Sustainable Chemistry and Pharmacy 8 (2018) 76–81

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Sustainable Chemistry and Pharmacy

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Extraction of essential oils from damask rose using green and conventional T
techniques: Microwave and ohmic assisted hydrodistillation versus
hydrodistillation
⁎
Roghaieh Manouchehria, Mohammad Jamal Saharkhiza, Akbar Karamia, , Mehrdad Niakousarib
a
Department of Horticultural Science, School of Agriculture, Shiraz University, Shiraz 71441-65186, Iran
b
Department of Food Science and Technology, School of Agriculture, Shiraz University, Shiraz, Iran

A R T I C LE I N FO A B S T R A C T

Keywords: Damask rose is cultivated as the main species used in the production of rose water and relevant essential oils
Rosa damascena Mill. (EOs) of rose for its fragrance and therapeutic applications. Since the flowers are highly perishable, the ex-
Solvent free microwave-assisted extraction traction of oil should be done rapidly in order to produce rose EO successfully and optimally. Solvent free
Ohmic assisted hydrodistillation microwave-assisted extraction (SFME) and ohmic assisted hydrodistillation (OAHD) are advanced and green
Essential oil
distillation techniques, which utilize microwave, and ohmic heating processes respectively for the extraction of
Rose oil composition
EOs. In this study, SFME and OAHD of EOs were performed on fresh flowers of damask rose, and the findings
were compared with the traditional hydrodistillation (HD). The findings of EO analysis indicated considerable
alterations in EOs compounds extracted by SFME and OAHD methods compared with the traditional HD. To
reach the desirable temperature of extraction (nearly 100 °C) and to get the first EO droplets’ evaporation with
steam, the mixture was heated for 2.50 ± 0.29 min in SFME and for 17.33 ± 0.33 min in OAHD, while for the
HD the heating had to take more than 40 min (42.66 ± 0.32 min). The total extraction time of EOs extracted
from damask rose by using the green extraction procedures (SFME and OAHD) were compared with HD ex-
traction method. Extraction by SFME occurred much earlier than extraction by OAHD. Also in this study, the
analysis of EOs indicated that the chemical profile of damask rose may fluctuate quantitatively with respect to
the constituents and structure of the extracted molecules. This would depend on the system of extraction that
influences the characteristics of the EOs.

1. Introduction
The damask rose (Rosa damascena Mill.) is considered as a major
species of rose on which extractions are performed to yield of EOs,
products of rose water and perfume of rose in industries (Rusanov et al.,
2012; Karami et al., 2012). Two major rose oil production areas re-
cognized widely in the world are rose cultivations in Isparta of Turkey
and Kazanlik of Bulgaria (Baydar et al., 2008). In addition to those
regions, the Fars province of Iran is another leading producer of damask
rose where 8598 t of flowers are produced annually in 6149 ha of
gardens (Iranian Ministry of Agriculture, 2014). Generally, EO yield of
damask rose flowers are very little (0.03–0.04%) and the fresh top-
quality rose flowers are harvested in the early hours of morning for
highest EO yields (Baydar and Baydar, 2005). Traditionally, the full-
bloom phase is the most appropriate period of plant growth when
considering the purpose of obtaining extraction of rose oil or rose
water. Nonetheless, recent investigations indicate that the yield of rose
oil distilled from buds of rose is the same or greater in amount for the
same flower material weight when compared to distillation performed
on full-bloomed flowers (Rusanov et al., 2012). Various methods are
employed for isolating oils from different materials of plant. It may
seem comparatively easy to separate such oils, but the composition of
oils could differ substantially, based on the extraction method that is
applied (Anitescu et al., 1997; Cassel et al., 2009). Technologies of
traditional extraction are often inconvenient and energy-consuming.
Concerns pertaining to cost and the environment have demanded re-
ductions in CO2 emissions. This encourages researchers to find sub-
stitutes and equipment based on their cost-effective criteria. The
equipment and method need to be sustainable, and to have better po-
tentials of making products with similar principal features. Green
technology is becoming popular recently. Microwave-assisted extrac-
tion (MAE) and OAHD, for example, have optimum heating mechan-
isms, they are cost-effective, and exhibit better performance when at-
mospheric conditions prevail. Shorter durations of time are required by

⁎
Corresponding author.
E-mail addresses: akarami2004@gmail.com, akbarkarami@shirazu.ac.ir (A. Karami).

