DATURA USE IN NORTH AND
CENTRAL AMERICA
Humans have been using hallucinogens derived from plant and
fungi sources for millennia (Ratsch 2005:37–41). In North America,
one of the most potent hallucinogens was, and still is, produced
from plants in the genus Datura. Members of the Solanaceae
family, Datura are a series of owering plants whose leaves,
seeds, and owers contain tropane alkaloids such as atropine,
scopolamine, and hyoscamine (Lester et al. 1991). These alkaloids
produce hallucinogenic effects but also are toxic when consumed
in high enough doses.
Datura plants are found around the world, from North and South
America to Asia, Europe, and Africa. However, its natural range
is difcult to determine because it has become so widespread
(Lesteretal.1991). Datura is cultivated commercially in Central
America, North Africa, Ethiopia, India, and England for pharma-
ceutical purposes (Gerlach 1948) and is a common ornamental
plant found throughout North America.
Its use in North America before the coming of Europeans has
been conrmed by various kinds of archaeological evidence.
Datura seeds have been found in Archaic period contexts in
the Lower Pecos of Texas (Boyd and Dering 1996), in Ancestral
Pueblo (AD 1250–1300) contexts in Colorado (Litzinger 1981),
and in Mississippian (AD 1100–1200) contexts in Illinois (Emerson
and Jackson 1984). Further, it has been argued that imagery and
Datura fruit efgy pottery vessels conrm its presence from Mex-
ico (Kan et al. 1989) into the Southwest and even into the South-
east (Lankford 2012,2014). The sixteenth-century Aztec-language
Florentine Codex includes Datura as an important medicine plant
among the Aztecs (Ratsch 2005:41), and Datura continues to be
part of Native American medicine ways and ritual practices to this
day (Ratsch 2005:480–482).
Descriptions of modern-day practice indicate that Datura is used
for a variety of purposes, depending on the dose and method
of consumption (see Ratsch 2005:477–485). In Mexico and the
American Southwest, Datura is included in topical medicines
designed to treat physical injuries and ailments. Low doses, often
delivered by smoking the leaves, are considered an aphrodisiac
and also used in ritual divination. Tea produced from the leaves
and seeds delivers the highest doses of alkaloids and creates the
powerful hallucinatory experiences associated with shamanism
and spiritual journeys (Ratsch 2005:477).
THE SAMPLE AND METHODS
In an attempt to nd evidence of Datura use through absorbed
residues, we sampled 18 shell and 55 pottery vessels held in the
collections of the Gilcrease Museum at the Thomas Gilcrease
Institute of American History and Art in Tulsa, Oklahoma. The
tables below include information on each vessel included in this
study. Because all were acquired by Thomas Gilcrease from deal-
ers in the early twentieth century, we do not know the full history
of each piece, and this creates limitations that are apparent in the
tables as well as others that we will discuss below.
Thomas Gilcrease was an enrolled member of the Creek Nation
who had a lifelong passion for western American art, especially as
it related to the history of the west and his own Native American
culture. As a tribal member, Gilcrease wanted his collections to
exemplify the artistry, sophistication, and genius of Native Amer-
icans, past and present, and his collecting was guided by that
goal. Thanks to wealth generated by his oil businesses, Gilcrease
became a very successful collector of art, historical documents,
and Native American artifacts. In 1955, after decades of collect-
ing and an attempt to establish a museum in San Antonio, Texas,
Gilcrease transferred his collection to the city of Tulsa, Oklahoma,
and the museum that bears his name was established (Gilcrease
Museum 2018). The Gilcrease archaeology collections are prod-
ucts of their time, when standards guiding the recovery and
acquisition of artifacts were different. Although we do not have
specic information for each vessel included in this study, we pre-
sume that many were recovered using methods that today would
be considered destructive. Further, we suspect that many were
November 2018 Advances in Archaeological Practice A Journal of the Society for American Archaeology 313

Adam King et al.
TABL E 1. Mississippian and Caddoan Mississippian Ceramic Vessels Sampled.
