1

“Scents in the ancient civilizations of

the Mediterranean basin:

archaeometric studies on Cleopatra’s

officine (En Boqeq, Israel) and on

Pyrgos/Mavroraki’s perfumery

(Cyprus) ”

Alessandro Lentini

CNR-ITABC, ROME

alessandro.lentini@itabc.cnr.it

CLEOPATRA'S OFFICINE AT EN BOQEQ (ISRAEL)

*including Giuseppe Donato † notes.

1- Geography and vegetation

The archaeological area of En Boqeq was discovered in the early

1980s by Professor Mordechai Gichon of the University of Tel

Aviv. The site lies at the southern tip of the Dead Sea, 30 kilometres

south of the En Gedi oasis, in one of the world’s deepest

depressions, some 400 metres below sea level. The Dead Sea Basin

was formed 5 million years ago as part of the great Syrian-African

depression; Jordan’s Moab mountains lie to the east, the Wilderness

of Judaea to the west and the Negev desert to the south-west. The

Dead Sea is a terminal lake, meaning it has no outlet (Fig. 1). It is

fed mainly by the Jordan river, which flows in from the north, and

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by hot springs along the shores, and occasionally by winter rains.

The only way that water can leave the Dead Sea is by evaporation.

Fig. 1

This process is a very active one, due to the area's high

temperatures and extremely low humidity (O. Potcher, 2000).

The water level has been falling steadily, and as a result the lake has

gradually shrunk and changed its shape. It is currently about 70 kms

long and 17 kms wide, and covers an area of about 1,000 sq. km.

Due to its high average salinity levels, the Dead Sea is classified as

polyhalinic. The temperature and salinity variables in this unique

habitat are among its fundamental features. The organisms (bacteria

and algae) that currently inhabit it are classified as euryhalines and

eurytherms, meaning that their salt and temperature-tolerance range

is very broad.

The stressful physical conditions have kept the area’s biodiversity

very low. According to observations reported in the literature,

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physiologically stereohaline fish coming from the Jordan die as soon

as they enter the Dead Sea, because they cannot adapt their osmosis-

regulating processes quickly enough. Temperature, precipitation and

salinity are major limiting factors; data on them are summarised in

the two climate graphs shown in (Figs. 2 and 3). The data for 1971-

1987 were supplied by the Israeli Ministry of Transportation and

Communication's Weather Service.

Figs. 2 and 3

Due to evaporation and to shore erosion caused by lake water and

runoff down the surrounding cliffs, the concentration of mineral

salts in the Dead Sea (for the most part, magnesium, sodium and

potassium chlorides) is almost ten times higher than in the open

seas. At present, the vegetation that makes up the Dead Sea area’s

typical biome is distributed in nine basic micro-environments

(marshes, salt-water rivers, the cliffs above the Jordan, the shores,

the lowlands, wadis and depressions, the halophytic belt, seasonal

vegetation and widely disseminated arboreal vegetation. Marshes

abound in the area, especially around Ein-Fashkha. Their vegetation

belongs to the Junco-Phragmition, Tamaricion-Tetragynae and

Atriplico-Suaedion alliances. The latter is classified as

mesohalophytic, due to the presence of the saltworts Salsola pachoi

and Salsola vermiculata, and is in direct contact with wet earth. The

Junco-Phragmition alliance forms the reed belt that runs along the

banks of the Jordan; Phragmites australis is very common here. The

cliff-sides above the river are occupied by the species Suaedetum

maritimae (Asthenatherum forskalii, a member of the Poaceae

family), while the shores of the estuary flowing into the Dead Sea

(at high altitude) are mainly populated by Tamarix jordanis. The

shore environment is made up of the Saharo-Sindian element, whose

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basic unit is a community in which Zygophylletum dumosi is allied

with the evergreens Anabasidion articulatae, Chenoleion arabicae

and Suaedion asphalticae. These evergreens also inhabit the

lowlands, where the low humidity of the air is offsetted by runnels

that keep the soil moist. Seasonal grassy vegetation appears only in

the wintertime, when the short rainy season fosters the growth of a

plant community that includes Suaedetum asphaltica, Suaedetum

palaestinae, Suaedetum fruticosa and Chenoletum arabica, plus

small percentages of Kickxia judaica, Ophioglosum polyphyllum,

Withania obtusifolia and Polygomum argyrocoleum. Wadis (small

permanent or seasonal streams) and depressions host thin vegetation

consisting of alliances among Anabasis articulata, Zilla spinosa,

Hammada scoparia, Salsola pachoi and Salsola vermiculata.

Various Anabasis species (syriaca, oropediorum and seblera are

also present, though in lower percentages. The territory hosts three

tree alliances (Fig. 4), more or less persistent. Proceeding from the

shoreline to the hinterland, we find Populus euphratica on the banks

of the stream, then intermediate communities centred on Zizyphus

spinachristi, and finally a Saharo-Sindian alliance formed by

various Acacia species (Acacia tortilis Hayne, Acacia raddiana Savi

and Acacia pachyceras).

Fig. 4

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2-En Boqeq– Cleopatra’s workshop

The excavations directed by Professor Mordechai Gichon led to the

discovery of an Officina, or workshop, for the fabrication of

ointments and perfumes (M. L. Fischer, M. Gichon and Oren Tal,

2003). It had been built in the 1st century B.C., during the reign of

Herod the Great, who wished to exploit the area's mineral resources

and hot springs. Later (34-33 B.C.), Mark Antony gave Cleopatra

control over the Dead Sea districts from Jerico south, and she

became the owner of the establishment. During the excavations, the

workshop was found to be in an excellent state of preservation (Fig.

5), especially the walls and the floor.

Fig.5

It was a highly complex structure, with nine rooms. Room A is

marked by the presence of a washtub, while rooms B and C – used as

waiting rooms for customers – were fitted with stone benches and

seats, still in place. Sector G contains two mills and a tub, which were

used to grind and decant different products. Room E contains two

large tubs used for steeping and decanting, a large oven and a

fireplace used in the final steps in the preparation of ointments and

perfumes. In rooms F and G of this well-preserved structure, the

archaeologists identified several deposits of organic residue from the

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production processes (Figs. 6 and 7), and took samples for physical,

chemical and archaeobotanical analysis. Above sector H rose a tower

that had probably been used to keep an eye on the crops growing

around the building. Quantities of bituminous mud were discovered

inside the laboratory. This substance is found in natural beds in some

parts of the Dead Sea area; Pliny tells us that in Latin it was called

asphaltite, and that the whole Dead Sea was known to the Romans as

Lacus Asphaltite, the Asphalt Lake:

“Nihil in Asphaltite, Judaeae lacu qui bitumen gignit, mergi potest....

(Pliny, Nat. Hist. II) (In Asphaltite, a lake in Judaea that produces

pitch, nothing sinks...) Asphaltite nihil praeter bitumen gignit: unde et

nomen...“ (Pliny, Nat. Hist. V) (The Asphalt Lake produces nothing

but pitch, hence its name....).

Figs. 6 and 7

3 Description and composition of Dead Sea

Dead Sea mud, locally called Judaean pitch or Syrian asphalt, is a

bitumenous substance (Fig.8) derived from petroleum via evaporation

of light hydrocarbons (C<12) and partial oxidation of the residue. It is

found in nature in the form of a very fragile and shiny black lump that

gives off a salty/sulphurous odour and is very salty. In flame tests

performed to determine its combustion point, Dead Sea mud was

found to burn easily, with a bright flame. Its abundant content of

potassium, calcium, iron, magnesium, silicon, sodium, sulphur,

iodine, aluminium and lithium makes it especially effective in treating

skin diseases (psoriasis, eczema, scaling).

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Density: 1.00-1.18. Insoluble in water, acids and alkalis. Soluble in

oil of turpentine, petroleum, alcohol, chloroform, acetone and ether.

Fig. 8

Chemical Compounds %

MgCl2 32

KCl 25

NaCl 16

Br 0,4

Sulphates 0,2

Residual insoluble 0,2

Degree of crystallization in H2O 26

Tab. 1 -Average percentages of major components

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4 Description and composition of Dead Sea salts

Dead Sea salts consist of odourless white and cream-coloured

crystals: in organoleptic tests, they are found to have a very strong taste.

Components: magnesium, calcium, potassium, sulphates, bromide, trace

carbonates of other cations and anions.

Through an osmosis-hydration process, these components can pull a

great part of the impurities ensconced in the deepest layers of the skin

to the surface. Their main functions are shown on the following table:

Magnesium

Anti-allergic for the sensitive skins, optimal hydrating

and corrector of many necessary enzymes for cellular

activity.

