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J.

of Supercritical Fluids 48 (2009) 15–20

Contents lists available at ScienceDirect

The Journal of Supercritical Fluids


journal homepage: www.elsevier.com/locate/supflu

Review

Comparison of extraction of patchouli (Pogostemon cablin) essential oil with


supercritical CO2 and by steam distillation
A. Donelian a,∗ , L.H.C. Carlson b , T.J. Lopes a , R.A.F. Machado a
a
Laboratório de Controle de Processos, Departamento de Engenharia Química e Engenharia de Alimentos, Universidade Federal de Santa Catarina,
caixa postal 476 CEP: 88010-970, Florianópolis, SC, Brazil
b
Coordenação de Engenharia de Alimentos/CCAA/UNOCHAPECÓ, Av. Sen. Attílio Fontana, 591-E, Bairro Efapi, caixa postal 747, CEP: 89809-000. Chapecó, SC, Brazil

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

Article history: Patchouli essential oil is an important raw material for the perfume and cosmetics industries, besides being
Received 12 September 2007 used as a natural additive for food flavoring. Patchoulol and ␣-patchoulene are important compounds
Received in revised form 7 September 2008 of patchouli essential oil, and their concentrations are directly proportional to the quality of the oil.
Accepted 10 September 2008
Nowadays, the usual method employed to obtain patchouli essential oil is steam distillation; however,
this causes thermal degradation of some oil compounds. In this study patchouli essential oil was extracted
Keywords:
with supercritical carbon dioxide (scCO2 ) under different conditions of pressure (8.5 and 14 MPa) and
Supercritical extraction
temperature (40 and 50 ◦ C) and also by steam distillation to compare the extraction methods. It was
Patchouli
Essential oil
demonstrated that the extraction with supercritical carbon dioxide provided a higher yield and a better
Carbon dioxide quality of patchouli essential oil.
© 2008 Elsevier B.V. All rights reserved.

Contents

1. Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
2. Experimental . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
2.1. Material . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
2.2. Supercritical equipment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
2.3. Supercritical extraction procedure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17
2.4. Steam distillation equipment and procedure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17
2.5. Chromatographic analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17
3. Results and discussion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17
4. Conclusions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19
References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19

1. Introduction Administration) list of substances approved for human consump-


tion, in section 172.510, as a natural additive for food flavoring [7].
Patchouli oil is obtained from the leaves of Pogostemon cablin Moreover, the plant (P. cablin) is widely used in traditional Chi-
(patchouli), a plant of the Lamiaceae family, originating from nese medicine as it offers various types of pharmacological activity
Malaysia and India [1]. It is an important essential oil in the perfume according to the composition of the oil [1,8].
industry, used to give a base and lasting character to a fragrance The composition of patchouli oil is unique and complex because
[2,3,4]. The essential oil is very appreciated for its characteristic it consists of over 24 different sesquiterpenes, rather than a blend
pleasant and long lasting woody, earthy, and camphoraceous odor, of different mono-, sesqui- and di-terpene compounds [5]. The
as well as for its fixative properties, being suitable for use in soaps sesquiterpene patchoulol is the major constituent and is the pri-
and cosmetic products [5,6]. It is also on the FDA’s (Food and Drug mary component responsible for the typical patchouli aroma. This
essential oil is also characterized by a large number of other
sesquiterpene hydrocarbons such as ␣-/␤-/␥- patchoulenes, ␣-
∗ Corresponding author. guaiene, seychellene, and ␣-himachalene. Although ␣-patchoulene
E-mail address: adriana@enq.ufsc.br (A. Donelian). is found in small amounts, it is an important constituent of