Vessel
Accession Sample
Number Number Method Culture Period/Date Type Form Location Datura
5425-250 9 Sonicator Caddoan AD 1400–1500 Hardman Engraved Turtle-frog effigy Middle Ouachita River X
5425-296 21 Sonicator Mississippian Late Mississippian/
Protohistoric
Mississippi Plain Bottle Eastern Arkansas
5425-482 18 Sonicator Caddoan AD 1200–1300 Haley/Glassel
Engraved
Bottle Lafayette County, Arkansas
5425-576 13 Sonicator Mississippian Protohistoric Mississippi Plain Bottle with
medallions
Chickasawba (3MS5)
108 Burr
5425-595 23 Sonicator Mississippian Protohistoric Mississippi Plain Pedestaled bottle Chickasawba (3MS5)
110 Burr
5425-669 116 Sonicator Caddoan AD 1400–1500 Hatchell Engraved Bottle Lafayette County, Arkansas
5425-809 17 Sonicator Mississippian Protohistoric Walls Engraved Bottle Friend (3MS6)
107 Burr
5425-824 15 Sonicator Mississippian Late Mississippian/
Protohistoric
Walls Engraved Bottle Friend (3MS6) X
5425-858 22 Sonicator Mississippian Protohistoric Walls Engraved Bottle Friend (3MS6)
105 Burr
5425-885 1 Sonicator Caddoan AD 1500–1700 Hodges/Natchitoches
Engraved
Compound bowl Lafayette County, Arkansas X
5425-1105 24 Sonicator Mississippian Late Mississippian/
Protohistoric
Mississippi Plain Cat monster
effigy bowl
Castile Landing (3SF12)
5425-1213 20 Sonicator Mississippian Late Mississippian/
Protohistoric
Mississippi Plain Bottle Bradley (3CT7)
104 Burr
5425-1220 12 Sonicator Mississippian Late Mississippian/
Protohistoric
Mississippi Plain Frog effigy bowl Notgrass (3MS15) X
5425-1270 11 Sonicator Caddoan AD 1400 East/Friendship
Engraved
Compound
bottle
Montgomery County,
Arkansas
5425-1294 10 Sonicator Mississippian Protohistoric Untyped Red and white
head pot
Notgrass (3MS15)
111 Burr
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314

Absorbed Residue Evidence for Prehistoric Datura Use in the American Southeast and Western Mexico
TABL E 1. Continued
Vessel
Accession Sample
Number Number Method Culture Period/Date Type Form Location Datura
5425-1303 6 Sonicator Mississippian Protohistoric Carson Red-on-buff Head pot Rose Mound (3CS27) X
109 Burr
5425-1327 5 Sonicator Mississippian Protohistoric Untyped Female effigy
bottle
Mississippi County,
Arkansas
5425-1334 2 Sonicator Mississippian Middle
Mississippian
Untyped Female effigy
bottle
Eastern Arkansas
5425-1358 112 Sonicator Mississippian Protohistoric Rhodes Incised Bottle Rose Mound (3CS27)
5425-1426 117 Sonicator Mississippian Late Mississippian/
Protohistoric
Bell Plain Bottle Eastern Arkansas
5425-1510 4 Sonicator Mississippian Late Mississippian/
Protohistoric
Untyped Female effigy
bottle
Eastern Arkansas
5425-1514 3 Sonicator Mississippian Middle
Mississippian
Untyped Female effigy
bottle
Eastern Arkansas X
5425-1582 114 Sonicator Caddoan Untyped Bottle Southwest Arkansas
5425-1590 16 Sonicator Caddoan AD 1400 Hatchell Engraved Bottle Lafayette County, Arkansas
5425-1938 7 Sonicator Caddoan AD 1600–1700 Hodges/Natchitoches
Engraved
Composite bottle Red River Great Bend
5425-1949 27 Sonicator Mississippian AD 1500–1600 Walls Engraved Bottle Bradley County, Arkansas X
5425-2030 115 Sonicator Caddoan AD 1500–1600 Hatchell Engraved Bottle Lafayette County, Arkansas
5425-2541 113 Sonicator Caddoan AD 1400–1500 Untyped bottle Bottle Tillar Farms (3DR30)
5425-3619 8 Sonicator Mississippian Old Town Red Bottle Perr County, Arkansas
5425-4894 14 Sonicator Mississippian Late Mississippian/
Protohistoric
Mississippi Plain Bottle with
medallions
Banks (3CT13)
5425-5161 19 Sonicator Mississippian Late Mississippian/
Protohistoric
Mississippi Plain Bottle Banks (3CT13)
106 Burr
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Adam King et al.
TABL E 2. Mississippian and Caddoan Mississippian Shell Vessels Sampled.
Shell Cup
Accession Sample Sample
Number Number Method Location Date (AD) Style Form Location Datura
9025-544 63 Burr Cut columella 1200–1450 Craig B Decorated top Spiro (34LF40) X
9025-546 65 Burr Cut columella 1350–1450 Craig C Decorated top Spiro (34LF40) X
9025-553 68 Burr Cut columella 1200–1450 Craig B Decorated top Spiro (34LF40)
9025-554 78 Burr Interior back 1200–1450 Craig B Decorated fragment Spiro (34LF40) X
9025-587 75 Burr Lip left center 1100–1200 Braden A Decorated fragment Spiro (34LF40) X
9025-598 73 Burr Cut columella Whole undecorated Spiro (34LF40) X
9025-598 79 Burr Lip left center Whole undecorated Spiro (34LF40) X
9025-599E 67 Burr Cut columella Whole undecorated Spiro (34LF40)
84 Burr Lip left center Whole undecorated Spiro (34LF40)
9025-599H 25 Sonicator Whole undecorated Spiro (34LF40) X
60 Burr Cut columella Whole undecorated Spiro (34LF40) X
9025-599H 74 Burr Lip left center Whole undecorated Spiro (34LF40)
9025-599I 71 Burr Cut columella Whole undecorated Spiro (34LF40)
83 Burr Lip left center Whole undecorated Spiro (34LF40) X
9025-1472 64 Burr Cut columella 1350–1450 Craig C Decorated top Spiro (34LF40) X
9025-1473 66 Burr Cut columella 1200–1300 Braden B Whole decorated Spiro (34LF40) X
80 Burr Lip left center 1200–1300 Braden B Whole decorated Spiro (34LF40) X
9025-1554 62 Burr Cut columella 1200–1400 Craig A Decorated top Spiro (34LF40) X
9025-1665 69 Burr Cut columella 1350–1450 Craig C Decorated top Spiro (34LF40) X
9025-1670 61 Burr Cut columella 1350–1450 Craig C Decorated top Spiro (34LF40) X
9025-1718 77 Burr Interior 1200–1450 Craig B Decorated fragment Spiro (34LF40)
9025-1720 70 Burr Cut columella Whole undecorated X
81 Burr Lip left center Whole decorated Spiro (34LF40) X
9025-1727a 76 Burr Lip left center Undecorated outer whorl Spiro (34LF40)
9025-1749 72 Burr Cut columella Whole undecorated X
82 Burr Lip left center Whole undecorated Spiro (34LF40) X
acquired by Gilcrease in ways that do not meet today’s ethical
standards (Society for American Archaeology 2018).