https://doi.org/10.1016/j.scp.2018.03.002
Received 11 November 2017; Received in revised form 11 March 2018; Accepted 11 March 2018
Available online 21 March 2018
2352-5541/ © 2018 Elsevier B.V. All rights reserved.
R. Manouchehri et al.
MAE and OAHD for extraction to take place effectively. MAE and OAHD
are capable of producing higher extraction yields when viewed in
comparison with conventional extraction methods (Farahnaky et al.,
2010; Chan et al., 2011; Gavahian et al., 2011, 2013). Damask rose
industries partly focus on which extraction technology can be more
optimum as a better option compared with traditional methods. Both
OAHD and SFME are technologies that have received considerable at-
tention recently in the industry. Both have similar advantages including
the reduction in process time. Therefore, the aims of this study were to
compare the extraction yield, time of extraction, and the EO composi-
tion from fresh flowers of damask rose obtained by OAHD and SFME
methods in comparison to those obtained by the HD method.
2. Materials and methods
2.1. Plant materials
Damask rose fresh flowers were obtained from cultivated popula-
tions in their full flowering stage in Layzangan (Darab, Fars Province,
southern Iran). The plant species was specified and authenticated by A.
Khosravi, a plant taxonomist at Shiraz University, Shiraz, Iran. A spe-
cimen of voucher was related with the herbarium.
2.2. Solvent free microwave-assisted extraction (SFME)
SFME was performed in a modified way as described by Wang et al.
(2006). The EOs were obtained from fresh flowers of damask rose by
distillation without the use of solvents for 25 min using a Clevenger
type apparatus (Fig. 1). One hundred grams of damask rose samples
were placed in a modified microwave oven (ME343, Samsung, Korea,
230, 1550 W; variable in 110 W increments, 2450 MHz). The micro-
wave oven operated at 1000 W during the first 3 min and then at 400 W
for 22 min. All EOs from the sample were extracted in this period. Over
anhydrous sodium sulphate, the oil was dried and conserved in brown
sealed vials at 4 °C for further use.
2.3. Ohmic assisted hydrodistillation (OAHD)
OAHD was carried out employing an ohmic distillatory tool and
platinum electrodes in the Department of Food Science and Technology
of Shiraz University, Shiraz, Iran (Fig. 1). Processing variables like
temperature, processing time, and power consumption were controlled
applying a software application coupled with a Wattmeter to record the
ohmic apparatus input power to check the software data. OAHD was
done at 220 V, 50 Hz, and at differing current rates in accordance with
the time of process (Farahnaky et al., 2010). To eliminate water, the
extracted EOs were dried on anhydrous sodium sulphate and kept at
Fig. 1. Solvent free microwave-assisted extraction (A); Ohmic assisted hydrodistillation (B) apparatuses set-up.
77
Sustainable Chemistry and Pharmacy 8 (2018) 76–81
4 °C in amber vials for further trials.
2.4. Hydrodistillation (HD)
HD was performed as SFME, applying a heater (FINTECH; Korea;
and 500 W). The proportions and volume of the operated container
were alike those employed for MAHD. Fresh flowers of the damask rose
(100 g) and 500 mL distilled water were put in a round bottom flask and
linked to a Clevenger-type device. After boiling, HD was completed for
three h. The sample's oil yield was estimated on a moisture free basis.
Over anhydrous sodium sulphate, the oil was dried and was stored in
sealed brown vials at 4 °C.
2.5. Physical constants
Specific gravity of the EOs from the fresh petal of damask rose was
estimated based on Food Chemical Codex (FCC) (FCC, 1996) at 25 °C.
2.6. Analysis of the oil
GC analysis was done on over Agilent 7890-A GC with the help of a
Flame Ionization Detector (FID) using a HP-5 fused silica capillary
column (30 m × 0.32 mm i.d.; film thickness 0.25 µm; J & W Scientific,
Folsom). The temperatures of injector and detector were, respectively,
250 and 280 °C. As a carrier gas, nitrogen was applied at 1 mL/min flow
rate, and in the split mode, 0.1 μL of EO samples diluted in n-hexane
were injected. The temperature of oven was programmed from 60 °C to
210 °C with a gradient of 4 °C/min, and then increased to 240 °C with a
gradient of 20 °C/min and isothermally kept for 8.5 min. A split ratio of