Bromine

Antiseptic, healing, calming, alleviates the conditions

of dermatological pathologies (es. psoriasis) and

contributes to the relaxation of the nervous

extremities.

Sodium Activate in transporting substances through the

cellular membranes, it favours escapes it of toxic

substances from the inside toward the outside.

Potassium

Rule and controls the water equilibrium it accelerates

the cellular metabolism and the growth of new cells.

Chlorine

It contributes to becoming stabilized itself of the new

cells.

Calcium

It strengthens the walls of the cellular membrane,

alleviates the pains and assets the enzymes.

Zinc Enzymatic regulator of the cellular reproduction.

Table n° 2 - Main component of salts and relative officinal’s functions.

5- The most important historical sources

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Research conducted in the 1980s in collaboration with Professor

Alberto Grilli, of the State University of Milan, enlarged and

updated an initial bibliography on fragrant substances in antiquity,

on which work had begun in the '70s (G. Donato, M. E. Branca and

A. Rallo, 1975). The essential data are described below.

The first evidence we have of the use of ointments for the human

body dates from 2450 B.C. (R. J. Forbes, 1955); it concerns the

religious aspects.

The earliest written descriptions of the use of scents are in the

Bible. In the Old Testament we come upon actual recipes, like the

one for the holy oil used to anoint ritual objects and altars (Exodus

30:22-25): 500 shekels of myrrh, 250 shekels of cinnamon, 250

shekels of sweet calamus, 500 shekels of cassia and a hin of olive

oil. Starting in the 7th century B.C., as trading intensified, the use of

cosmetics spread to other areas too. Herodotus (I:193,195) tells us

that the Babylonians, who did not use olive oil, coated their bodies

with ointments based on sesame oil (Sesamum indicum).

Xenophon (Cyropaedia VII:8, 20) describes certain substances

used by the Persian notables; they are very similar to some of the 27

ingredients in the "Royal Ointment" described by Pliny the Elder

centuries later (XIII:2,2). Herodotus also describes some of the

customs of the barbarian peoples; the Scythians, for instance, were

in the habit of alternating between steam baths and coating of soft

pastes made of cypress and cedar bark plus incense.

As to Greece, the use of fragrant substances is first mentioned in

Homer, where they are still associated with religious ceremonies.

Starting in the 7th

century BC, the sources describe their use as

beauty products for women, and also the Greeks' growing use of

products imported from Persia. Archaeological excavations likewise

document the Greeks' frequent use of oils, starting in the 8th century

B.C. The documentation is provided not by organic residues found

in the excavations, but by a series of small proto-Corinthian

aryballoi and alabastra, and also by small jars fashioned in oriental

bucchero.

The diffusion of these containers for precious substances suggests

the development of a vast export trade throughout the Mediterranean

basin. In parallel with the importation of fragrant substances from

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the East, there were also local artisan-scale perfume productions that

varied over time, depending on fashion and taste, which shifted

from perfumes made on the Greek isle of Delos to those from the

Nile delta city Mendes, from Kyzikos in Asia Minor and from

Corinth. Centuries later, Pliny also wrote of adulterated scents: by

no means a phenomenon of our own day alone. Starting in the 6th

century B.C., we have more accurate descriptions of the fragrant

essences used in the Greek world, written by naturalists; many of

these authors recapitulated earlier works that have not come down to

us in the original.

One treatise widely read in antiquity was De plantis, attributed to

Aristotle's Lyceum and included in the Corpus edited by

Andronicus in the 1st century B.C., based on indications by the

philosopher Theophrastus of Eresus.

The text handed down through the medieval tradition (Atheneum

IV, 129) is thought by many scholars to be a fake (G. Donato, M. E.

Branca and A. Rallo, 1975). The earliest scientific texts that are

considered original – the first ones written on the basis of direct

observation – are Theophrastus's History of Plants and The Cause

of Plants.

The former is devoted to basic botanical classifications and

contains the first taxonomic indications on morphology; the latter

describes reproduction techniques. Besides these earliest scientific

writings, we have an innumerable quantity of quotations from the

ancient poets on the use of perfume (R. Cantarella, 1967). As regards the Etruscans, written references are rare but we have

significant documentation in paintings of daily life, which give

many details on women's use of bronze mirrors. Scholars believe

that the Etruscans were the first to introduce oriental perfumes in

Italy, though the artes unguentarie documented in various

archaeological excavations (G. Donato, G. Gullini, E. Negroni and

N. Negroni Catacchio, 1982) came from cities in Magna Graecia;

Sybaris, for instance, imported products from the East and exported

them to central Italy (Forbes, p.23).

The Romans were the direct heirs of the experiences of

Hellenistic civilisation and oriental pharmacology; after their time,

botanical, agricultural, environmental and technological knowledge

remained unchanged in Europe until the 17th century.

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The earliest evidence we have on the production, sale and use of

perfumes in Roman civilisation comes from Plautus and other poets

of his day, while the earliest scientific treatise was written by Pliny

(XIII: 24-25).

The Romans' use of fragrant substances is also described in

government documents. In 189 B.C., for example, the censors

banned the sale of unguenta exotica in the city of Rome, and a

century or so later also banned imports of these substances. The

reasons for these political and commercial measures were most

likely related to particular economic contexts.

The first ban was a step taken against the city of Capua; it hosted

the most important perfumeries but its inhabitants did not have the

status of Roman citizens. The second ban was an exceptional

measure taken during the civil wars of the 1st century B.C.

Perfume consumption peaked during the Empire, and a number of

reports on the matter have come down to us. Horace makes it clear

in various writings that he disapproved of the excessive use of

scents; Ovid, Martial and Juvenal document the types most widely

used; Lucilius, who lived during Nero's reign, notes their high cost.

The most authoritative and exhaustive source that has come down to

us, though, is Pliny's Naturalis Historia.

This work is extremely useful for its detailed descriptions of the

geographic and environmental origins, morphological and

physiological features, farming methods, technologies, costs,

marketing, uses and possible adulterations of officinal plants and

other natural substances used to make perfumes, ointments, resins,

oils, creams and essential oils (Pliny, Nat. Hist. XXXI:46,

XXXVI:26, 190; XXXVII).

Pliny also passes on reports from a variety of other sources,

including earlier works since lost; unfortunately, this information is

undocumented and cannot be used for comparative purposes.

Dioscurides, a contemporary of Pliny's, was the first to apply the

basic principles of botany to medicine. His pharmacological

prescriptions, like Galen's two centuries later, continued to be used unchanged until the 18th century.

In enlarging their territorial conquests, the Romans gained greater

knowledge of many rare and little-known products. Plying new

shipping routes, especially in the east, they brought back to Italy

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spices, fruit, seeds, aromatic substances and very rare plant species

that were turned to advantage in medicine, cookery, farming and

manufacturing.

From the writings of Pliny, Dioscurides and Galen, it appears that

the natural sciences and knowledge of particular substances and

materials were highly developed in their day and contributed to

progress in many areas of Roman civilisation (botany, general

education, instruction in medicine and pharmacology, hygiene,

commerce, wetland drainage, farming methods, and so on).

The decline of Greek and, later, Roman civilisation probably led

to the loss of many of the ancient world's scientific and

technological discoveries.

6- The archaeometric investigation

Research on the organic substances present in the samples taken

from the En Boqeq workshop was a much more complicated matter

than the bibliographic research.

The aim was to characterise the types of plants used in fabricating

aromatic substances and ointments at the site. Samples of process

residues were taken from rooms B, C, E, F, G and H (Fig. 5), and a

core of archaeological sediments was sampled from the main

entrance to the workshop (In 7) (Fig. 5); the core should represent

the period of time when the site was most frequented. It was thought

that the plants native to the local natural landscape and the imported

species could be identified via a series of paleopalynological

analyses.

In parallel, detailed tests and chromatographic analyses were

performed on the same samples; this made it possible to focus the

chemical investigation on the possible components of the active

principles present in the plant species identified from the

palynological spectra.

This study was based on the results obtained from an initial

screening of the texture of the sediments, the ∆pH measurements

and the quantity of organic matter. To protect the samples from

external pollution, the paleopalynological extraction was performed

with methods that prescribe the use of HCl and HF in a sterile

environment.

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To calculate absolute pollen frequencies (C. A. Accorsi, 1986) –

i.e., the number of granules per gram of sediment – a tablet of

Lycopodium was added to each sample. The average number of

pollen granules counted per level ranged from 984 to 1548. The

pollen spectra are based on the total number of granules counted (D.

