i n d u s t r i a l c r o p s a n d p r o d u c t s 2 9 ( 2 0 0 9 ) 171–176

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Steam distillation modeling for essential

oil extraction process

E. Cassel a,∗ , R.M.F. Vargas a , N. Martinez b , D. Lorenzo b , E. Dellacassa b

aLaboratório de Operações Unitárias, Engineering Faculty, PUCRS, Av. Ipiranga 6681, CEP 90619-900, Porto Alegre, RS, Brazil
bCátedra de Farmacognosia y Productos Naturales, Facultad de Química, Universidad de la Republica,
Avda. General Flores 2124, CP-11800 Montevideo, Uruguay

a r t i c l e i n f o a b s t r a c t

Article history: A mathematical model was evaluated to predict the essential oil recovery by steam distilla-
Received 21 December 2007 tion of rosemary (Rosmarinus officinalis L.), basil (Ocimum basilicum L.), and lavender (Lavandula
Received in revised form dentata L.). The aim of the work was to obtain yield experimental data to compare with a
11 March 2008 mathematical model used in the simulation of essential oils extraction by steam distilla-
Accepted 24 April 2008 tion. The extraction model is based on single plate particle description on mass transfer.
This model requires only one adjustable parameter, effective diffusion coefficient (D), to
predict the essential oil yield experimental curves.
Keywords: © 2008 Elsevier B.V. All rights reserved.
Labiatae
Rosemary
Basil
Lavender
Distillation
Mathematical model

1. Introduction
A large number of plant species contain volatile chemi-
cal compounds which can be extracted as an essential oil.
Different methods are used to separate these oils from
the various plant materials. Although it seems relatively
simple to isolate such oils, the composition of oil may
vary to a large extent depending on the extraction method
used. The advantages and disadvantages of some methods
such as hydrodistillation, solvent extraction, simultaneous
distillation-extraction, supercritical carbon dioxide extraction
and the use of microwave ovens have been discussed in exten-
sion (Scheffer, 1993). Cassel and Vargas (2006) modeled the
extraction of Cymbopogon winterianus essential oil using a dif-
fusional model at laboratorial scale allowing a good prevision
on industrial scale. The aim of this study is to apply the same
mass transfer mathematical model, this time developed to
predict the essential oil extraction process behavior in three
species of Labiatae: Rosmarinus officinalis L., Ocimum basilicum
L., and Lavandula dentate L.
Essential oils from rosemary (R. officinalis), basil (O.
basilicum), and lavender (Lavandula dentata) have a strong con-
tribution on international market, mainly as additives in the
production of food and perfume products (Rezzoug et al.,
2005). Rosemary essential oil has also shown antibacterial
activity (Valero and Salmeron, 2003). Lavender essential oil
production is directed to fragrance industry, but it is also
used in food manufacturing as beverage and ice cream flavor-
ing (Chemat et al., 2006). The antioxidant capacity (Tomaino
et al., 2005) and antimicrobial activity (Opalchenova and