0896-8446/$ – see front matter © 2008 Elsevier B.V. All rights reserved.
doi:10.1016/j.supflu.2008.09.020
16 A. Donelian et al. / J. of Supercritical Fluids 48 (2009) 15–20

patchouli oil because, together with patchoulol, it also determines


the aroma of the oil. Also, it is believed that the antifungal activ-
ity of the essential oil is closely related with these two compounds
[2,5,8]. Thus, the greater the concentration of these compounds in
the essential oil, the better the quality and the higher the commer-
cial value [9].
Therefore, as the commercial value of patchouli essential oil is
directly correlated with its qualitative and quantitative composi-
tion, which varies according to the cultivation region and extraction
technique [1,2], an improved process for its extraction would be of
industrial interest. It should be noted that patchouli plants are the
only commercial source of patchoulol and that cost-effective syn-
thetic routes for enantiomerically pure patchoulol have yet to be
developed [5].
Nowadays, patchouli essential oil is traditionally obtained by
steam distillation [1,2,5]. This procedure, performed at a high tem-
perature, can cause the degradation of thermally labile compounds
resulting in the formation of undesirable compounds [10]. In this
regard, extraction of essential oils using supercritical carbon diox-
ide (scCO2 ) has been the subject of considerable interest, mainly
for the extraction of natural products. Carbon dioxide has sev-
eral unique characteristics and physico-chemical properties, since
it is non-toxic and inert and has low critical pressure (7.38 MPa)
and temperature (31.1 ◦ C). Compared with conventional extraction
methods, extraction with scCO2 has many advantages including
more selective extracts without thermal degradation and which
are solvent-free, thus providing an oil of superior quality [11,12].
The selectivity of carbon dioxide in relation to the essential oil
can be adjusted by changing the temperature and pressure condi-
tions, leading to oils with different compositions. Carlson et al. [12]
observed that the best condition for the extraction of lemongrass
essential oil was 12 MPa and 40 ◦ C.
The objective of this study was to compare the variations in the
yield and chemical composition of patchouli essential oil obtained
under different conditions (pressure and temperature) of supercrit-
ical extraction with CO2 and by steam distillation. No information
could be found in the literature regarding the use of scCO2 for
patchouli essential oil extraction.

2. Experimental

2.1. Material

Patchouli plants [P. cablin (Blanco) Benth] were collected in


November 2002 from “Colônia Penal Agrícola” (Palhoça, SC, Brazil).
For the extraction, the leaves were collected manually from the Fig. 1. Experimental unit of supercritical fluid process: (1) CO2 cylinder; (2, 4, 8, 14)
flow control valves; (3) gas booster; (5 and 10) pressure transducers; (6) jacketed
plants and all of them were from the same lot.
surge tank; (7) pneumatic control valve; (9) jacketed extraction vessel; (11) forward
Patchouli leaves were dried in an oven with air circulation pressure regulator; (12) manometer; (13) separation vessel; (15) micrometer valve;
(Model TE – 394/2, TECNAL, Brazil) for 1440 min at 30 ◦ C and (16) flow meter; (17 and 18) thermostatic water baths.
180 min at 35 ◦ C. These temperatures were selected because they
have previously been used in the drying of patchouli leaves for
essential oil extraction [13]. The dried leaves were ground with a volume and 0.55 m height). The jacketed surge tank was placed
knife grinder (Model MA – 580, Marconi, Brazil) and, in the case of between the gas booster and the extraction vessel in order to avoid
the supercritical extractions, were then sieved (mesh 30) in order potential pressure overshoots allowing a better pressure control.
to standardize the size of the particles. The temperatures of the surge tank and extraction vessel were con-
trolled by a thermostatic water bath (18) (Model MQBTC 99-20,
2.2. Supercritical equipment Microquímica, Brazil).
The extraction pressure was maintained by the gas booster,
The extractions with scCO2 were performed in a pilot unit monitored by a pressure transducer (10) (Model RTP12/BE53R, AEP,
schematically represented in Fig. 1. Italy) and controlled by a pneumatic control valve (7) (Model: 807,
A gas booster (3) (Model DLE 15-1, MAXPRO Technologies, Ger- Badger Meter, USA). The samples were collected at different time
many) received liquid CO2 (99% purity, White Martins, Brazil) from intervals in a separation vessel (13) at a pressure of 2.4 MPa and
a cylinder (1) and pressurized a jacketed surge tank (6) (Labsolda, temperature of 34 ◦ C, allowing the separation of the oil by changing
UFSC, Brazil, 4.6 × 10−3 m3 volume) which in turn provided gas to the CO2 phase. The temperature was maintained by a thermostatic
a jacketed extraction vessel (9) (Labsolda, UFSC, Brazil, 1 × 10−3 m3 water bath (17) and the pressure by a forward pressure regulator
A. Donelian et al. / J. of Supercritical Fluids 48 (2009) 15–20 17

valve (11) (MTR Model 200-70, Brazil). The solvent flow was con-
trolled manually through a micrometer valve (15) (Model SS-21RS4,
Swagelok, Ohio, USA) and was measured at the exit of the separator
by a flow meter (16) (Model PV005LPMOCC, Key Instruments, USA)
under ambient conditions.