1:50 was maintained.
The same Agilent gas chromatograph as above coupled with a mass
spectrometer detector (Model 5975 C) and equipped with a HP-5 MS
fused silica capillary column (30 m × 0.25 mm i.d.; film thickness
0.25 µm; J & W Scientific, Folsom) was used to conduct the GC/MS
analysis. Helium was employed as a carrier gas. The source of ion and
interface temperatures of 230 °C and 280 °C were employed, respec-
tively. 70 eV ionization voltage was applied. The range of mass was set
between 45 and 550 amu. The temperature of oven programme was as
the temperature used for GC-FID. The temperature-programmed
Retention Indices (RIs) of EO components were calculated using a
mixture of n-alkanes (C8-C25) and the same chromatographic conditions
as above and compared with those expressed in previous studies
(Adams, 2007). In addition, their mass spectra and those contained in
mass spectral libraries (Willey/ChemStation data system and NIST 08/
National Institute of Standards and Technology) were compared. The
percentages of relative region estimated via FID were utilized for
quantification with no application of the correction parameters.
R. Manouchehri et al.
Table 1
Effect of extraction methods on starting time of oil accumulation, extraction duration, essential oils yield and specific gravity of damask rose.
Extraction Process Yield (%) Process starting time for oil accumulation (min)
SFME ** 0.056 a* ± 0.002 2.5c ± 0.29
OAHD 0.047 b ± 0.002 17.3 b ± 0. 33
HD 0.033c ± 0.002 42.6 a ± 0.32
* The same letters in each column indicate that the means are not significantly different (p < 0.05).
**SFME, Solvent free microwave-assisted extraction, OAHD, Ohmic assisted hydrodistillation; HD, Hydrodistillation.
2.7. Statistical analysis
The statistical significance of differences between treatments was
concluded by analysis of variance (ANOVA) and then the testing pro-
cess for variations among mean values was determined using Duncan's
novel multiple-range test and SPSS 21 at p ≤ 0.05. Data were provided
as mean values ± standard deviation (SD).
3. Results and discussion
3.1. Comparison of temperature profiles of the extraction methods
The profiles of temperature in OAHD, SFME, and HD extractions are
given in Table 1. For achieving temperature of extraction (almost
100 °C) and to get the first EO droplets’ evaporation with steam, the
mixture was heated for 2.50 ± 0.29 min in SFME and 17.33 ± 0.33 in
OAHD while it was higher than 40 min for HD (42.66 ± 0.32 min). The
data show meaningful differences among novel and conventional
methods based on the temperature increment rate and extraction with
SFME and OAHD. Gavahian et al., 2015 demonstrated that this measure
by OAHD and MAHD in fresh aerial parts of peppermint is relatively
similar. By the HD, it requires almost 30 min to evaporate the initial EO
droplets. Here, the SFME and OAHD methods started the build-up of
essential oils quite earlier than the HD. It is known that the SFME
gathers the first droplets of oil when almost three minutes has elapsed.
But the OAHD gathers the first droplets after about 17 min. Previously,
it was reported that non-thermal ohmic heating (electroporation)
makes membranes and cell walls penetrable. This was performed by the
OAHD, in the presence of an electric field, which facilitated EOs as they
were extracted from mint glands (Gavahian et al., 2015).
3.2. Comparison of total extraction time
The total extraction durations of EOs from damask rose was com-
pared between the novel extraction methods (SFME and OAHD) and the
traditional method of extraction (HD). As shown in Table 1, the ex-
traction of SFME started much earlier than OAHD methods (about
24.67 ± 0.031 min for SFME and more than 42 min (42.33 ± 0.033)
for OAHD). In other words, OAHD and SFME need durations that are 6
and 10 times shorter than that required by HD. Additionally, a mean-
ingful variation was seen among conventional and green extraction
procedures based on total time of extraction. This is because of the
effective heating in the microwave and ohmic assisted extraction
methods. In contrast to the conventional conductive heating proce-
dures, microwave and ohmic method may increase the temperature of
the whole sample by a higher rate. This shows that they are capable of