Thirty-one of the ceramic vessels sampled (Tabl e 1 )derive
from various Mississippian and Caddoan Mississippian sites in
Arkansas. Contextual information associated with each vessel
is quite limited. However, thanks to the assistance of David Dye
of Memphis University and Ann Early and George Sabo of the
Arkansas Archaeological Survey, we were able to assign each ves-
sel to a type, time period, and, in some cases, a known archae-
ological site. All vessels date to the period between AD 1400
and 1700 and were chosen because of their unique forms (most
often bottles and efgies) and recognizable imagery (engraved
or incised in two dimensions or as three-dimensional forms). Our
operating assumption was that bottles and symbolically loaded
vessels are likely to have contained special liquids in the past.
In most cases, we know little more about their context than the
state and county where they were found.
The shell cups and fragments sampled (Tabl e 2 ) all reportedly
come from the famous Mississippian period Spiro site in LeFlore
County, Oklahoma (see Brown 1996). Spiro is well known for its
Craig Mound, built between AD 1250 and 1450, and was rst
brought to the attention of professional archaeology in the 1930s
by treasure hunters who leased the mound from the Pocola Min-
ing Company (La Vere 2007). Subsequent systematic excavations
and decades of work to reconstruct the nature of the features it
contained have revealed a unique set of mortuary practices that
included incredible quantities of engraved and plain shell cups
along with an unequaled cache of various sacred objects made of
pottery, shell, stone, and copper (Brown 2010). We presume that
the shell samples at the Gilcrease are part of that Craig Mound
assemblage, but we do not know for certain. Alex Barker of the
University of Missouri’s Museum of Art and Archaeology assisted
with stylistic associations for each of the decorated cups included
in Tabl e 2 .
It has long been assumed that shell cups, made from the outer
whorl of whelk shells (genus Busycon), were used as dippers
for serving and consuming ritual beverages. This assumption is
based on the many historic-period descriptions of Native Amer-
icans using shell cups in ritual settings, particularly for the con-
sumption of a Native American tea made from yaupon holly
called the Black Drink (see Hudson 2004).
Twenty-four of the ceramic vessels we sampled were collected
from various sites in western Mexico dating between the Early
Formative (1400–1000 BC) and Early Postclassic (AD 900–1250)
periods. While very little contextual information is associated with
the vessels (Tabl e 3 ), Chris Beekman of the University of Colorado
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316

Absorbed Residue Evidence for Prehistoric Datura Use in the American Southeast and Western Mexico
TABL E 3. Western Mexico Ceramic Vessels Sampled.
Accession Sample
Number Number Method Period/Phase/Date Form Location Datura
54.20362 44 Sonicator Comala phase, AD 1–500 Dog head effigy Colima
54.20459 28 Sonicator Terminal Early Formative,
1400–1000 BC
Bottle X
54.20461 30 Sonicator Early or Middle Formative,
2000–900 BC or 900–300
BC
Tall-neck jar Comala
5444-1713 101 Burr Comala phase, AD 1–500 Squash effigy Comala
5444-2092 99 Burr Comala phase, AD 1–500 Vegetable effigy Comala
5444-2094 100 Burr Comala phase, AD 1–500 Vegetable effigy Colima
5444-7346 42 Sonicator Middle Formative, 900–300
BC
Two-tiered gourd effigy jar Coastal Jalisco
5444-7366 33 Sonicator Late Formative, 300 BC–AD
200
Bowl X
5444-7411 38 Sonicator Late Formative–Early Classic,
300 BC–AD 500/600
Trophy head effigy Colima
5444-7551 35 Sonicator Late Formative–Early Classic,
300 BC–AD 500/600
Zoomorphic Jalisco
5444-8180 102 Burr Comala phase, AD 1–500 Squash effigy Colima
5445-1706 103 Burr Postclassic, AD 900–1500 Spouted vessel Aztatlan
5445-3551 39 Sonicator Comala phase, AD 1–500 Squash effigy globular jar Colima
5445-3571 32 Sonicator Comala phase, AD 1–500 Squash effigy globular jar Coastal Colima
5445-3585 34 Sonicator Postclassic, AD 900–1500 Molcajete X
5445-3597 29 Sonicator Late Formative–Early Classic,
300 BC–AD 500/600
Shallow bowl Nayarit X
5445-3800 31 Sonicator Postclassic, AD 900–1500 Molcajete X
5445-3947 43 Sonicator Late Formative, 300 BC–AD
200
Anthropomorphic effigy jar
5445-3986 41 Sonicator Late Formative–Early Classic,
300 BC–AD 500/600
Small tripod human effigy Possible Jalisco
5445-4002 37 Sonicator El Grillo phase, AD 500–900 Anthropomorphic face effigy Central Jalisco
5445-4004 40 Sonicator Comala phase, AD 1–500 Small bottle Colima
5445-4039 36 Sonicator Late Formative–Early Classic,
300 BC–AD 500/600
Foot effigy
5445-4256 45 Sonicator Comala phase, AD 1–500 Frog effigy Colima
5445-7384 26 Sonicator El Grillo phase, AD 500–900 Shallow bowl X
assisted in assigning each vessel to a type, cultural afliation, and
time period. The vessels were chosen for sampling because of
their unusual shapes—often specialized functional types or efgy
vessels—and because we assume that these unique vessels may
have held special liquids.