2.3. Supercritical extraction procedure

To perform the tests the sieved patchouli plant material was


divided into equal portions of 0.15 kg and four extractions were
performed. Extractions were carried out at temperatures of 40
and 50 ◦ C, pressures of 8.5 and 14 MPa, and CO2 flow rate of
6.0 × 10−3 kg/min based on the density of the CO2 exiting the sep-
arator under ambient conditions. These temperatures were chosen
based in the rate commonly used in the supercritical extraction of
essential oils [14] and the flow rate was defined as being close to
the average CO2 flow rate of 4.7 × 10−3 kg/min used by Carlson et
al. [12] in the supercritical extraction of lemongrass essential oil.
The influence of pressure and temperature on the patchouli
extracted and chemical composition of the patchouli essential oil Fig. 2. Extraction curves obtained under different conditions of pressure and tem-
were evaluated using a two-level factorial design. perature.
Each supercritical extraction experiment was carried out for
a period of 340 min. The extract samples were collected in the
250 ◦ C, the transfer line temperature 260 ◦ C, the ion source tem-
separation vessel (13) at predefined time intervals and weighed
perature 230 ◦ C and the ionization mode was electron impact at
immediately. The time intervals were shorter at the beginning
70 eV. The oven temperature was programmed to increase from
of the extraction and they increased gradually until the end of
60 to 240 ◦ C at a rate of 3 ◦ C/min. The carrier gas was helium at a
the extraction. The extracts collected during the experiment were
flow rate of 1.0 × 10−3 L/min and the sample volume injected was
mixed at the end and submitted to chromatographic analysis.
0.03 ␮L of the pure oil with a split rate of 1:100.
2.4. Steam distillation equipment and procedure
3. Results and discussion
The steam distillation was carried out with approximately 0.1 kg
of dry and ground patchouli plant material. The sieved leaves were Fig. 2 shows the supercritical extraction curves (percentage yield
placed on a perforated plate (3), which was located some centime- relative to dried patchouli leaves) obtained under different condi-
ters away from the extractor bottom (4). The extractor was then tions of pressure and temperature.
filled with water up to the plate and heated by a hot-plate (2) pro- In Fig. 2 it can be observed that the curves obtained at a pressure
ducing water vapor. After passing over the patchouli the vapor was of 14 MPa indicate two main stages. The first, known as the stage
condensed in a cooling system (5), collected in a funnel (6) together of constant extract rate, is linear and refers to the stage in which
with the oil and then separated. The separated oil was collected in the oil accessible through the cell rupture by grinding is extracted
an Erlenmeyer flask (7) and weighed immediately after collection. easily by the solvent. After a certain time, which depends on the
The extraction experiment was carried out for a period of 120 min, extraction conditions (e.g. 100 min at 14 MPa and 40 ◦ C), there is
after which time the amount of essential oil collected in the funnel a transition period, in which the extraction decreases rapidly and
(6) did not increase. then continues at a much slower rate, when the oil is extracted
from inside the vacuole (second stage). This kind of curve is typical
2.5. Chromatographic analysis of processes where the solid has a high initial concentration.
However, in extractions at a pressure of 8.5 MPa, the curves did
Analysis of the samples obtained under different conditions not show the same behavior. This is because both the decrease in
of supercritical CO2 and by steam distillation was performed by pressure and the increase in temperature promoted reductions in
Embrapa (Rio de Janeiro, RJ, Brazil). the density of the scCO2 , as can be observed in Table 1, reducing
The separation of essential oil compounds was performed on a the solubilization of the oil in the solvent (scCO2 ).
Hewlett-Packard gas chromatograph with flame ionization detec- In order to analyze statistically the influence of the pressure and
tor (Model HP 5890 series II, USA) using a fused-silica capillary temperature on the patchouli essential oil yield at the end of the
column HP5-MS (25 m length × 0.25 mm internal diameter and extraction, the data were organized as shown in Table 2. It can be
0.33 ␮m film thickness). The flame ionization detector was main-
tained at 280 ◦ C and the injector temperature was 250 ◦ C. The oven Table 1
temperature was programmed to increase from 60 to 240 ◦ C at a rate Patchouli essential oil yield and CO2 density under different conditions of supercrit-
of 3 ◦ C/min. The carrier gas was helium at a flow rate of 1.0 mL/min, ical extraction and by steam distillation.
and the sample volume injected was 0.03 ␮L of the pure oil with a Extraction with scCO2
split rate of 1:100.
Pressure (MPa) Temperature (◦ C) Density (kg/m3 ) Yield (%)
Identification of essential oil compounds was based on com-
parison of the mass spectra obtained in the gas chromatography 8.5 40 3.57 × 10−4 1.38
8.5 50 2.48 × 10−4 0.44
with those obtained from the GC–MS library [15]. The chromatogra-
14 40 7.64 × 10−4 5.07
phy was performed on a gas chromatograph (Model Agilent 6890), 14 50 6.74 × 10−4 3.92
using a fused-silica capillary column HP5-MS, coupled to a selec-
Steam distillation 1.50
tive mass detector (Model 5973N). The injector temperature was
18 A. Donelian et al. / J. of Supercritical Fluids 48 (2009) 15–20