∗
Corresponding author. Tel.: +55 51 3320 3653; fax: +55 51 3320 3625.
E-mail address: cassel@pucrs.br (E. Cassel).
0926-6690/$ – see front matter © 2008 Elsevier B.V. All rights reserved.
doi:10.1016/j.indcrop.2008.04.017
172 i n d u s t r i a l c r o p s a n d p r o d u c t s 2 9 ( 2 0 0 9 ) 171–176
Obreshkova, 2003) contribute to consumption of basil essen-
tial oil. Culinary uses are another important application of
basil essential oil (Grayer et al., 2001).
The mathematical modeling of steam distillation must be
considered as an inevitable step to project industrial plants
with good operational conditions. Mathematical models are
used to simulate a process without the need to run experi-
mental procedures to know about extraction process behavior.
Therefore, the importance of mathematical modeling of the
steam distillation process is to allow alternative strategies to
evaluate the selection of the process variable conditions.
In the literature, there are some studies of mass transfer
modeling to simulate extraction process. Spiro and Selwood
(1984) interpreted their results in terms of a model based on
steady-state theory of extraction. The authors presented a
study of the particle size effect in the extraction and related
the diffusion coefficient of caffeine in the coffee bean parti-
cles and being of meaningful order of the 10−11 m2 /s. Spiro
et al. (1990) reported the kinetics of extraction of ginger
rhizome with dichloromethane, ethanol, 2-propanol and an
acetone–water mixture. In their modeling, all the extractions
proceeded in three stages: an initial “washing” stage, a fast
stage and a much slower stage, with a different diffusion coef-
ficient at each one of the stages. The diffusion coefficient was
reported in the interval 10−13 to 10−12 (m2 /s) for diffusion of the
soluble constituent through the particles and in the interval
10−10 to 10−11 (m2 /s) to diffusion of the constituent through the
Nernst layer, in function of the solvent. Benyoussef et al. (2002)
additionally modeled the extraction of coriander essential oil
by steam distillation using two diffusional models: the first
one takes in consideration only diffusion, while in the second
the solution of the transferred species is additionally modeled.
2. Experiments
2.1. Plant material and extraction of the essential oil
Plant materials were obtained between 1996 and 1999, and
established as a small-scale experimental area cultivated at
the Experimental Farm of Tekton Óleos Essenciais Ltda. in the
state of Rio Grande do Sul (Southern Brazil; latitude, 30◦ 05 S;
longitude, 50◦ 47 W; altitude, 100 m). Plants were grown from
small quantities of seed obtained from Biotechnology Insti-
tute, Universidade de Caxias do Sul, Brazil. All materials were
established in rows 1 m apart with 30 cm plant spacing. Irri-
gation was applied regularly during the growing season. The
amount of water applied in equivalent of mm rainfall per year
(1400) is desirable. Fertilizer was applied annually in equiva-
lent kg/ha of N (86.5), P205 (97.5), and K20 (70), according to soil
test results to ensure that soil fertility was not limiting crop
production.
According to the evaluation of the plants behavior in
response to seasonal factors in different collections over
the year, samples of fresh leaves, representing the entire
populations of rosemary, basil, and lavender essential oils,
were collected randomly in the Experimental Farm of
the Tekton Óleos Essenciais Ltda. during the full flower-
ing (September–November) period at the spring seasons of
1999–2001. All the flowering plants were chosen in order to
Table 1 – Average quantities of plant experimental data
Rosemary Basil Lavender
Mass of plant (g) 225.57 212.90 312.72
Thickness of leaf (m) 0.00044 0.00047 0.00047
Density (g/mL) 0.812 0.825 0.837
be representative to the same pedoclimatic and collection
conditions, and extraction conditions were identical for all
samples. Therefore, the influence of environmental and tech-
nical parameters on the chemical composition of the essential
oil was avoided. The oils were extracted from wet leaves
without any pre-processing. The average moisture contents
of the aromatic plants were 78.19%, 79.34%, and 79.45% to
rosemary, lavender, and basil, respectively. The steam distil-
lation apparatus used includes a 4.000 mL glass boiler heated
by an electric resistance, a 3.000 mL glass extraction cham-
ber, and a modified Clevenger trap with 5.00 mL graduated
tube. In the boiler is generated saturated steam at T = 366.65 K
and P = 1.01 bar with a steam flow = 3.4 mL/min. The appar-
ent density of the bed to rosemary, basil, and lavender were
0.075 g/mL, 0.0710 g/mL, and 0.1042 g/mL, respectively. Three
experiments for each plant were performed and average val-
ues of plant experimental data: leaf thickness, plant mass, and
density are showed in Table 1.
Thus the oil quantity m(t) is the average value obtained.
The extraction degree, e, was calculated using m(∞) as the
maximum value reach for each plant. The average yield
was calculated on a wet weight basis from the relationship
between essential oil mass, obtained from experimental vol-
ume and density, and mass of leaves of the fresh aromatic
plants. These results as time function are showed in Table 2.
2.2. GC analysis
The composition of the oil was carried out by GC on a Shi-
madzu 14 B gas chromatograph equipped with a FID and a
Shimadzu data processor software EZ-Chrom, using two cap-
illary columns. The first was a SE-52 (Mega, Legnano, Italy)
cross-linked fused-silica capillary column (25 m × 0.32 mm
i.d.), coated with 5% phenyl-polymethylsiloxane (0.40–0.45 ␮m
phase thickness); column temperature, 60 ◦ C for 8 min, ris-
ing to 180 ◦ C at 3 ◦ C/min, 180–250 ◦ C at 20 ◦ C/min, then 250 ◦ C
for 10 min. Injector temperature 250 ◦ C; detector temperature
280 ◦ C; injection mode, split; split ratio 1:40; volume injected,
0.2 ␮L of the oil. Carrier gas was hydrogen, 55 kPa.
The second was a Carbowax 20 M (Ohio Valley, USA) bonded
fused-silica capillary column (25 m × 0.32 mm i.d.), coated
with polyethylene glycol (0.25 ␮m phase thickness); column
temperature, 40 ◦ C for 8 min, rising to 180 ◦ C at 3 ◦ C/min, then
to 230 ◦ C at 20 ◦ C/min. Injector temperature 250 ◦ C; detector
temperature 250 ◦ C; injection mode, split; split ratio 1:40;
volume injected, 0.2 ␮L of the oil. Carrier gas was hydrogen,
30 kPa.
2.2.1. GC–MS analysis
GC–MS analyses were conducted using a Shimadzu QP 5050
apparatus equipped with reference libraries (Adams, 2001;
McLafferty and Stauffer, 1991) using two capillary columns.
The first was a SE-52 (Mega, Legnano, Italy) cross-linked
 i n d u s t r i a l c r o p s a n d p r o d u c t s 2 9 ( 2 0 0 9 ) 171–176 173