Our samples were collected using one of two methods (Tabl e s 1–
3). The rst, known as the burr method (Powis et al. 2002),
removes a portion of the interior surface and vessel through abra-
sion. For this sampling method, a clean piece of sandpaper was
used to collect each sample, and gloves were worn and changed
between samples. Each sample was collected on a fresh piece of
multipurpose paper and transferred to a clean vial for transport.
Although sample sizes varied, our target size was at least 1 ml.
The second method employed a Branson 2510 Ultasonic Bench-
top Cleaner. Traditionally used to clean objects, a sonicator has
a water tank that is vibrated using sound waves. In our sam-
pling, we placed 100 ml of distilled water in each vessel and
then placed the vessels in a shallow plastic container that oated
on the surface of the water in the tank. The water and the vessel
oating on it were then vibrated for 30 minutes, after which time
the samples were transferred to clean vials for transport.
Each sample collected was analyzed using mass spectrometry,
looking for peaks indicative of atropine and scopolamine. These
are two of the primary alkaloids found in Datura giving the plant
its hallucinogenic properties. In North and Central America,
no other plants are known to contain these particular alkaloids,
making it possible to use them as exclusive biomarkers for the
presence of Datura (Duke 2015).
All of the objects from which our samples were taken are
stored at the Gilcrease on open shelves. As a result, there is the
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Adam King et al.
TABL E 4. Contamination Samples.
Sample
Location Number Sample Type
Curation shelving: D3F right 46 Water
Curation shelving: D3F right 85 Cotton ball
Curation shelving: D3G center 47 Water
Curation shelving: D3G center 86 Cotton ball
Curation shelving: D3 top center 48 Water
Curation shelving: D3 top center 87 Cotton ball
Curation shelving: C3D right 49 Water
Curation shelving: C3D right 88 Cotton ball
Curation shelving: H9G left 50 Water
Curation shelving: H9G left 89 Cotton ball
Curation shelving: H5G right 51 Water
Curation shelving: H5G right 90 Cotton ball
Curation shelving: I1 top left 52 Water
Curation shelving: I1 top left 91 Cotton ball
Worktable foam 53 Water
Worktable foam 92 Cotton ball
Curator’s desk 54 Water
Curator’s desk 93 Cotton ball
Conservation desk 55 Water
Conservation desk 94 Cotton ball
Conservation room worktable 56 Water
Conservation room worktable 95 Cotton ball
Conservation room coffee maker
area
57 Water
Conservation room coffee maker
area
96 Cotton ball
Flat drawers near freezer and
cabinets
58 Water
Flat drawers near freezer and
cabinets
97 Cotton ball
AV room 59 Water
AV room 98 Cotton ball
possibility that they have been, and continue to be, exposed to
modern sources of contamination through air circulation systems
and human activities. For example, artifacts stored in this way
are exposed to caffeine-laden dust, which confounds the search
for cacao residue (Washburn et al. 2012). As a way of assessing
the potential for modern contamination in the Gilcrease sam-
ples, we collected and analyzed dust from shelving units and
work areas at the museum (Tabl e 4 ). Contamination samples were
collected by swabbing areas with cotton balls that had been
cleaned with alcohol and dampened with distilled water and by
wetting areas with distilled water, which was then collected using
clean pipettes.
LABORATORY METHODS
Atropine, scopolamine, and formic acid were purchased from
Sigma-Aldrich Chemical Co. (St. Louis, Missouri). All solvents
were mass spectrometry grade, and all other chemicals used
were of the highest grade available. An ACQUITY UPLC C18
1.7 µm(1×150 mm) column was purchased from the Waters
Corporation, Milford, Massachusetts.
A total of 117 samples were extracted using the following pro-
cedure. For the burr samples, 90 to 200 mg of burr from each
sample were added to a 0.25 ml water:methanol mixture (1:1).
Samples were vortexed and incubated at 80°C for 30 minutes.
After incubation, samples were sonicated (one minute), vortexed
(one minute), and centrifuged (three minutes). The resulting pre-
cipitate from each sample was removed, and the supernatant
was ltered with 5 kD membrane lters. Water-based samples
obtained by sonicator were freeze-dried completely. A 0.25 ml
water:methanol mixture (1:1) was added, and the samples were
sonicated (one minute), vortexed (one minute), and centrifuged
(three minutes). The supernatant was ltered with 5 kD mem-
brane lters. The ltrates from both extraction methods were
transferred to vials for ultra performance liquid chromatography
(UPLC)/tandem mass spectrometry (MS-MS) analysis.
Linearity, accuracy, precision, limit of detection, and limit of quan-
titation parameters were determined for atropine and scopo-
lamine. To calculate limits of detection, various concentrations—
0.05, 0.10, 0.25, 0.50, 1.0, 2.5, 5.0, 10, 25, 50, 100, 250, 500, 1,000,
and 5,000 pg/ml—of the analytes were injected to UPLC/MS-
MS. The injected amount that resulted in a peak with a height
at least three times as high as the baseline noise level was used
as the limit of detection. Intraday precision and accuracy were
determined by calculating the percent coefcient of variation and
relative error of the measurement of ve replicates of each of the
validation standard concentrations, analyzed on the same day.