Table 2 is the principal component of the oil, and ␣-patchoulene, which is


Effect of pressure and temperature on patchouli essential oil extraction yield.
the second most important component.
Effect* SEM p −95.0% +95.0% Thus, in order to evaluate the quality of the patchouli essential
Mean 2.70 0.0525 0.012366 2.03 3.37
oil obtained under the different extraction conditions, chromato-
Temperature −1.04 0.1050 0.063753 −2.38 0.29 graphic analysis of the oil obtained under each set of conditions
Pressure 3.58 0.1050 0.018640 2.25 4.92 was carried out in order to identify the qualitative and quanti-
SEM = Standard error of the mean. tative composition. Table 3 shows the comparative composition
*
Estimated values of the effect. of the patchouli essential oil obtained under the different condi-
tions.
It can be observed in Table 3 that patchouli essential oil is
observed, through the p level value, that only the pressure was sig- comprised of a mixture of chemical compounds, most of them in
nificant at the 95.0% level, since the p value for the pressure is small quantities. The compounds present in higher quantities are
less than 0.05. Therefore, an increase in the pressure of the sys- the same in all patchouli essential oils: patchoulol, ␦-guaiene, ␣-
tem can lead to a significant increase in the patchouli essential oil guaiene, ␣-patchoulene and ␤-caryophyllene. These compounds
yield during the extraction, while the temperature does not exert are the same as those found by Betts [6] in the analysis of a commer-
a significant influence. Thus, within the conditions studied, the cial sample of patchouli essential oil (Rivendell, Bunbury, Western
pressure of 14 MPa and temperature of 40 ◦ C provided the best con- Australia). The commercial sample had 28.5% of patchoulol, 12.0%
ditions for the extraction of patchouli essential oil in terms of yield. of ␦-guaiene, 10.4% of ␣-guaiene, 6.9% of seychellene, 6.4% of ␣-
According to Heath [16] and Moyler [17], the fraction of patchouli patchoulene, 4.7% of caryophyllene and 1.7% of ␤-patchoulene.
oil obtained by steam distillation was between 1.5% and 3.0%, which Furthermore, on analyzing Table 3 it can be observed that
is in agreement with the value obtained experimentally which was although the increase in pressure promoted an increase in yield, this
1.5%. However, the extraction with scCO2 at 14 MPa and 40 ◦ C pro- increase was not associated with a reduction in selectivity. This can
vided a much higher yield of 5.07% (no papers or scientific studies be highlighted by the fact that at 40 ◦ C the increase in pressure from
relating to the extraction of patchouli essential oil with scCO2 could 8.5 to 14 MPa led to an increase in the patchoulol concentration
be found for comparison). from 14.90% to 31.39%, while the total quantity of the compo-
Increase in the pressure led to a higher density of the scCO2 nents identified remained almost the same (80.00% for 8.5 MPa
inducing a greater solubilization and, consequently, an increase in and 78.02% for 14 MPa). This result indicates that the greater yield
the extraction yield, however, with a tendency to reduce the selec- obtained at high pressure is not exclusively due to the extraction of
tivity due to the extraction of undesirable components in terms of undesirable components such as cuticular waxes. The results could
the oil quality, such as cuticular waxes. Thus, given that the indus- be further improved with an extraction treatment using scCO2 to
trial interest is mainly concerned with obtaining a product with remove the waxes, which are normally extracted with the oil. How-
a greater concentration of active principles Santos [18], the quan- ever, in this study this type of treatment was not carried out since
tity of an essential oil is generally evaluated through an analysis of the main aim was to assess the viability of the supercritical extrac-
its principal components. In the case of patchouli essential oil, this tion of patchouli essential oil, in view of the fact that no data are
quality is evaluated from the concentrations of patchoulol, which available on this subject in the literature.