Table 2 – Experimental data of accumulated average volume and yield of essential oils
t (min) Rosemary Basil Lavender

V (mL) Yield (w/w) V (mL) Yield (w/w) V (mL) Yield (w/w)

0 0.00 0.0000 0.00 0.0000 0.00 0.0000

2 0.45 0.0016 0.17 0.0007 0.10 0.0003
4 0.68 0.0024 0.34 0.0013 0.25 0.0007
6 0.88 0.0031 0.49 0.0019 0.40 0.0011
8 1.08 0.0038 0.59 0.0023 0.55 0.0015
10 1.20 0.0043 0.72 0.0028 0.65 0.0017
12 1.30 0.0047 0.86 0.0033 0.75 0.0020
14 1.33 0.0048 0.93 0.0036 0.95 0.0025
16 1.38 0.0049 0.93 0.0036 1.00 0.0027
18 1.38 0.0049 0.96 0.0037 1.10 0.0029
20 1.43 0.0051 0.99 0.0038 1.10 0.0029
22 1.43 0.0051 0.99 0.0038 1.15 0.0031
24 1.43 0.0051 0.99 0.0038 1.20 0.0032
26 1.43 0.0051 0.99 0.0038 1.20 0.0032
28 1.43 0.0051 0.99 0.0038 1.20 0.0032
30 1.43 0.0051 0.99 0.0038 1.20 0.0032

fused-silica capillary column (25 m × 0.25 mm i.d.), coated cess the soluble constituent concentration was homogeneous
with 5% phenyl-polymethylsiloxane (0.25 ␮m phase thick- and constant for all particles. Furthermore, at boundaries
ness); column temperature, 60 ◦ C for 8 min, rising to 180 ◦ C steam carried out all oil, the oil concentration at the bound-
at 3 ◦ C/min, then to 230 ◦ C at 20 ◦ C/min. Injector temperature aries was very small (cA = 0). The mathematical formulation
250 ◦ C; injection mode, split; split ratio 1:40; volume injected, can be represented as follow
0.2 ␮L of the oil. Helium was used as a carrier, using 122.2 kPa
(51.6 cm/s); interface temperature 250 ◦ C; acquisition mass ∂2 cA 1 ∂cA
= in 0≤x≤L (1)
range, m/z 40–400. ∂x2 D ∂t
The second was a BP 20 (SGE, Australia) bonded fused-silica
initial conditions
capillary column (25 m × 0.25 mm i.d.), coated with polyethy-
lene glycol (0.25 ␮m phase thickness); column temperature,
cA = cA0 in t=0 (2)
40 ◦ C for 8 min, rising to 180 ◦ C at 3 ◦ C/min, then to 230 ◦ C at
20 ◦ C/min. Injector temperature 250 ◦ C; injection mode, split;
boundary conditions
split ratio 1:40; volume injected, 0.2 ␮L of the oil. Carrier
gas was He, 92.6 kPa (55.9 cm/s); interface temperature 250 ◦ C;
acquisition mass range, m/z 40–400. cA = 0 in x=0 (3)