A Waters Xevo TQ triple quadrupole mass spectrometer was
used to record MS and MS-MS spectra using electrospray ion-
ization in positive ion mode, with capillary voltage of 3.0 kV, an
extractor cone voltage of 3 V, and a detector voltage of 500 V.
Cone gas ow was set at 50 L/hour, and desolvation gas ow
was maintained at 600 L/hour. Source temperature and des-
olvation temperature were set to 150 and 350°C, respectively.
The collision energy was varied from 6 to 13 to optimize four
different daughter ions. The acquisition range was 20–350 D.
Pure standards (Figure 1; atropine and scopolamine) were intro-
duced to the source at a ow rate of 10 μl/minute by using a
methanol:water (1:1) and 0.1% formic acid mixture as the carrier
solution to develop a multiple reaction monitoring method for
UPLC/MS-MS operation.
UPLC/MS-MS analyses of all the samples were carried out with
a Waters ACQUITY UPLC System connected with a Xevo TQ
triple quadrupole mass spectrometer. Analytical separations on
the UPLC system were conducted using an ACQUITY UPLC C18
1.7 µmcolumn(1×150 mm) at a ow rate of 0.15 ml/minute.
The gradient started with 100% A (0.1% formic acid in H2O) and
0% B (0.1% formic acid in CH3CN) changed to 50% A over three
minutes, followed by a four-minute linear gradient to 10% A,
resulting in a total separation time of seven minutes. The elutions
from the UPLC column were introduced to the mass spectrom-
eter, and the resulting data were analyzed and processed using
MassLynx 4.2 software (Figure 1). A pure standard mixture was
used to optimize the UPLC conditions prior to analysis. Blanks
Advances in Archaeological Practice A Journal of the Society for American Archaeology November 2018
318

Absorbed Residue Evidence for Prehistoric Datura Use in the American Southeast and Western Mexico
FIGURE 1. Ultra performance liquid chromatography/tandem mass spectrometry chromatograms: (A) standard atropine; (B)
blank; (C) representative Gilcrease sample confirming the presence of atropine.
were run in duplicate at the beginning, middle, and end of each
run after the standards.
The developed method was validated by determining limit of
detection, limit of quantication, linear dynamic range, precision,
and accuracy (Tabl e 5 ). The analytical parameter determinations
of the atropine and scopolamine were done using standard mix-
tures. The results indicated that the limit of detection was 0.5 and
1 pg and the limit of quantitation was 1.5 and 3 pg for atropine
and scopolamine, respectively, suggesting that the developed
method is highly sensitive. The linearity of the method was deter-
mined from the calibration curves constructed for atropine and
scopolamine. The data for accuracy, precision, and recovery
are presented in Tab l e 5. These results provide support that
this method is dependable and reproducible for the analysis of
atropine and scopolamine.
RESULTS
As Tabl e 1 shows, seven of the 31 Mississippian ceramic ves-
sels returned results positive for atropine, while none contained
scopolamine. The presence of atropine was further conrmed
by co-chromatography (Supplemental Figure). All of these pos-
itives were identied in samples collected using the sonicator.
This might suggest that the burr method somehow systematically
selected against recovering atropine. However, the eight vessels
sampled using both the sonicator and burr method produced
November 2018 Advances in Archaeological Practice A Journal of the Society for American Archaeology 319

Adam King et al.
TABL E 5. Validation of Detection Method.
Variable Atropine Scopolamine
Limit of detection 0.5 pg 1pg
Limit of quantitation 1.5 pg 3pg
Linearity 0–5,000 pg 0–5,000 pg
Standard concentration (pg) %CVPrecision % RE Accuracy %CVPrecision % RE Accuracy
0.05 23.1 3.0851
0.10 41.1 5.2151 51.4 11.9111
0.25 12.9 0.6866 43.7 10.1706
0.50 15.6 0.5274 34.2 4.1028
1.0 8.0 0.1772 21.2 1.3881
2.5 12.1 0.1349 12.1 0.4348
5.0 5.2 0.0499 6.0 0.1797
10 5.8 0.0386 8.9 0.2092
25 2.5 0.0113 6.4 0.0988
50 1.5 0.0051 6.9 0.077
100 3.1 0.0069 7.1 0.0554
250 1.8 0.0025 3.1 0.0143
500 5.9 0.0052 3.8 0.0121
1,000 3.0 0.0013 4.0 0.0067
2,500 1.6 0.0004 1.3 0.0008
5,000 0.7 0.0001 1.2 0.0005
Note: %CV=percent coefficient of variation; % RE =percent relative error.
consistent results, in this case all negative. These ndings, along
with the results from the shell samples, suggest that both meth-
ods are equally effective in recovering atropine residue. Among
the positive Mississippian vessels are bottles and bowls, includ-
ing special efgy forms, potentially representing both the storage
and consumption of Datura beverages.
Fourteen of the shell cups and fragments we sampled contained
traces of atropine (Tabl e 2 ), while none contained scopolamine,
a pattern also seen with the ceramic vessels. Only one shell cup
was sampled using the sonicator (Cat. #54250-1949). Because the
vessel had to oat in the sonicator for this method to work, cura-
tors at the Gilcrease agreed to allow this sampling method with
only one shell. The sonicator sample found traces of atropine in
the cup, but the two subsequent burr samples from the same
cup did not. Seven other cups or fragments were sampled in
two locations using the burr method. Those locations included
the area along the outer whorl of the cup and the cut surface at
the top of the shell where the inner column had been removed.