instilling heat in products quickly (Sastry, 2005; Goullieux and Pain,
2005; Gavahian et al., 2015). Even though the heating mechanism in
SFME is not similar to OAHD, they can heat the mixture quicker com-
pared with HD and, so, this can decrease the needed time for the pro-
cess of extraction to progress.
3.3. Comparison of essential oil yield
extraction procedure impact on EO yield is shown in Table 1. As the
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Sustainable Chemistry and Pharmacy 8 (2018) 76–81
Total extraction time (min) Specific gravity
24.65c ± 0.031 0.766 a ± 0.006
42.33 b ± 0.033 0.766 a ± 0.006
236.67 a ± 1.63 0.766 a ± 0.007
data shows, the more novel methods (SFME and OAHD) caused higher
recovery of oil by comparison with the traditional studied method (HD)
which completed oil recovery after more than 236 min. Therefore, the
shorter amount of time needed to complete oil recovery is a noticeable
advantage prioritizing these novel extraction procedures compared
with conventional procedures. The EO yield mean value in SFME was
superior to OAHD. The EO isolation yield in SFME is 17% more than
OAHD (0.056% for SFME vs. 0.047% for OAHD). Owing to lower
electrical conductivity of EOs and plant material, OAHD can merely
heat the surrounding area; therefore, the ohmic heating operates in the
water chronic stage, because of the requirement of ionic mobility, and it
cannot directly heat low electrical conductivity materials similar to
droplets of oil in mixed systems (Goullieux and Pain, 2005). Unlike
conventional systems, SFME heats the material by microwave – a type
of internal heating. Accordingly, biomaterials are exposed to micro-
waves which pass through, thereby heating up the whole of the plant
material. This means that heating occurs more quickly by the SFME, in
comparison to HD (Singh and Heldman, 2001; Gavahian et al., 2015).
Sahraoui et al. (2008) extended a novel procedure to extract dry
lavender flowers (Lavandula angustifolia Mill.) named microwave steam
distillation (MSD), and evaluated it to set a contrast with traditional
steam distillation (SD). EOs separated by SD and MSD were qualita-
tively and quantitatively alike; however, MSD was superior than SD as
speediness is concerned (6 min vs 30 min, respectively). An additional
effort was made by Wang et al. (2006) who developed a new extraction
technique of EOs extraction from C. cyminum L. and Zanthoxylum bun-
geanum which they called microwave-assisted hydrodistillation
(MAHD). A similar yield of the EO extracted from Thymus vulgaris took
a significantly shorter extraction time compared to HD when using
MAHD by Golmakani and Rezaei (2008). This made the extraction
process require less energy and was therefore extra sustainable. One of
the most optimum and most common methods, used as a modified
method of MAE, for the extraction of EOs, is the solvent free micro-
wave-assisted extraction (SFME). As compared with conventional
techniques, SFME considerably reduces the extraction time ranging
from a few hours to 20–30 min when extracting EO. Furthermore, it is
characterized by a medium resource and low operating charge of en-
ergy (Chan et al., 2011). The EOs extracted from cardamom essential oil
(Eletaria cardamomum L.) by SFME are more valuable compared with
those extracted by HD because of the superior amount of oxygenated
compounds relevant to highly aromatic compounds. These factors make
SFME a better extraction method compared to HD (Lucchesi et al.,
2007). Although MAE has been effectively used in laboratory condi-
tions, the number of scale up instances stay low (Leonelli and Maso,
2010; Stratakos and Koidis, 2016).
3.4. Effects of extraction method on the physical attributes
The physical properties (specific gravity) of damask rose EOs ex-
tracted via OAHD, SFME, and HD are given in Table 1. no meaningful
variation was found regarding specific gravity among the evaluated
methods. Research by Gavahian et al. (2015) reported that no sig-
nificant differences exist among physical properties of mint EOs (i.e.
their refractive index, specific gravity, and color) while they were ex-
tracted using methods of OAHD, MAHD, and HD. By studying the
R. Manouchehri et al. Sustainable Chemistry and Pharmacy 8 (2018) 76–81