Walker and Y. Pittelkow, 1981).

It should be noted that archaeological sediments from desert or

semi-desert environments often contain iron and manganese oxides,

due to the presence of a mineral known as rock varnish. For this

reason, the analyses may be much more complicated than in

traditional applications (e.g., undisturbed geological formations and

areas not settled by humans), and the results may be hard to

interpret. The findings are shown in table 3, which lists the identified

species and their respective percentages, in their order of

immigration, and also in two graphs (Fig. 9). The first refers to the

AP NAP ratio (arboreal to non arboreal plants) found by adding up

pollen from trees and grassy plants; the second shows the species

most represented (Fig.11) shows the percentage palynological graph

produced with Tilia and Tilia Graph software (E. Grimm, 2002) and

the relevant zoning (L. Orloci, 1967).

ANTHROPISATION INDICATORS - The evidence for these

factors, plotted in the central parts of the palynological graph with a

significant portion of spectra, due to the cultivation of grain and

legumes (I. Greig, 1982), produces curves with indicative trends

when, as in this case, they belong to anthropised palynological

contexts (W. Van Zeist and W. A. Caspaire, 1984). The

morphobiometric study of these pollen types was recently recast

with the aid of an image analyser (F. Foster, 1995). Automatic

counts and measurements of morphobiometric features (as proposed

by S. T. Andersen) were made for Cerealia and the other

Graminaceae. As regards the Fabaceae, meaning Vicia (vetch) and

Pisum (pea), reference was made to the parameters suggested by

P.D. Moore and J. A. Webb (1978).

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Tab. 3

Fig. 9

15

The presence of Cerealia type is evidenced by four types of

pollen:

A) Pollen from plants belonging to the Hordeum group: Hordeum

vulgare L. (cultivated barley), Triticum monococcum L. (einkorn

wheat) and certain wild species. The curve for Hordeum pollen is

steady all along the sequence.

B) Panicum pollen is present more discontinuously between levels -

54 cm and -34 cm. It comes from cultivated millet (Panicum

miliaceum L.) and from some wild species.

C) Pollens from wheat and oats, the Triticum/Avena group (Fig. 10),

are present from the level of -110 cm and become a constant

presence on the graph.

Fig. 10

D) Pollen from Fabaceae, meaning peas and vetch, is found between

levels -110 cm and -30 cm (Fig. 11), and is confined to a well-

defined part of the graph. The analytic procedures found no

evidence of contamination. The state of preservation of these

pollens is not such as to justify their attribution to a period different

from that of the rest of the characterised species, and there appeared

to be no phytogeographic reason to do so. As a result, they have

been included as contemporary with the rest of the spectra, even if

their trend can be thought a case of under-representation (A.

Horowitz, 1992) that can be associated with the ancient forms of

agriculture (W. Van Zeist, 1984).

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Fig.11

In the upper part of the graph, between levels -34 and -44 cm,

there is also a significant presence of pollen from wild rubble-loving

plants, halophytes (salt-loving) plants such as saltworts (Salsola

sp.), and non native species introduced by humans, such as grasses

(Graminaceae) and goosefoot (Chenopodiaceae) (Fig. 12). Some

varieties of the Plantaginaceae are also present; these plants are

characteristic of anthropised places because of their ability to resist

trampling (M. A. Mooney, 1983). Though wild, they are considered

anthropic indicators (J. Greig, 1982) because they are related to

human activities. The significant presence of Artemisia sp. (Fig. 13),

Salsola sp. and Taraxacum sp. (dandelion), which are found on arid

steppes, is indicative of a transition towards an arid state (G.

Nieborg and W. Van Zeist, 1990), accompanied by deterioration and

impoverishment of the soil. Acacia (Fig. 14), which is present in all

the stratigraphic units examined, can be considered another element

typical of the ancient vegetation in the Dead Sea area. It is

documented not only by a notable percentage of pollen, charcoal

and wood, but also by pods from which tannin was extracted (M.

Kislev, 1990). The types of pollen found in these samples and

repeatedly reported for other sites in the Dead Sea area (W. Van

Zeist and S. Bottema, 1991) can be considered typical components

of Saharo-Sindian environments (M. Zohary, 1973); they are

17

probably not native to the area investigated (M. Zohary, 1962), and

indicate a gradual increase in its aridity.

Figs.12, 13 and 14

TREES - In the phase represented between levels -74 cm and -103

cm, trees such as Pinus (Fig.15), Juniperus (Fig.16) and Cedrus are

present in significant percentages. They are native to the Dead Sea

area (A. Eig, 1931-32) and are reported as growing wild in

neighbouring areas (U. Barrich, 1986). In the Near East, the area

where hard pines (Pinus brutia Ten.) grow wild is Lebanon (Zohary,

1973). Pinus halepensis Miller grows wild in western Jordan

(Zohary, 1973) and near the Sea of Galilee, in Israel (U. Barrich,

1986). The Lebanese cedar (Cedrus libani A. Richard in Bory)

grows in the mountains of Lebanon (N. Liphschitz and B. Gideon,

1991) and in western Syria (M. Zohary, 1973). Juniperus phoenicea

L. has its range north of the Sinai and in the Edom area in Jordan

(M. Zohary, 1973), though significant quantities of juniper and cedar

wood have been found at the pre-dynastic site of Maadi, on the Nile

(W. Van Zeist and G. J. Roller, 1993), and a cone from an Aleppo

pine (Pinus halepensis Miller) was found at the Egyptian site

Bakchias, in SU B96/90 (A. Lentini, 1996). Wood and resin from

Pinus halepensis and Cedrus libani have been found in other

contexts in Egypt as well, but in all these cases they are thought to

be imports (A. Lucas and J. R. Harris, 1962). In 1888, W. M. F.

Petrie found Juniperus phoenicea twigs at the Graeco-Roman

necropolis of Hawara. The analytic data seem to suggest that a

remnant of the Mediterranean steppe forest had survived near the

oasis, thanks to the hot and humid climate, but all the taxa were

drastically reduced in the SUs from -54 cm to -30 cm. In an earlier

and more humid phase, this Mediterranean-type plant alliance had

18

probably managed to spread farther south than the area where it

exists today (Shokey Ibrahim Saad, 1979). The second part of the

graph shows the natural arboreal vegetation representative of a

streamside environment: willows (Salix) (Fig. 17), poplars (Populus)

and tamarisks (Tamarix) in association with water-loving plants

such as reeds (Phragmites), rushes (Juncus), bulrushes (Thypha),

sedge (Cyperus) and water-lilies (Nymphaceae), which testify to the

strong influence of hydrological features on the territory.

Figs. 15. 16 and 17

The woodland component includes Mediterranean evergreens (F. Di

Castri and H. A. Mooney, 1973) such as the evergreen or Kermes

oak (Quercus calliprinus) and other oak species (Fig. 18), olive trees

(Olea sp. fig. 19), ivy (Hedera sp.,) pistachio trees (Pistacia sp.) and

jujube trees (Zizyphus sp.,fig. 20), which were also identified in the

paleopalynological study of the Sea of Galilee (U. Barrich, 1990); as

noted above, these trees remain from an older, Mediterranean-type

phase.As regards olive trees, the morphobiometric findings did not

enable us to differentiate sharply between the cultivated variety

(Olea europea L. var. europea) and the wild variety (Olea europea

L. var. sylvestris), but the quantities of pollen found at all the

anthropised levels make cultivation the more plausible hypothesis.

Figs. 18, 19 and 20

19

7- Zoning the histograms for the En Boqeq area

Zoning palynological histograms via multivaried analysis is a

valid aid for analysing them and comparing them with the results

obtained with other methods (D. Walker and Y. Pittelkow, 1981).

Sediment analysis showed the presence of oxidised elements in the

various SUs investigated, in different percentages. These results

seem to identify both natural components and components of human

origin, which would have contributed to the growth of the deposit.

Multivaried analysis does not recognise these components, hence it

groups SUs that in reality are separated by palynological facies and

physical-chemical facies. The cluster analysis results (Figs 21 and

22) essentially agree. The parameters used to define the clusters

were 0.75 for the chord distance (L. Orloci, 1967) and 0.50 for the

Whittaker index (H. J. B. Birks and A. D. Gordon, 1985). The

distribution obtained from the botanical elements was as follows:

1) Steppe-type vegetation, with the presence of Artemisia, Ephedra

and Plantago. 2) Grassy vegetation characterised by the presence of

Cerealia and Graminaceae. 3) Hydrophytic vegetation, with the

presence of the riverside plants Populus, Salix, Tamarix and

Cyperus.4) Arboreal vegetation with a prevalence of Pinus,

Pistacia, Ziziphus, Quercus and Acacia. 5) Arboreal vegetation

evenly distributed with grassy vegetation.6) Prevalently arboreal

vegetation.