Our results show that both areas have the potential to contain
atropine traces.
Of the 24 vessels deriving from western Mexico, 6 had traces
of atropine, but scopolamine was absent in all cases (Tabl e 3 ).
These vessels range from the Early Formative (1400–1000 BC)
to the Early Postclassic (AD 900–1250), showing that Datura use
persisted over a long period in the region. Three of the vessels
are simple bowls that we can assume were used to consume
Datura beverages. Two of the vessels are tripodal mocajetes with
a grinding surface built into their form, suggesting that they were
used in the preparation of Datura beverages. The last sampled
vessel is a small bottle that may have been used to hold prepared
Datura beverages.
As noted above, we also collected and analyzed samples of dust
recovered from 14 different locations in the curation and work
areas of the Gilcrease Museum (Tab l e 4). In all cases, no traces
of atropine or scopolamine were found in the dust samples. The
absence of these alkaloid residues on the shelves suggests that
the atropine we found in the shell and pottery vessels was likely
not introduced through contamination within the museum. While
it is still possible that the atropine residues detected are the
result of other kinds of contamination, we see that as unlikely.
Atropine is not found in high levels in groundwater like other
alkaloids such as caffeine (Fram and Belitz 2011), so postdeposi-
tional contamination through water percolation or postrecovery
contamination through washing seems unlikely. Given that we
do not know the full history of the Gilcrease Museum objects
sampled, it is possible that they were contaminated with modern
sources of atropine through intentional or unintentional human
actions. This is unlikely because, outside of recreational use, the
most common uses of atropine are in the medical eld, where
it is most often administered intravenously or through injection
(American Society of Health-System Pharmacists 2016).
DISCUSSION
All of the Mississippian vessels that tested positive for atropine
either are decorated with iconographic motifs or are efgy ves-
sels in forms related to the Mississippian cosmological concept
of the Beneath World—one of three realms of the Mississippian
cosmos (Lankford 2007a,2011; Reilly 2004). The others are the
sky realm, or Above World, and the surface realm, This World.
Each of these three realms was associated with its own super-
naturals, unique powers, and ritual themes. The Beneath World
Advances in Archaeological Practice A Journal of the Society for American Archaeology November 2018
320

Absorbed Residue Evidence for Prehistoric Datura Use in the American Southeast and Western Mexico
FIGURE 2. Drawing of imagery on Walls Engraved bottle, GM
5425–824, Gilcrease Museum, Tulsa, Oklahoma (Perino et al.
1960:149; reproduced with permission of Central States
Archaeological Journal).
was a place of chaos and the realm of the dead, as well as the
source of water and the growth of the natural world. Each day
when the setting sun descended into the Beneath World, the day
sky and the Beneath World switched places. Beings such as the
Lord of Death and an earth mother gure associated with the
moon inhabited this underwater and night sky realm. Given these
associations, Beneath World powers would have been involved
in rituals associated with death, but they were also important
as sources of rain and the productivity of the earth and human
populations.
One vessel that tested positive for Datura is a medium-sized
bottle incised with images representing the Underwater Panther
and the Great Serpent (Figure 2; Perino et al. 1960). According
to Lankford’s (2007b) research with Native American sacred nar-
ratives, both of these images represent avatars of the Lord of
Death in the Beneath World. Keeping with this thematic associ-
ation, two additional Datura-positive vessels are efgies of frogs
or a turtle, both of which are associated with the watery Beneath
World, and another is engraved with a swirl design also arguably
associated with that same realm (Lankford 2011).
Another of the Datura-positive Mississippian vessels is an efgy
of a female gure, understood to be a cognate of historic-period
earth mother gures such as Old-Woman-Who-Never-Dies
(Figure 3). Many groups in the Eastern Woodlands of North
America consider this woman to be the moon in the night sky,
so she is often associated with the Beneath World realm and its
powers (Duncan and Diaz-Granados 2004). Dye (2015) has argued
recently that female efgy vessels found in the Lower Mississippi
Valley may have helped create a connection between women
and female guardian spirits. These bottles were efgies of those
spirits as well as living manifestations of them. In her study of
guardian spirits, Ruth Benedict (1923) noted their widespread
occurrence in North America and the use of Datura as a source
FIGURE 3. Female effigy bottle, GM 5425-1514, Gilcrease
Museum, Tulsa, Oklahoma.
of dreams through which women found and communicated with
such spirits. Our discovery of atropine residue in a female efgy
bottle from Arkansas lends support to this argument.
The remaining Datura-positive vessel is a human head efgy
(Figure 4). Similar heads appear as early as the twelfth century in
Mississippian art, and they have been interpreted as belonging
to an Above World creator gure who was decapitated battling
monsters in the Beneath World (Brown 2007;Walker2004). This
decapitated creator gure was brought back to life by his sons
after they brought his head back from the Beneath World. While
there are multiple potential associations of this human head
efgy, it may also be related to powers and rituals of the Beneath
World. If that is the case, then it may have been part of rituals
focused on the return of spirits after death.
Ten of the shell cups and fragments with atropine residue were
decorated, and their stylistic assignments are listed in Tabl e 1 .