cA = 0 in x=L (4)
2.2.2. Identification and quantification
The components of the oil were identified by comparison of
where L is the thickness of the plate and D is the effective
their linear retention indices (LRIs) on the two columns, deter-
diffusion coefficient.
mined in relation to a homologous series of n-alkanes, with
The Eqs. (1)–(4) are a Sturm Liouville problem. It was used
those from pure standards or reported in literature. Compari-
the separation variable technique and the following solution
son of fragmentation patterns in the mass spectra with those
was established (Kreider et al., 1966)
stored on the GC–MS databases (Adams, 2001; McLafferty and
Stauffer, 1991) was also performed. 
∞
4cA0 2
The percentages of each component were reported as cA (x, t) = sen(ˇn x)e−Dˇn t (5)
n
raw percentages without standardisation. Repeatability of the n=1
measuring system showed variation coefficients under 5% for
all the components reported in Table 3 for the essential oils where
extracted.
n
ˇn = (6)
L
3. Mathematical modeling with n = 1, 2, 3, . . ..
The mass flow as function time was obtained from the
A mathematical model of the extractive process was applied mass flux at the boundary multiplied by normal surface area
in this work. In this model the stage controlling process resulting
was the diffusion in the particle. It was simulated the
4cA0 DA  −Dˇ2 t
steam distillation process using a model based on Fick’s law ∞

in unsteady-state for one-dimensional rectangle geometry ṁA (t) = e n (7)

L
(Cassel and Vargas, 2006), assuming that in the beginning pro- n=1
174 i n d u s t r i a l c r o p s a n d p r o d u c t s 2 9 ( 2 0 0 9 ) 171–176

Table 3 – GC–MS of essential oils extracted by steam distillation

Compound LRIa Rosemary Lavender Basil

Rt b %c Rt % Rt %
Tricyclene 927 – – – – 10.07 0.02
␣-Thujene 930 – – 12.43 0.05 10.37 0.02
␣-Pinene 938 13.58 37.22 12.94 3.07 10.73 0.76
Camphene 944 14.06 3.97 13.68 1.10 11.46 0.74
Thuja-2,4(10)diene 951 14.21 0.40 13.97 0.24 – –
Sabinene + ␤-pinene 973 15.54 2.81 15.46 4.38 12.92 2.26
Myrcene 990 16.40 1.95 16.25 0.65 13.91 0.94
␣-Phellandrene 1000 17.07 0.27 16.96 0.10 - -
␣-Terpinene 1014 17.84 0.52 – – 15.29 0.05
1,8-Cineole 1034 19.34 23.76 19.50 42.47 16.76 22.29
cis-␤-Ocimene 1045 – – – – 17.32 0.37
trans-␤-Ocimene 1054 – – – – 17.84 0.13
␥-Terpinene 1060 20.55 1.19 20.41 0.11 18.37 0.58
cis-Sabinene hydrate 1063 21.01 0.33 – – – –
␣-Terpinolene 1084 22.35 1.13 23.48 1.49 – –
Fenchone 1087 – – 22.86 14.96 – –
Linalool 1100 23.35 2.93 23.69 0.96 21.94 35.97
cis-Thujone 1110 24.00 0.02 – – – –
endo-Fenchol 1115 24.58 0.35 24.72 4.60 – –
Camphor 1146 27.08 0.40 26.42 10.85 23.85 11.52
cis-Chrysanthenol 1163 27.82 2.66 – – – –
Pinocarvone 1165 28.03 0.66 27.20 0.24 – –
Borneol 1169 28.31 0.80 – – 24.72 0.51
4-Terpineol 1171 – – 28.23 0.44 25.31 0.41
Cryptone 1179 – – 28.81 0.52 – –
p-Cymen-8-ol 1186 – – 29.25 0.56 – –
␣-Terpineol 1189 29.59 1.51 29.51 1.24 26.38 1.95
Myrtenol 1198 – – 30.27 0.16 26.58 0.08
Verbenone 1208 30.86 2.88 30.88 0.16 26.96 0.04
trans-Carveol 1217 – – 31.45 0.11 – –
Citronellol 1228 31.62 0.18 – – – –
Cumminaldehyde 1235 32.11 0.21 – –
Neral 1240 32.50 0.19 – – – –
Carvone 1242 – – 32.39 0.22 – –
Geraniol 1253 33.63 2.94 – – 30.33 0.23
Linalyl acetate 1259 – – 33.82 trd – –
Bornyl acetate 1285 35.18 1.70 – – 32.11 0.08
Pinocarvyl acetate 1320 – – – – 34.39 0.03
␣-Cubebene 1353 – – – – 35.74 0.03
Eugenol 1359 – – – – 36.85 6.14
␣-Copaene 1371 – – – – 37.29 0.21
␤-Bourbonene 1379 – – – – 37.78 0.27
Geranyl acetate 1380 40.59 0.22 – – - -
␤-Elemene 1388 – – – – 38.33 1.46
Methyl eugenol 1400 41.67 0.13 – – – –
␤-Caryophyllene 1419 42.67 1.52 42.47 0.25 39.91 1.62
␤-Farnesene 1420 – – 43.14 0.32 – –
␤-Copaene 1429 – – – – 40.28 0.08
trans-␣-Bergamotene 1437 – – – – 40.72 1.08
␣-Humulene 1454 44.06 0.20 – – 41.53 0.34
Germacrene D 1483 – – – – 43.02 3.53
Germacrene A 1500 – – – – 43.88 0.63
␥-Cadinene 1513 – – – – 44.22 0.60
trans-Calamenene 1522 – – – – 44.48 0.10
(1,10-di-epi)-Cubenol 1616 – – – – 47.72 0.19
␣-Muurolol 1647 – – – – 48.63 1.17
␤-Eudesmol 1658 – – – – 48.88 0.13