Figs. 21 and 22 - Dendogram: results of the cluster analysis applied to 1)

the d issimilarity matrix (chord distance); 2) the dissimilarity matrix

(Whittaker index

20

Based on our data, the En Boqeq site appears to have evolved into

an exposed, semi-arid environment characterised by steppe-type

vegetation, with a clear prevalence of Graminaceae, Artemisia,

Taraxacum and other Composites, the latter associated with other

grassy plants such as Plantaginaceae (plantains), Salsola,

Chenopodiaceae and various typically Saharo-Sindian Acacia

species (J. A. Cotzee, 1955-56) that were originally not native to the

area. Arboreal vegetation is present, though always in small

quantities, limited by the arid conditions and fluctuating over time.

The vegetation is fairly diversified, as witness the Mediterranean-

type trees (Pinus, Juniperus, Cedrus, Quercus, cultivated and wild

Olea, Pistacia) and plants typical of streamside environments

(Populus, Salix, Tamarix, Thypha, Juncaceae and Nymphaceae). The site became more and more anthropised, as can be seen by the

significant increase in the spontaneous anthropogenic indicators,

especially starting from level -30 cm. Subject to the limitations of

paleopalynological analysis, as described above, the evidence for

the practice of agriculture implies the cultivation of olive trees,

barley, einkorn wheat, millet and Fabaceae such as peas and fava

beans. Based on the paleopalynological evidence, the site was an

exposed environment with little tree cover and broad steppe-like

stretches. Evidence of humid areas is limited, and is probably

related to the seasonal streams flowing near the site.

8 - Residues from workshop production processes

In the 1980s, samples of what appeared to be organic matter were

taken from process residues found near artefacts in various parts of

the En Boqeq workshop (Figs. 6 and 7). These samples were

subjected to paleopalynological, chemical and physical analysis.

First, they were characterised chromatically, using the Munsell

method (Munsell Soil Color Chart, 1981); the results are shown in

table 4. Next, pollen extraction was effected with the acetolysis

method: 9 parts of (CH3CO)2O to 1 part of 98% H2SO4 (G.

Erdtman, 1943).

21

id Original position in the site Munsell Formula Color Standart Cielab Ns°of pollens

1374/22

Organic matter near the table

HUE10YR5/4 Yellowish brown 1050

1372/

20

Ash layers on the table HUE10YR3/1 Very dark gray 725

1307/

8

From the caudel yard HUE10YR5/1 Gray 810

1375/23

Level near the table HUE10YR8/6 Yellow 856

1595/

15

White layers near basin HUE10YR7/2 Light gray 786

1035 From the upper layers near

caudel

HUE2.5Y7/1 Light gray 892

1244 From the floor near the mill HUE10YR3/1 Very dark gray 1025

1373/

21

Naer the table of basin two HUE7.5YR7/2 Pinkish gray 942

1143/2

Ash layer from the caudel HUE10YR3/4 Dark yellowish brown 654

1283 From the stone near furnace HUE10YR3/1 Very dark gray 688

1776/23

Near the Eastern oven HUE10YR4/5 Very dark gray 832

1514/

16

Near the North Eastern

oven

HUE7.5YR2/0 Black 963

1371/

19

Near the first wait room HUE10YR4/1 Dark gray 871

1776/24

From the central oven HUE10YR7/3 Very pole brown 857

Table n° 4 – List of the residual ones relative at the officinalis workings to

the system of colours Munsell classification.

22

Examination of the extracted palynomorphs, which averaged 838

granules in 14 different tests, made it possible to identify multiple

morphologies of pollen, spores and airborne matter. The pollens

were found to contain pollen granules from Myrtus (Fig. 23), Laurus

(Fig. 24), Rubia (Fig.25), Papaveraceae (Fig. 26), Sambucus and

Acorus, mixed with pollens from species characterised outside the

building and attributable to the most representative biome.

Figs. 23, 24, 25 and 26

The outdoor pollens had been deposited in the indoor sediments by

climatic vectors (G. Rapp and J. A. Gifford, 1983) such as wind and

water, and by the comings and goings of humans. Small percentages

of pollen from Gypsophila sp. were also found (Tab. 5); its presence

was probably related to the tower that rose above the building.

Medicinal species were found in varying percentages in all the

samples examined. They were probably brought intentionally into

the shop; the circumstance squares with the historical sources (A.

Grilli, 1984) for the period when En Boqeq was frequented, and

indirectly confirms the widespread use of these species, which are

among the ones most often mentioned in historical texts.

Moreover, in the historical sources we find indications of the

officinal uses of certain species (Pinus, Cyperus, Oleaceae and

Artemisia) proper to the biome represented via the

paleopalynological investigations of areas outside the workshop. Oil

omphacine (pressed from olives harvested a few months before their

natural ripening season) was considered the basic ingredient in most

of the ointments and perfumes made in those times.

23

Taxa 1374/4 1372/20 1307/8 1357/23 1592/15 1035 1244

Myrtus 6.95 7.54 8.18 7.51 6.38 6.84 7.74

Laurus 4.29 3.59 8.43 8.33 7.40 7.40 4.51

Labiatae 4.38 3.23 4.96 4.93 4.59 4.60 4.70

Rubia 1.14 4.13 4.46 4.46 3.06 4.04 1.86

Artemisia 10.48 11.49 10.16 10.09 9.06 8.97 9.89

Papaveraceae 8.38 7.18 8.80 8.69 7.91 7.74 8.81

Malvaceae 9.14 9.16 7.43 7.75 6.51 7.29 8.72

Sambucus 2.00 1.80 2.73 2.93 2.81 3.36 2.74

Acorus 9.14 7.90 9.05 8.80 7.91 7.85 7.93

Cyperus 6.48 5.75 4.96 4.93 5.23 5.49 6.86

Gypsophila 8.10 7.00 6.44 6.81 9.31 9.08 8.62

Olea 11.43 13.82 10.04 9.98 14.03 11.43 11.66

Pinus 14.29 14.36 11.52 11.27 12.50 12.78 12.54

Spore 2.10 1.62 1.49 1.88 2.30 1.79 1.86

Table n° 5 - List of the species with the relative percentages, recovered

inside of the residual ones of the workings on the workshop.

The presence or absence of pollen from other officinal species not

native to the area in question but mentioned in the literature as among

the most widely used (Cistus, Iris, Rosaceae, Trigonella foenum

graecum, Verbena officinalis, and so on) may depend on the ancient

procedures for processing certain parts or sections of the plants used

in the preparation of ointments, perfumes and other therapeutic

substances. The possibility that pollen from non-native species may

have been dispersed in the shop may depend on the places these

species came from, and may have been determined by a selection of

plant parts or sections made at their place of origin to prepare them

24

for shipment over long distances. Pliny (XII: 20) reports such

circumstances for Amomum zingiber L. and Amomum curcuma J.

(turmeric), imported from India, and for Ocotea caudata (an essential

ingredient in "Royal Ointment"), of which only the woody part was

used (G. Donato and E. Donato, 1987), in a mixture with local

products (oil omphacine, pine resin, myrtle flowers, and the leaves

and primary branches of bay laurel).

Conclusions - The results of the paleopalynological analyses of

fourteen samples from the En Boqeq workshop enable us to formulate

some brief botanical considerations on the seasonal nature of the

shop's production processes and on the officinal species that were

characterised. The large presence of pollen from Pinus, Cyperus,

Oleaceae and Artemisia is significant. These species, which are

considered officinal (G. Donato, M. E. Branca and A. Rallo, 1975)

and are among the best known and most characteristic of the natural

landscape at En Boqeq, produce especially large amounts of pollen.

Their pollen output peaks in late spring (Fig. 2), and the pollen is

spread throughout the environment by climatic and anthropogenic

vectors whose action is abetted by the morphological features of the

pollen granules produced by these species (P. D. Moore and J. A.

Webb, 1978). The attempt to use the same method to document pollen

granules from other officinal plants mentioned in the literature was

one of the first directions taken in multidisciplinary scientific

investigation. Indeed, the significant presence of granules from

Myrtus (fig.27), Laurus, Labiatae (fig. 26), Rubia, Malvaceae (fig.