Only one of these is a whole vessel, and it was decorated in
the Braden B or Late Braden style (Phillips and Brown 1978). It
exhibits the amphisbaena theme, which is a creature with snake-
like characteristics associated with the Beneath World (Figure 5).
November 2018 Advances in Archaeological Practice A Journal of the Society for American Archaeology 321

Adam King et al.
FIGURE 4. Carson Red-on-buff human head effigy bottle, GM 5425-1303, Gilcrease Museum, Tulsa, Oklahoma.
FIGURE 5. Braden B shell cup, GM 9025-1473, Gilcrease Museum, Tulsa, Oklahoma.
The other eight atropine-positive samples are vessel fragments
and all exhibit imagery executed in the Craig A, B, or C style
(Phillips and Brown 1984). The theme of the imagery on each is
difcult to understand given their fragmentary nature. It may be
important to note that, regardless of attached imagery, shell is
associated with water and therefore the Beneath World.
There is also some interesting patterning in the decoration
and form of the Datura-positive vessels from West Mexico.
Two of these bowls are painted with designs that appear to
mimic Datura seedpods. One of the vessels is a shallow bowl
(Cat. #5444-7366) dating to the Late Formative period (300 BC–
AD 200) with imagery resembling a maturing Datura seedpod
(Figure 6). Another vessel is a shallow bowl (Cat. #5445-3597)
dating to the Late Formative/Early Classic period (300 BC–AD
500/600), and it is decorated with motifs that resemble an open-
ing Datura seedpod (Figure 7). Ceramics in the region are well
known for taking recognizable efgy forms of plants, fruits, and
even animals. It is often assumed that the vessel form is related to
its use (Schondube 1998), and this pattern appears to be the case
for these two bowls with Datura residue in them.
It is worth noting that two of the Datura-positive vessels take
the mocajete form (Figure 8) and date to the Early Postclassic
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322

Absorbed Residue Evidence for Prehistoric Datura Use in the American Southeast and Western Mexico
FIGURE 6. Late Formative bowl, GM 5444–7366, Gilcrease Museum, Tulsa, Oklahoma.
FIGURE 7. Late Formative–Early Classic bowl, GM 5445-3597, Gilcrease Museum, Tulsa, Oklahoma.
period (AD 900–1250). While this may be an artifact of our limited
ceramic sample, it appears that earlier uses of Datura in West
Mexico were associated with bowls decorated with Datura motifs.
Later Datura preparation and consumption are associated with
another kind of specialized vessel, this time one with a prepared
grinding surface built in.
SIGNIFICANCE
Until now, the only direct means of identifying Datura use in pre-
historic contexts was through the recovery of preserved portions
of Datura plants. Charred seeds have been found in context
(Emerson and Jackson 1984:333), and there is the possibility that
Datura phytoliths may be recoverable as well. The use of Datura
has also been inferred more indirectly through the interpretation
of imagery as well as the presence of what some have argued are
Datura fruit efgy vessels. With our demonstration that Datura
is preserved as absorbed residues in both pottery and shell ves-
sels, we have introduced another means of directly identifying
the plants’ use in prehistoric contexts. Absorbed residues have
the benet of being preserved more commonly than actual plant
remains and being recoverable from a ubiquitous type of mate-
rial culture (pottery), whose form and style allow it to be dated
November 2018 Advances in Archaeological Practice A Journal of the Society for American Archaeology 323

Adam King et al.
FIGURE 8. Molcajete vessels, Gilcrease Museum, Tulsa, Oklahoma: (a) GM 5445-3800 (b) GM 5445-3585.
and sourced fairly readily. Also, often vessels are directly associ-
ated with imagery that further allows for some understanding of
the connection between Datura use and ritual themes.
In this study, we have demonstrated the efcacy of the sonicator
sampling method for recovering absorbed residues from pottery
and shell, especially residues containing atropine. While other
water-based sampling methods have been used to recover caf-
feinated beverage residues from pottery (Washburn et al. 2012),
the sonicator method has not been used to sample pottery for
absorbed residues until now. However, Zarrillo and colleagues
(2018) did use a sonicator to collect starch grains from ceramic
vessels and also to sample cacao absorbed residues from stone
bowls. The sonicator method is less destructive than burr meth-
ods, which actually remove a portion of the vessel. It also has
the benet of using vibration to release absorbed residues from
vessel matrices, while other wash sampling methods rely only on
solubility to collect samples.
Admittedly, the provenience information available for the objects
we sampled does not meet modern standards, and that places
limits on what we are able to infer from our results. Despite this
Advances in Archaeological Practice A Journal of the Society for American Archaeology November 2018
324

Absorbed Residue Evidence for Prehistoric Datura Use in the American Southeast and Western Mexico
limitation, we can make some useful inferences from the data
generated. We can, with reasonable condence, conclude
that Datura was used in Mississippian and Caddoan contexts
in Arkansas and from the Middle Mississippian (AD 1350–1450)
to the Protohistoric (AD 1500–1700) period in Oklahoma in both
ceramic and shell vessels. We already had an idea that it might
have been used in this area because of mentions in ethnographic
reports and archaeological data, but now we have conrmed it.
We can also conclude that Datura consumption involved ceramic
bottles and bowls, as well as shell vessels. Based on historical
information, it has long been assumed that shell cups were used
in ceremonies that included the Black Drink—a tea made from
yaupon holly leaves. Now we must be open to the idea that these
vessels were used in the consumption of more than one kind of
ritual beverage.