Table 3
Main compounds identified in patchouli essential oil.

Compounds Comparative chemical composition (%)

8.5 MPa/40 ◦ C 8.5 MPa/50 ◦ C 14 MPa/40 ◦ C 14 MPa/50 ◦ C Steam distillation

1-Octen-3-ol 0.12 0.18 0.79 0.08 –


Limonene 0.78 0.40 0.08 0.07 –
Linalool 0.07 0.09 – 0.02 –
␦-Elemene 0.26 0.22 0.17 0.16 –
␤-Patchoulene 2.89 3.26 1.72 1.62 2.6
␤-Elemene 0.99 0.65 0.52 0.50 1.8
␤-Caryophyllene 5.67 5.85 3.29 3.13 4.8
␥-Elemene 0.03 – – 0.03 –
␣-Guaiene 23.05 24.16 14.09 13.38 20.0
␣-Himachalene 0.16 0.17 0.11 0.10 0.9
␣-Patchoulene 5.73 6.21 4.80 4.59 5.8
Seychellene 2.14 2.31 1.83 1.72 3.3
9-Epi-caryophyllene 0.68 0.69 0.48 0.45 0.7
cis-␤-Guaiene 0.08 0.09 0.06 0.06 –
Ledene 0.39 0.41 0.03 0.28 –
␣-Selinene 0.21 0.24 0.49 0.46 3.9
␦-Guaiene 20.75 21.16 16.79 15.55 23.3
␤-Curcumene 0.08 0.10 0.08 0.09 –
7-Epi-␣-selinene 0.19 0.20 0.18 0.17 –
Longicanfenolene 0.41 0.37 0.61 0.62 –
Caryophyllene oxide 0.19 0.16 0.15 0.16 –
Globulel 0.16 0.15 0.24 0.30 –
Epi-␣-cadinel 0.07 – 0.12 0.12 –
Patchoulol 14.90 12.93 31.39 32.23 19.4
␦-Patchoulene – – – – 8.0
␦-himachalene – – – – 0.6
Ftalete – – – – 1.7