29), Papaveraceae (fig. 30), Sambucus and Acorus – all of them

species from different Mediterranean environments – confirmed the

findings from the historical research conducted in parallel. This

method, which represented a first approach to the definition of the

basic features of the ancient economy of the settlement studied in the

early 1980s, is also a valid tool for gaining knowledge of the basic

elements of the ancient natural landscape in the En Boqeq area.

9 - The chemical investigation

The chemical investigation of the samples (Tab. 5) taken in the En

Boqeq workshop (Fig. 5) was conducted in 1982-84 with methods and

25

equipment which at the time were considered among the most

reliable. Observed at first under low magnification, the samples

appeared very dark, and evidently contained a wealth of plant matter

(Figs. 6 and 7). The first analysis aimed to determine the percentage

of organic matter via the calcination-loss method (P. Duchaufour,

1970); it was found to be 8%, far above the average data reported in

the archaeometric literature. Considering that olive oil, according to

the bibliographic sources, was one of the ingredients used most

widely in ancient times in the production of perfumes and therapeutic

substances, and taking account of the findings from the palynological

analyses of the same samples, which showed a significant presence of

Oleaceae pollen in all the spectra, the next step was to test for olive

oil via the Bellier reaction (which prescribes extraction with

petroleum ether from a sample of known quantity, removal of the

supernatant and addition of fluoroglucine and HNO3). At the end of

the reaction, the solution had the red colour typical of olive oil. To

confirm this first positive result and to characterise in greater detail

the presence of olive oil in these samples, it was decided to follow up

with two complementary analytic methods. The first was based on the

atomic absorption of the mineral fraction of olive oil (the

unsaponifiable fraction), as represented by the salts of metals such as

Fe, Se, Cu, Mn and Zn, in which olive oil is particularly rich; the

mineral fraction is the subject of great interest in the chemical and

archaeometric literature. In the second, conducted in parallel with the

first, a series of high pressure liquid chromatography (HPLC) tests

were run to seek the kinds of hydrocarbons that are produced during

synthesis of the fatty acids contained in olive oil.

10 - The heavy metals investigations

In the 1980s, atomic absorption spectrometry (AAS) was an

essential analytic procedure in any chemical investigation, because of

its high precision in determining and measuring trace metals.

In AAS, the wavelength interval is determined by the radiation

source, the components of the optical path and the detector. The

spectrum range used in this study was between 852.1 nm, the

wavelength of cesium, and 193.7 nm, the wavelength of arsenic (B.

Welz and M. Sperling, 1989). The AAS spectrometer operates in the

range of UV-vis spectrophotometers. The radiation sources used in

26

the chemical characterisation of the samples of process residues from

En Boqeq generate discrete beams capable of emitting, with the use of

hollow cathode lamps (HCLs), a single spectral line for each element

analysed.

The qualitative and quantitative tests were slanted towards certain

trace metals (A. Tessier, P. G. C. Campbell and M. Bisson, 1979) –

Fe, Se, Cu, Mn and Zn, expressed in ppm – present in the

unsaponifiable fraction of olive oil. Some of these trace metals, like

Fe and Cu, are transition elements that operate in biochemical

synthesis as catalysts for the process of stabilising olive oil against

oxidation both at room temperature and in heat treatments. According

to the archaeometric literature (A. M. Pollard and C. Heron, 1996),

under certain preservation conditions these elements persist in

archaeological sediments.

The samples (Table 7) that proved richest in organic matter and

positive in the Bellier test (P. J. Potts, 1997) were made soluble via

treatment with hot HF and HNO3; the teflon crucibles containing the

samples were placed in a 70° C. sand bath. The reference curves for

the individual elements analysed were obtained from certified AAS

standards.

The current reference sample, which came from a selection of oil

omphacine pressed from olives harvested in central Italy in the month

of August, was analysed in undiluted form.

The results obtained with AAS and the addition method (R. J. W.

McLaughlin, 1977) confirmed the presence of these elements (Tab.

7), though at the beginning of this experimental procedure there had

been much doubt as to the validity of an archaeometric

parametrisation established with materials from a long period of time.

The quantities found were probably influenced by the state of

preservation of the samples, by their different geographic origins, by

the geomorphological diversity of the deposits and by instrumental

conditions during the analyses, but they represent one of the first

actual attempts to characterise organic residue from a specific

archaeological context. Considering the amount of time that has gone by since these first

methodological experiences, the identification of archaeometric

parameters that can be verified in organic materials via diagnostic

procedures is certainly one of the most important achievements of the

27

late Professor Giuseppe Donato, the promoter of these first

methodologically rigorous investigations.

ID Cu ppm Fe ppm Mn ppm Zn ppm Se ppm

1594/16 1.35 1.28 1.80 1.02 0.96

1372/20 1.10 1.28 1.75 1.00 0.56

1371/19 1.45 1.25 1.76 1.15 0.88

1776/24 1.32 1.22 1.70 1.09 0.80

1373/21 0.98 1.22 1.62 1.00 0.63

Table n° 7: Average of the eight readings carried out via AAS for every

single element of the analyzed champions. ppm = parts per million.

11- The Chromatography investigation

To verify the analysis protocol, a sample of commercial olive oil

certified by the Spoleto branch of the Experimental Institute for Olive

Cultivation was prepared for chromatographic analysis in the same

way as the archaeological samples (the chromatographic investigation

was conducted in collaboration with the Chromatography Institute of

the Italian National Research Council – Rome 1 Research Area).

HPLC, a highly innovative method in the 1980s, made it possible to

separate, purify, identify and quantify various compounds in a

mixture (the mobile phase) by exploiting their different speeds

towards a stationary phase (M. Nardelli, 1978). All the samples

examined were desalted and treated with methylene chloride (E.

Stahl, 1969), then transferred (through an injection hole) into a layer

of inert material positioned at the start of the chromatographic

column. A traditional detector (IR/UV-vis mass spectrometer) and a

computer were connected to the end of the column to enable

continuous monitoring of the different analytic phases.

Very high pressure was applied at the start of the column, to enable

the liquid in the mobile phase to flow, avoiding problems of

28

longitudinal deviation (lengthwise movements of the mobile phase)

and alternate paths, and maintaining the speed of elution (passage of

the mobile phase through the column) constant and controlled until

the individual differentiated compounds reached the stationary phase.

This method is speedy, requires only very small quantities

(microlitres) of material, and gives highly precise results.

The results obtained from the certified commercial sample and the

archaeological samples were comparable, and were characterised by

the presence of squalene in very similar quantities. The two

chromatograms obtained were compared with one of the first

databases published by the U.S. National Institutes of Health and the

U.S. Environmental Protection Agency for searches in comparative

libraries, and in both cases the diagnosis was squalene, a triterpene

whose formula is C30H48. This is a complex lipid found in large

quantities in shark liver (whence its name, from the Latin squalus,

shark), and also in human sebum (around 12%). Olive oil contains a

very high percentage (400 mg. per 100 gr.), more than any other kind

of oil. Its concentration in olive oil is higher than that of phenols, so

even very small levels can be a significant marker. The same

methodologies were used to characterise samples of process residues

selected in various rooms in the En Boqeq shop. The most

representative compounds (active ingredients), and the ones that could

be safely assigned were mirtenol (from Myrtus sp.), calamone (Acorus

sp.), pinene and silvestrene (Pinus sp. and Laurus sp.), and

trigonelline (Trigonella foenum graecum). Compounds such as

quercitine, eugenol, geraniol and linalol, which are harder to assign

because they are present in more than one species, were differentiated

several times during this analytic cycle.

12 - Reconstruction of fragrant substances used in classical times.

In the preliminary studies aimed at reconstructing ancient fragrant

substances, the team formed at the National Research Council's

Institute of Technologies Applied to Cultural Heritage (CNR-ITABC)

focussed on the period between the first century B.C. and the first

century A.D. The researchers succeeded in establishing the natural

sources of the basic plant species used to extract fragrant substances,

which were brought to Italy from the Middle East, India and other

parts of Asia, Scythia (now southern Russia), and Mediterranean

lands such as Egypt, Syria and Cyprus. After tracing officinal species

29

that ripen in different seasons back to the areas in which they were

harvested (not without difficulty, because their names changed over

time), the team conducted further studies to determine the best way to

obtain substances identical to the original ones described in the

historical sources. Ruling out modern equipment and materials, the

researchers proceeded in the laboratory according to the canons of

experimental archaeology (G. Donato, W. Hensel and S. Tabaczynski,

1986), using the ancient methods of officinal pharmacology and

material from plants with different natural ripening seasons. From

among the best-known methods, the team chose steeping.

