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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
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
2. Experimental
2.1. Material
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.
Table 3
Main compounds identified in patchouli essential oil.
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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