Total 92.84 89.46 96.56

a
LRI, linear retention time.
b
Retention time.
c
Relative proportions of the essential oil constituents were expressed as percentages obtained by peak-area normalization, all relative response
factors being taken as one. Percentages were obtained on SE-52.
d
tr, <0.01%.
 i n d u s t r i a l c r o p s a n d p r o d u c t s 2 9 ( 2 0 0 9 ) 171–176 175

Thus, the extracted mass of soluble constituent can be pre-

sented as

8mA0  (1 − e−(2m+1)  Dt/L )

∞ 2 2 2

mA (t) = , (8)
2 (2m + 1)
2
m=0

and the extraction degree defined by


∞
2 2
(1 − e−(2m+1)  Dt/L2 )/(2m + 1)
2

mA (t) m=0
e(t) = = (9)
mA (∞) 
∞
2
1/(2m + 1)
m=0 Fig. 1 – Steam distillation yield extraction curves vs. time:
mathematical model (– – rosemary, — basil, and - - - - laven-
der) and experimental data ( rosemary, 䊉 basil, and ×
4. Results and discussion
lavender).

The yield curve was constructed from the oil mass extracted
relation to the sample amount used in the extraction based
on wet weight. Table 4 shows the quantities used in the sim-
balance across internal surface of particle assuming that the
ulation.
components to be extracted are uniformly distributed inside
In the diffusional model, the parameter D was directly
the particle and the surface resistance is negligible, that is
adjusted using the Eq. (9) with one term in the series
close to reality. The first step of the curve may be considered
and the data presented in Table 4. The values obtained to
a straight line, corresponding to a constant extraction rate
parameter D were 4.36 × 10−11 m2 /s to rosemary essential oil,
while the second step approaching a limit value, which was
5.96 × 10−11 m2 /s to basil essential oil, and 3.32 × 10−11 m2 /s to
given by the potential steam distillation amount of extractible
lavender. This parameter was estimated by minimization of
substances.
the sum of square of errors between the experimental data
and the prediction from model.
The comparison among the experimental data and the 5. Conclusions
results of the mathematical model of steam distillation-
extraction yield with time for rosemary, basil, and lavender The development of essential oil sector has a direct relation
is shown in Fig. 1. with the improvement of process technology in industrial
The analysis of the results showed in Fig. 1 indicated that plants. This study introduces a model based on single
diffusional model, based on mass transfer, fitted very well the plate particle description to predict the behavior of steam
experimental data. The diffusional model is based on material distillation-extraction process using the laboratorial exper-
imental data. The model parameter evaluation could be a
useful tool during the scale-up of the extraction process and/or
during pilot or industrial operation in order to evaluate the
Table 4 – Data used in the mathematical simulation as a extraction time required to obtain a given yield. Three essen-
function of time
tial oils were used as models: rosemary, basil, and lavender,
t Rosemary Basil Lavender and the extraction curve followed the same behavior in all
m e m e m e cases. The maximum yield values obtained for rosemary, basil,
and lavender oils were 0.51%, 0.38%, and 0.32% (w/w), respec-
0 0.00 0.00 0.00 0.00 0.00 0.00
tively.
2 0.37 0.30 0.14 0.17 0.08 0.08
4 0.55 0.45 0.28 0.34 0.21 0.19
6 0.71 0.59 0.41 0.49 0.33 0.30 references
8 0.87 0.72 0.49 0.59 0.46 0.42
10 0.98 0.81 0.60 0.72 0.54 0.49
12 1.06 0.88 0.71 0.86 0.63 0.57
Adams, R.P., 2001. Identification of Essential Oils Components by
14 1.08 0.89 0.77 0.93 0.80 0.72
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16 1.12 0.93 0.77 0.93 0.84 0.76
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