Petals, roots, teguments, pulp, pieces of flowers and leaves were

selected from the species in question and put to steep in non-acidic

olive oil (known to the ancients as oil omphacine) pressed from

unripe olives harvested in central Italy in the month of August. After

steeping at length at medium temperature, the plant parts were

strained out. The dense liquid thus obtained was then mixed with

other products obtained via a similar procedure to create the scented

ointments described by Pliny and Dioscurides (sometimes the

different morphological parts of a species contain different oils,

because of variations in the concentrations of the different terpenes).

In another method used to steep flowers and leaves, they are first

pressed to make the oil-bearing cells break, then put to steep in warm

vegetable oil, which absorbs their essence. The process is repeated

until a concentrated substance has been obtained.

Further technological evolution envisages applying a third method for

the extraction of essences, one that was widely used in certain

historical periods (the early Roman Empire). It was an intermediate

form of steam distillation, without a metal worm, and is documented

by certain types of Egyptian and Cypriot pottery (M. R. Belgiorno,

2004). This method exploits the high volatility of essential oils and

their nearly universal insolubility in water. Depending on the density

of the oil, it will either float on water or precipitate after condensation.

The water that circulates during the process becomes impregnated

with the scent of the plant matter being distilled, giving rise to useful

by-products such as "rose water," a generic term initially used to

denote essences extracted for perfumery and fumigation.

There are various types of scents, initial or conclusive, fleeting or

longer-lasting, intermediate or basic, substantial ones that last several

30

days, fine scents and scents with high molecular weights and high

boiling points, which evaporate very slowly.

AROMATIC AND THERAPEUTIC SUBSTANCES

FROM THE PREHISTORIC SITE OF PYRGOS

MAVRORAKI (CYPRUS): PRELIMINARY

CHEMICAL-TOXICOLOGICAL INVESTIGATION

Our archaeometric investigation (begun during the 2003-2007

archaeological excavations) aimed to separate out certain apparently

organic-resinous sediments. These sediments (Stratigraphic Units

G7L5, J5L8, J7L2, J7L6, F8L4, G7, G7L3, G7/8, G9, G9L4 Palette

H1044) implied particular preservation conditions; in fact, they were

found in sealed levels composed mainly of sand and fine mud.

The areas we investigated contain sediments and residues from two

large courtyards, two bronze-working shops, an oil-press area with jar-

storage space and (in the north-east corner) a workshop used for the

production of aromatic and therapeutic essences, two textile workshops

and a winery.

1-Materials and methods .

The investigation used several colour-test methods generally reported

in the chemical-toxicological literature (the Halphen-Grimaldi method,

the Bloor mixture, the Liebermann, Marquis, Bellier, Chen, Vitali,

Bechi and McNally reactions and toxicological tests). These methods

are based on dissolving residues extracted from archaeological

sediments in acidified or alkalinised solvents, in order to trigger, with

an appropriate reagent, the development of a specific colour that

narrows the analytic field; in the end, the unknown substance can be

identified by a specific reaction. In certain circumstances, we used

chloroform acidified with HCl to extract alkaloids that had been salified

in the chloroform phase. The extreme sensitivity of these reactions

makes it possible to work with very small quantities of archaeological

sediments.

31

PY03H5L6, was extracted from a loom weight, using chloroform. It

was found to contain exclusively turpentine through colorimetric tests

(chloroform + HCl) (M. Feigi, 1989). The solution assumed a hyaline-

yellow color in the superior layer and no color in the inferior. The

turpentine was obtained by boiling some resin, which itself was

obtained by cutting the trunk of the Pistacia terbinthus (turpentine of

Cyprus or of Chio), a typical phytocenosis of Cyprus (R. R. Riedel,

1991). The turpentine had always been used in the production of

resinated wines (B. Bruni, 1932). The production process consists of

boiling the resin in water, cooling it and then filtering it in filters made

from a woven vegetal material. The result is the thickening of the resin,

which is then scented with fennel (M. Fregoni, 1991). The essence can

be mixed with other perfumes or used for fumigation.

PY03 sample 3, the analytical test was done with the Halphen-Grimaldi

method (Bromine dissolved in Chloroform) through the specific

reaction of sylverstrene (acetic anhydride + H2SO4).

The resin is secreted by coniferous wood containing pinene,

sylverstrene, and bornile acetate. It is used in aromatic balsamic baths

and fumigation due to its well-known antiseptic property (G. Luis,

1969).

Test alcohol + HCl diluted, and then progressively more

concentrated. Subsequently the presence of bergamot was further

confirmed with the Halphen-Grimaldi method (W.R.Biers, R. and

P.E.McGovern, 1990).

Citrus bergamia, the fruit is grated onto a vegetal sponge (luffa).

When the sponge is saturated, it is squeezed, and the liquid obtained is

filtered. The feculent residue is boiled to obtain low-grade bergamot

oil (R. Benigni, C. Capra and P.E. Cattorini, 1997). This method was

applied for essences derived from fruits and soft rinds.

PY 03 J6L5 Alabastron. The three essences were extracted with

Bloor’s mixture (2 alcohol + 1 ether). During the extraction, a red oil

emission came from the alabastron pores, a typical indication of

coriander (Fig.27). The essences were then color tested (F. Mari, 1986)

with Iron chloride in concentrated H2SO4 (Coriandrum) and diluted

alcohol + HCl, which was progressively, concentrated (Laurus). The

presence of turpentine was confirmed through a chloroform + HCl test.

32

Essence of Laurus and Coriandrum, like many other essences, do not

have a particular perfume when they are concentrated. When diluted

with turpentine or other solvents, however, they acquire particular and

long-lasting aromas. The concentrated essences were often conserved

for long periods of time because oxygenation forms aldehyde and

ketons and the amount of perfume increases (F. Capasso and G.

Grandolini, 1998). The aging also creates dimers, trimers, polymers,

and polyphenols.

Fig. 27

PY03 sample 4. The residues taken from the bottom of the container

were treated with alcohol acidified with diluted HCl, using heat (R.

Benigni, C. Capra and P.E. Cattorini, 1997). Color tests (choloroform +

HCl) were done to detect the presence of Amygdalus communis L. var.

Amara (ether + iodine) and Myrtus communis L.. Bromine dissolved in

chloroform was used to detect the presence of Petroselinum sativum

terpene and turpentine. The essences of Myrtus and Petroselium were

extracted with the enfleurage method and diluted with turpentine (M.

Pedretti, 1997). Amygdalus oil can be made two ways: bitter or sweet

oil. Bitter oil is obtained by boiling minced almonds in water. The oil is

emulsified in boiling water and cooled to separate the substances. Sweet

oil comes from soaking minced almonds along with rye flour to

separate the bitter, poisonous component from the essence.

Subsequently, the essence is separated from the unusable components

through defecation of lime. This technique was applied to flowers,

33

leaves and volatile essences (M. Pedretti, 1997 – C. Piccioli, G. Scala

and A. Rizzo, 1996). The enfleurage method, still used in some Asian

countries, uses a property quite evident in olive oil (and to a certain

degree, in other oils and animal fats) to absorb volatile terpenes from

air. This method consists of imbibing cotton gauze with oil and then

putting the product in wooden containers. These containers are piled up

and put in a closed environment. The vegetal material to be treated is

separated (petals, tubers, bark, and so on) from the unusable parts, and

also put into the wooden containers. The oil captures the essence

contained in the vegetal material, and the gauze is then pressed to

extract the scented oil (G. Donato, 1984).

PY 03 G7L5. The sediments taken from the interior of a crater (Py 03

– G7L5), suspected to have conserved therapeutic substances, were

treated with the standard method for the extraction of alkaloids

(alcohol acidified with H2SO4 under heat). After cooling, some drops

of formic aldehyde were added to the extract (Marquis reaction),

demonstrating the typical yellow colour of the Narcotine and

Cotartine (V. Paolini 1947) found in opium (Papaver somniferum L.).

We independently confirmed the results obtained, using Liebermans

reaction (concentrated HNO3). This reaction evidenced the phenol

groups specific to morphine and maconic acid, both of which are

abundant in raw opium (P. Marfori and A. Putti, 1934).

Sediments taken from the inside of an abraded piece of pottery found

in pit area 6 of stratigraphic unit PY03 were treated with chloroform,

according to the standard method for complex extractions. The first test

was performed with ammonium molybdate and a 20% solution of

H2SO4; the reaction produced a yellow colour on the surface and dirty

yellow on the bottom. The dirty yellow revealed the presence of the

typical antioxidants in rosmarinic acid (from Rosmarinus officinalis L.).