Total 80.00 80.00 78.02 75.89 96.8


A. Donelian et al. / J. of Supercritical Fluids 48 (2009) 15–20 19

Table 4 Therefore, through Tables 4 and 5, it can be noted that the pres-
Effect of pressure and temperature on patchoulol concentration.
sure is a predominant factor in the variation in the concentration
Effect* SEM p −95.0% +95.0% of the principal components of the patchouli essential oil, and the
Mean 22.84 0.7275 0.020273 13.59 32.08
influence of temperature can be neglected. Moreover, on analyzing
Temperature −0.51 1.4550 0.783428 −19.00 17.97 the estimated values for the effect of pressure on the concentrations
Pressure 17.84 1.4550 0.051793 −0.64 36.33 of patchoulol and ␣-patchoulene, it can be verified that although
SEM = Standard error of the mean. this factor acts in a different way for each component, its effect
*
Estimated values of the effect. is the most significant in relation to the patchoulol concentration,
with increases in pressure leading to a patchouli essential oil richer
in patchoulol.
It can be seen in Table 3 that the concentrations of patchoulol in As the quality of patchouli essential oil is directly related to
the patchouli oil obtained by steam distillation (19.4%) was lower the concentration of patchoulol and ␣-patchoulene, supercritical
in relation to the oil obtained in the supercritical extractions with a extractions with higher pressure and low temperature besides pro-
pressure of 14 MPa (31.39% at 40 ◦ C and 32.23% at 50 ◦ C), and higher viding an oil of higher yield also provide an oil of better quality.
than that obtained with scCO2 at 8.5 MPa (14.90% at 40 ◦ C and Thus, in scCO2 extraction, the pressure and temperature conditions
12.93% at 50 ◦ C). For the concentrations of ␣-patchoulene, essential which give a higher yield will also provide an oil of better quality.
oil obtained by steam distillation presented a higher concentra-
tion (5.8%) in relation to the oil obtained through supercritical
4. Conclusions
extraction at 14 MPa (4.80% at 40 ◦ C and 4.59% at 50 ◦ C) and a con-
centration close to that of the oil obtained at 8.5 MPa (5.73% at 40 ◦ C
The extraction of patchouli essential oil with scCO2 at 14 MPa
and 6.21% at 50 ◦ C).
and 40 ◦ C gave the best yield (5.07%), which was higher than that
Moreover, the total number of compounds present in the
of steam distillation (of 1.50%).
patchouli essential oil (identified and non-identified) obtained by
In relation to the essential oil composition, only the pressure
steam distillation was 18, which is lower than the number found
had a significant effect on the composition, with a higher pressure
in the oils obtained by supercritical extraction (56, 45, 61, and 73
leading to a greater concentration of patchoulol, the main compo-
at 8.5 MPa/40 ◦ C, 8.5 MPa/50 ◦ C, 14 MPa/40 ◦ C, and 14 MPa/50 ◦ C).
nent of the oil. However, regardless of the operating conditions, the
These differences in whole the number of compounds and their
compounds present in greatest quantities in all of the patchouli
concentrations in the oils obtained using the two extraction meth-
essential oils were the same: patchoulol, ␦-guaiene, ␣-guaiene,
ods may be attributed to the degradation of some components
␣-patchoulene and ␤-caryophyllene. Highest concentrations of
through the use of a high temperature in the steam distillation
patchoulol were obtained in the extractions with supercritical
(approximately 100 ◦ C).
CO2 at 14 MPa, showing that the quality of the patchouli essen-
Nevertheless, it was verified that the quality of oil obtained by
tial oil improved with the increase in the yield. Although the
steam distillation is very similar to that obtained by supercritical
␣-patchoulene concentration decreased under these conditions,
extraction with CO2 at the lower pressure (8.5 MPa). However, this
the increase in the patchoulol concentration was of greater signif-
quality is lower when compared to the oil obtained with scCO2
icance.
at the higher pressure (14 MPa). Therefore, it was verified that,
Therefore, for the extraction of patchouli essential oil supercrit-
depending on the pressure condition of scCO2 , it is possible to
ical carbon dioxide shows better results in terms of yield and oil
obtain an essential oil of better quality and in higher yield than
quality than steam distillation, besides offering the advantage of
that obtained by steam distillation.
not promoting the decomposition of possibly thermolabile com-
A statistical analysis was carried out to evaluate the influence of
pounds. The best extraction conditions among those tested were
pressure and temperature on the composition of the oils obtained
14 MPa and 40 ◦ C, Future studies will be aimed at defining the
by supercritical extraction. It was found that the pressure has a
optimum operating conditions for the supercritical extraction of
greater effect than temperature on the patchoulol concentration
patchouli essential oil.
(Table 4), even though the statistical indices showed a slight ten-
dency not to be significant at the 95.0% level. The estimated effect
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