Because we chose Mississippian and Caddoan Mississippian
vessels that carried imagery (through their form or decoration),
we made it possible to explore the correlation between what
we understand about the thematic associations of particular
imagery and Datura consumption. In these areas there is a clear
correlation between the presence of Datura and Beneath World
beings and locatives on Mississippian and Caddo pottery ves-
sels. That association holds for the shell cups decorated in the
Braden stylistic tradition. The Craig imagery is different in that
it depicts ritual events that likely involved both people and
supernaturals. These are important observations because they
give us clues to the rituals that included Datura use in these cul-
tural settings.
We can also be reasonably condent that Datura was prepared
and consumed in West Mexico during the Late Formative to
the Early Postclassic period. The presence of atropine in the
mocajete vessel form suggests that grinding was part of the
preparation of Datura. Because modern mocajetes are used to
grind spices, including chili, it is often assumed that prehistoric
versions were used for the same purpose. While this has yet to
be demonstrated, it is apparent that the vessel form was used
to grind other plants included in specialized beverages, partic-
ularly Datura. Those beverages were served in, and probably
consumed from, simple bowls decorated to resemble a Datura
seedpod.
Probably the most important contribution this study makes is in
the potential it opens for future research. We have shown that
atropine preserves in ancient shell and pottery vessels, it can be
recovered using both sonicator and burr methods, and it can
be measured using liquid chromatography mass spectrometry.
The inferences we can draw from our current sample are limited
because of a lack of contextual information. However, future
targeted studies using objects with more detailed contextual
information can begin to explore a whole host of interesting
questions.
Several researchers (Lankford 2012; Litzinger 1981), along with
this study, have suggested that there may be particular vessel
types and decorative forms associated with Datura use. These
ideas can now be evaluated. We have introduced some infer-
ences about the thematic associations of Datura use in the Mis-
sissippian period. Future studies that correlate Datura presence
and iconographic interpretations will surely give us a fuller under-
standing of how and why Datura beverages were prepared and
consumed in different cultural contexts. We know a good deal
about recent uses of Datura (Ratsch 2005), but we know much
less about its older contexts of use and where it t into ritual
practices and ancient social systems. With targeted sampling of
more vessels from various places and contexts, it will be possible
to generate a clearer understanding of the use of Datura in time
and space.
Finally, special beverages like those made from Datura are asso-
ciated with ritual practices. Like so many other aspects of human
behavior, these practices often have a place of origin and history
of spread, alteration, and adaptation to new settings. The study
of ritual beverages allows for the exploration of ritual complexes,
their histories, and how they are part of culture-making on local
and regional scales.
Acknowledgments
We would like to express our appreciation to the curators and
staff at the Gilcrease Museum for providing us with access to
their collections for sampling. In particular we would like to thank
Ann Boulton, Laura Bryant, Susan Buchanan, Joanna Didik, and
Kate Galatian for their help, understanding, and patience. The
Savannah River Archaeological Research Program, the South
Carolina Institute for Archaeology and Anthropology, and the
Gilcrease Museum each funded portions of the project. A thank-
you also goes to Rob Cross of the Gilcrease Museum for taking
the vessel photographs. Finally, we wish to thank the anonymous
reviewers for providing valuable comments and improving our
essay.
Data Availability Statement
The mass spectrometry data generated using samples col-
lected from pottery vessels, shell vessels, and surfaces at the
Gilcrease Museum are archived at the Gaikwad Steroidomics
Laboratory (http://gaikwadsteroidomics.com/) and are available
upon request. The unanalyzed portions of the physical sam-
ples collected from archaeological specimens and surfaces
at the Gilcrease are also stored at the Gaikwad Steroidomics
Laboratory.
Supplementary material
To view supplementary material for this article, please visit
https://doi.org/10.1017/aap.2018.30
Supplemental Figure. UPLC-MS/MS chromatograms of sam-
ple extract (bottom) and sample extract spiked with standard
atropine (top).
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AUTHORS INFORMATION
Adam King South Carolina Institute of Archaeology and Anthropology,
University of South Carolina, 1321 Pendleton Street, Columbia, SC 29208, USA
(aking@sc.edu, corresponding author)
Terry G. Powis Department of Geography and Anthropology, Kennesaw
State University, 402 Bartow Avenue N.W., Kennesaw, GA 30144–5591, USA
(tpowis@kennesaw.edu)
Kong F. Cheong Department of Anthropology, American University, Hamil-
ton Building, 4400 Massachusetts Avenue N.W., Washington, DC 20016, USA
(kongcheong@trentu.ca)
Bobi Deere Department of Anthropology, University of Oklahoma,
455 West Lindsey, Dale Hall Tower 521, Norman, OK 73019, USA
(bobi.deere@ou.edu)
Robert B. Pickering Department of Anthropology, University of
Tulsa, Harwell Hall, 800 South Tucker Drive, Tulsa, OK 74104, USA (bob-
pickering@utulsa.edu)
Eric Singleton National Cowboy and Western Museum,
1700 Northeast 63rd Street, Oklahoma City, OK 73111, USA
(esingleton@nationalcowboymuseum.org)
Nilesh W. Gaikwad Gaikwad Steroidomics Laboratory, LLC, 1949 Fifth
Street, Suite 110, Davis, CA 95616, USA (nilesh@gaikwadsteroidomics.com)
November 2018 Advances in Archaeological Practice A Journal of the Society for American Archaeology 327