Colour tests (ether + iodine) were then performed; these produced an

orange colour and the colourless precipitate characteristic of active

ingredients such as anethol, limonene and carvone (M. Pedretti, 1983)

contained in preparations based on green anise (Pimpinella anisum L.)

and star anise (Illicium verum Hooker). The presence of active

ingredients characteristic of anise was confirmed via tests of the initial

precipitates, made with a series of increasingly concentrated solutions

of H2SO4 that led to the development of the white colour typical of

34

these active ingredients. The elements analysed in this first phase of the

study are not such as to enable us to determine without question the

origin of these active ingredients, because they are found in both

species of anise. The green anise cultivated in the Mediterranean area

was probably imported by the Greeks from the Orient (Pliny XX: 191-

195 reports what he read on the therapeutic uses of anise in a long series

of Greek authors, and tells us that Cretan anise was the most prized,

followed by the Egyptian). Ancient sources suggested many medicinal

applications of anise. Two of the most widely used remedies were

fumes of burnt anise for headache and crushed anise root combined

with olive oil for earache. Sometimes the poisonous fruits of hemlock

was mistaken for anise fruits (A. Lentini and G. Scala, 2004), with

unfortunate results.

-OILY SUBSTANCES.

PY04 F8 L4 – In the test for the presence of sterols, part of the

sediments was treated with chloroform acidified with H2SO4 and an

addition of (CH3CO)2. The outcome was negative. Next, another part of

the material was treated with NH2OH + CuSO4 (a few grains) + H2O2 (1

or 2 drops) ( G. Scala, 2001), to discover whether any type of oil or

resin was present. At the end of the reaction, the result was positive for

ebullition (signifying the presence of conifer resin and/or

polysaccharides). In the final test for the presence of resin, part of the

sediments was hot-extracted with chloroform, fluoroglucine and a small

quantity of HCl, which resulted in was the development of a red colour

typical of resinous substances (R. Riedel, 1991).

PYJ7L5 – Bowl 2. The residue in the bowl contained a certain amount

of dark yellow matter, apparently organic. It consisted of a more or less

homogeneous agglomerate containing small bits of dry organic matter

whose fractured surfaces were concave and porous, mixed with sand

and limestone. Examination under the optical microscope, at different

enlargements, revealed the presence of bits of insects (wings, reticular

tissues and fragments of legs and antennae - fig. 28) and the presence of

starches.

35

Fig. 28 and 29

Of the various toxicological tests performed, the only one that had a

positive outcome was the Chen (CuSo4 + NaOH 1M – M. Fejgi., 1989),

which resulted in a shift towards the very intense turquoise blue specific

to certain derivatives of ephedrine, and the formation of a precipitate.

According to the chemical-taxonomic literature (V. Villavecchia, 1931),

some resins from the Greek islands, Syria and the Near East turn green

when treated with ammonia; the bowl residue produced exactly this

reaction (Fig. 29). This type of resin was usually obtained by cutting

into the roots of scammony plants (Convolvulus scammonia). A

powerful cathartic, it is still present in some official drug indexes and is

sold under the name "Black Aleppo Scammony" (V. Villavecchia,

1931). The discovery of this compound (scammony + ephedrine) recalls

a preparation that worked well against constipation and other intestinal

disorders (A. Sabah, 1935).

PY03 G7L3 - Amphora. The residue was treated with ethyl alcohol and

acidified with H2SO4. The supernatant (the clear fluid above the

sedimentary precipitate) turned brown, indicating the presence of

methylpentynol, an alkaloid with tranquillising and soporific properties

that is contained in Valeriana officinalis L. and certain Verbenaceae (P.

Zangheri, 1976). Next, the solution was placed in a crucible to speed

evaporation of the alcohol, and the residue was treated with the Marquis

method, adding formaldehyde and H2SO4 . This produced the intense

brown colour that indicates the presence of alkaloids (the painkillers

ethorphine and oripavine) contained in the seed capsule of the opium

poppy (Papaver somniferum). The second fraction of the residue, tested

with the Lieberman reaction (H2SO4 + KNO2), turned pale green,

36

denoting the presence of colchicine, an alkoloid contained in meadow

saffron (Colchicum autumnale) (A. Leung and S. Foster, 2000), which

has antirheumatic, anti-gout, diuretic, anti-neuralgic, vermifuge and

sedative properties.

- PY05 G9L4, vase 6. The concretions were extracted with ethyl

alcohol, and after a few minutes, the supernatant was siphoned off. The

solution was then treated with diluted and increasingly concentrated

HCl, which turned it a brown colour corresponding to essence of

lavender (Lavandula sp.). A new extraction was then made with

chloroform, and after a few minutes concentrated HCl was added to the

supernatant. The cloudy liquid thus obtained was then shaken for a few

minutes. Two layers formed; the upper one was tinted lemon yellow

(turpentine) and the lower one remained colourless.

Next, a test made with H2SO4 and ammonium molybdate produced

an abundant azure precipitate typical of quinoline bases. This finding

was confirmed by an HCl + FeCl3 test, which produced the green colour

specific to quinoline derivatives (E. Mari, Tossicologia forense, p. 454).

These bases quinoline C9H7N ( , -benzopyridine) and isoquinoline

C9H6OHN – (hydroxyquinoline and , -benzopyridine) are present in

coal, from which they are extracted with terpenes such as turpentine and

other essences (lavender, as in this sample), and in animal oils obtained

by heating the solid parts of horns and hoofs (Dippel oil). Derivatives of

quinoline bases are present today in an antiseptic ointment called

Lorcoten Vioformio; other drugs containing quinoline derivatives, for

instance Kaierina, Loretina and Analgene, went out of production a few

years ago.

PYJ5L8, internal bowl. The sediments were treated with the Marquis

reaction (H2SO4 + formaldehyde), and developed the hyaline-yellow

colour typical of ephedrine derivatives (F. Capasso and G. Grandolini,

1998). Next, the Chen reaction (CuSO4 + NaOH 1M was used to check

for the presence of products originated by ephedrine. The result was an

azure colour (V. Paolini, 1947) that confirmed the presence of this

alkaloid. The preparation, treated with a 20% solution of H2SO4 and

examined under the microscope, was seen to contain single crystalline

structures (bars) and agglomerates (bars and needles) ( Figs. 30 and 31).

37

These are typical of toxicological substances similar to ephedrine

sulphate.

Figs. 30 and 31

This alkaloid, extracted from Ephedra, was commonly used in medicine

to treat respiratory and cardiovascular diseases (A. Leung and S. Foster,

2000).

PY04 G9 – Ewer. The Liebermann reaction (H2SO4 + KNO2) produced

an intense yellow colour corresponding to polyphenols or flavonoids

and their esters, which have an aromatic core. They are derived from

quercetin, a substance commonly present in the composition of

propolis, a yellowish, aromatic, resinous substance that bees gather in

the spring, especially to line the inside of their hives. In ancient times, it

was used (sometimes in the form of an ointment) – to treat disorders of

the respiratory, digestive and urinary systems. The Egyptians used it as

an antioxidant in their mummification process (A. Lucas and J.R.

Harris, 19624).

PY04 G9L4 – Palette 1.1, 1.3 and 1.6. Three samples were analysed

from cavities 1, 3 and 6 of the 18-cuppeled multiple limestone mortar.

The three residues were analysed first with the Marquis reaction, then

with the Liebermann reaction, to cross-check the results. All three

yielded a yellowish green colour specific to colchicine, a natural

alkaloid present in the seeds and bulbs of Colchicum autumnale L..

Among its known properties are its effectiveness in stimulating the

excretion of uric acid and its analgesic and anti-inflammatory action.

Because of these characteristics, colchicine was used in the past (M.

Pedretti, 1997) to treat and prevent gout attacks. Over time, its

38

therapeutic applications were narrowed down because of its notable

toxicity, even in small doses, for the digestive system.

PY04 G7-8 – Sample 2.6 Palette The sediments sampled from cavity 6

of the multiple mortar were extracted with chloroform and tested by

various methods for the presence of medicinal or oily ingredients. All

the results were negative. In a second series of analyses, the H2SO4 +

ammonium molybdate test produced a green colour which over 24

hours turned to azure, denoting the presence of quinoline or one of its

derivatives. To check for this compound, another test was run with HCl

+ FeCl3, which produced the green colour specific to quinoline

derivatives (F. Mari, 1986).

PY01 J7L2. The residues were extracted in alcohol and acidified with

diluted HCl, which produced a pale yellow colour (fig. 40). Next, as

increasingly concentrated HCl was added, the initial colour turned to

the green that is characteristic of turpentine (Pistacia terebinthus L.).

Fig. 32

PY03-G7 - Bowl. The sediments were analysed with formaldehyde +

H2SO4. After a few hours, the suspension thus obtained had turned to a

yellow tint that signals the possible presence of hydroxyephedrine or

colchicine . Colour tests were then performed (D. De Wied, W. De Jong

39

and A. Witter, 1995) to further differentiate the components. The

H2SO4 + KNO2 reaction was negative for colchicine, hence the sample

contained only alkaloids present in ephedrine.

PY02 J6I6. The deposits were treated with the standard method for

extracting alkaloids: HCl - acidified chloroform (F. Feigl, 1989). After

cooling, the treated substance had turned to a green proper to azulene, a

compound found in camomile (A. Pedretti, 1997). For further

confirmation of the compound, a few drops of a solution composed of

ether + iodine (the Marquis reaction) were added to the extract (R.

Benigni, C. Capra and P.E. Cattorini, 1962-64). This produced a colour

change to orange (Fig. 33) and a colourless precipitate specific to

azulene-based essences. The camomile that grows wild in the

Mediterranean region (P. Zangheri, 1976) is known in the

pharmacopoeia for various properties. Pliny described its presence on

various Mediterranean islands and classified it as an antispasmodic. The

name is commonly applied to many members of the Compositae family,

such as Anthemis nobilis, Anthemis cotula, Anthemis tinctoria and

Matricaria chamomilla.

Fig. 33

PY02 J5B - Pit scents area. The sediments were extracted with

chloroform, then a few drops of concentrated HCl were added to the

supernatant. After being shaken, the liquid separated into two layers,

the lower one colourless and the upper one a pale hyaline green, the

40

specific reaction for essence of turpentine. A second extraction with

alcohol plus a small amount of HCl 0.5M turned the preparation to a

pale pink. Adding a few more drops of concentrated HCl produced a

new colourless substance, indirectly confirming the presence of

turpentine. Another test with phenol + H2SO4 revealed the presence of

pine (Pinus sp.) resin, because the colour changed from green to violet.

The turpentine characterised by these tests was probably extracted from

pine resin.

CONCLUSIONS. The results of the chemical-toxicological analyses of

the Pyrgos residues (Fig. 36) sampled from different types of artefacts

found in adjoining areas enable us to formulate some brief

considerations on the natural botanical landscape in ancient times and

on the seasonal nature of the production of medicinal and fragrant

preparations (Tab. 8).

Fig. 33

The substances we characterised, which had been obtained from

medicinal plant species growing in the Mediterranean region, are

numerically significant. Many of the medicinal ingredients

characterised in the chemical investigation came from species

documented at the site through archaeobotanical studies that began

during the 2004 dig. A number of plant macro-vestiges have been found

41

during the work still in progress, including olive pits (Fig. 37) and

coriander seeds (Fig. 38). Paleopalynological analyses of the

archaeological levels from -180 to -230 cm in SU H5L6 document

pollen from Pinus, Cedrus, Pistacia, Amygadalus, Myrtus, Laurus,

Olea, Rosmarinus (Fig. 39), Colchium and Papaver in significant

quantities for the time period. Irano-Turanic conifers were one of the

most characteristic features of the vegetation on Cyprus (M. Zohary,

1973) in ancient times. They were present not only on the slopes of the

Trodos mountains, between 500 and 1000 meters above sea level, but

also on rocky ground and in general in places where other kinds of trees

would have found it harder to survive. Remnants of the ancient

vegetation can still be seen near Paphos and along the middle stretch of

the Pyrgos river, near the old asbestos mines (Dimmata).

Figs 37, 38 and 39

The plant species typical of the Mediterranean (F. Di Castri and H.A.

Mooney, 1973), such as Pistacia, Olea, Amygdalus, Myrtus, Laurus and

Rosmarinus, are still plentiful in the area covered by these

investigations, in the native phytocenoses. Among the ones considered

medicinal, Valeriana officinalis grows wild in glades at medium-high

altitudes in the Trodos mountains, and Colchicum autumnale – one of

the medicinal species best known and most sung in the traditions of

Mediterranean populations – is present in the mountain belt. Lavandula

sp., Matricaria sp., Petroselinum sp. and Papaver sp., which grow wild

in the Mediterranean basin (P. Zangheri, 1976), are now typical of

anthropised areas, growing at the edges of farmland and other places

where human activities are present.

It is still not clear whether there is an effective correspondence

between oil of bergamot – which contains mono and sesquiterpenic

hydrocarbons and their nonvolatile derivatives, which contain

cumarines and psoralenes and Citrus bergamia. The little

42

documentation existing on the origin of this species – located

generically between the eastern Mediterranean and the subtropical east

– makes its classification very complex. Based on recent genetic

applications (R. Herrero and M.J. Asins, 1996), there exist only three

species of Citrus; all the other members of the genus that used to be

considered species or subspecies should actually be considered natural

hybrids. Some of the most common active ingredients we identified

were known since ancient times, and were used both in simple

medicinal preparations and in initial crop treatments. Almost certainly,

the original names of the medicinal plant species changed over time and

place. Certain substances, for instance ephedrine, valerian, colchicine,

and opium and its derivatives,, are still present in official

pharmacopoeias. Others, like certain conifer resins and oxyquinoline,

were replaced only recently by synthetic drugs or more effective

derivatives. Our preliminary characterisation of these substances shows

how advanced the knowledge of medicinal species and their therapeutic

properties was in antiquity.

43

ID Square Layer Substance

PY01 J7L2 Turpentine (Pistacia terebinthus L.). Turpentine of

Cyprus or of Chios.

PY02 J6L6 Azulene-based essences (Matricaria chamomilla).

PY03 G7L3 Amphora Methylpentynol (Valeriana officinalis L.), Ethorphine

and Oripavine (Papaver somniferum L.), Colchicine

(Colchicum autunnale).

PY03 G7 Medium Bowl Alkaloids present in ephedrine (Ephedra sp.).

PY03 H5L6 Sample 1 Turpentine (Pistacia terebinthus L.). Turpentine of

Cyprus or of Chios.

PY03 H5L6 Sample 2 Pinene, Sylvestrene and bornile acetate (Coniferae),

Bergamot (Citrus bergamia).

PY03 J6L5 Alabastron A red oil, typical of coriander (Coriandrum sativum),

Essence of Laurel (Laurus sp.) and Turpentine

(Pistacia terebinthus L.).

P Y03 Sample 3 Pinene, sylvestrene and bornile acetate (Pinus sp.).

PY03 Sample 4 Bitter almonds (Amygdalus communis L. var. Amara),

Essence of Myrtle (Myrtus communis L.), Terpene of

parsley (Petroselinum sativum) Turpentine (Pistacia

terebinthus L.).

PY03 G7L5 Krater

Narcotine and cotarnine found in opium (Papaver

somniferum L.) presence of phenol groups specific to

morphine and maconic acid.

PY03 Pits Area Rosmarinic acid (Rosmarinus officinalis L.) Anethol,

Limonene and Carvone Green anise (Pimpinella

anisum L.) and Star anise (Illicium verum Hooker).

PY04 F8L4 Oily

Substances

Presence of conifer resin and/or polysaccharides.

PY04 J7L5 Bowl 2 Ephedrine and scammony (Convolvulus scammonia

L.). "Black Aleppo Scammony"

44

PY04 G9 Ewer Flavonoids and their esters, quercetin (Propolis ).

PY04 J5L8 Bowl

Interior

Ephedrine derivatives (Ephedra sp.).

PY04 G9L4 Palette 1.1 Alkaloid of colchicine (Colchicum autumnale L).

PY04 G9L4 Palette 1.3 Alkaloid of colchicine (Colchicum autumnale L).

PY04 G9L4 Palette 1.6 Alkaloid of colchicine (Colchicum autumnale L).

PY04 G7-8 Palette 2.6 Quinoline derivatives (animali oils)

PY04 G9 Rubble Pile

on Floor

Animal sterols (Cholesterol).

PY05 G9L7

Metalworking

Area

Hydrocarbons contained in olive oil (Olea europea L.

var. europea).

PY02 Perfumery

Area

The turpentine characterised by these tests was

probably extracted from pine resin.

PY05 G9L4 Vase 6,

Concretions

Quinoline and isoquinoline, are present in coal, from

which they are extracted with terpenes such as

turpentine and other essences. Essence of lavender

(Lavandula spiga L.),

Table n° 8 - Resulted of toxicological and chemical investigation.

45

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