Table 2 Table 2 (continued)

Chemical composition of damask rose essential oil obtained through HD, OAHD and
SFME. NO Compound RI* Chemical HD OAHD SFME
Class
NO Compound RI* Chemical HD OAHD SFME Compounds (%)
Class
Compounds (%) 70 Salvial− 4(14)-en− 1- 1590 AH – – 0.29
one
1 Heptanal 900 A 0.19 0.15 – 71 n-Hexadecane 1597 AH 0.21 0.15 0.19
2 α-Pinene 931 MH 0.14 0.26 t 72 Dill apiol 1622 B/Ph – – –
3 Camphene 946 MH – 0.07 – 73 γ-Eudesmol 1629 OS – – –
4 Benzaldehyde 957 A 0.02 0.01 – 74 epi-α-Cadinol 1639 OS – – –
5 n-Heptanol 963 AH 0.02 0.01 – 75 β-Eudesmol 1646 OS 0.06 0.09 –
6 Sabinene 970 MH t T – 76 n-Heptadecane # AH 3.79 3.09 4.43
7 β-Pintene 975 MH 0.04 0.03 – 77 (Z,Z)-Farnesol 1719 OS 0.23 0.2 –
8 3-Octanone 982 AH – 0.04 – 78 Benzyl benzoate 1760 B/Ph 0.13 0.21 0.36
9 6-methyl− 5- 983 A 0.01 – – 79 n-Tetradecanoic acid 1764 FA – – –
Hepten− 2-one 80 (E)−7-Octadecene 1772 AH 0.14 0.1 0.21
10 Myrcene 988 MH 0.06 0.09 t 81 n-Octadecane 1798 AH 0.49 0.45 0.86
11 n-Octanal 1001 A – – 0.02 82 6,10,14-trimethyl− 2- 1840 AH – – –
12 α-Phellandrene 1004 MH – – – Pentadecanone
13 α-Terpinene 1015 MH 0.01 0.03 – 83 Phenyl ethyl octanoate 1847 AH 0.23 0.26 0.39
14 p-Cymene 1022 MH t 0.08 – 84 1-Nonadecene 1874 AH 7.09 5.41 8.06
15 Limonene 1026 MH 0.26 0.17 0.03 85 n-Nonadecane 1900 AH 19.03 19.93 30.36
16 1,8-Cineole 1029 OM t 0.14 0.01 86 n-Hexadecanoic acid 1963 FA – – –
17 Benzyl alcohol 1030 B/Ph 0.02 0.03 – 87 1-Eicosene 1975 AH 0.36 0.26 0.5
18 (Z)-β-Ocimene 1034 MH t t – 88 Ethyl palmitate 1999 FA – – 0.57
19 Benzene acetaldehyde 1040 A 0.08 0.07 0.01 89 n-Eicosane 2003 AH 2.38 2.45 4.85
20 (E)-β-Ocimene 1044 MH 0.01 t – 90 10-Heneicosene 2093 AH 0.37 0.5 0.49
21 γ-Terpinene 1055 MH 0.03 0.09 – 91 n-Heneicosane 2105 AH 9.25 10.41 17.54
22 cis-Sabinene hydrate 1064 OM – t – 92 Ethyl linoleate 2169 FA – – 0.21
23 n-Octanol 1066 FA – – t 93 Ethyl stearate 2197 FA – – 0.3
24 trans-Linalool oxide 1069 OM 0.02 – – 94 Linoleic acid 2152 FA – – –
25 Terpinolene 1086 OM 0.02 0.05 – 95 n-Docosane 2201 AH 0.27 0.29 0.69
26 Linalool 1098 OM 0.42 0.95 0.07 96 1-Tricosene 2292 AH 0.31 0.51 1.11
27 n-Nonanal 1102 A 0.1 0.13 0.03 97 n-Tricosane 2307 AH 1.71 2.33 4.42
28 Phenyl ethyl alcohol 1110 B/Ph 2.25 2.63 0.73 98 n-Tetracosane 2402 AH 0.15 0.19 0.37
29 trans-Rose oxide 1125 OM 0.46 0.2 0.07 99 n-Pentacosane 2506 AH 0.43 0.79 1.84
30 Camphor 1142 OM – 0.13 0.03 C/G Ratio 8.12 8.46 41.78
31 Citronellal 1150 OM 0.07 0.11 0.02 Monoterpene Hydrocarbon MH 0.56 0.87 0.03
32 Nerol oxide 1151 OM 0.1 0.05 0.01 Oxygenated Monoterpene OM 42.27 38.49 14.7
33 Borneol 1163 OM – 0.16 0.03 Sesquiterpene Hydrocarbon SH 1.64 2.41 1.59
34 Terpinene− 4-ol 1174 OM 0.19 0.36 0.05 Oxygenated Sesquiterpene OS 0.38 0.73 1.62
35 α-Terpineol 1188 OM 0.12 0.13 0.03 Aliphatic Hydrocarbon AH 46.94 47.76 76.95
36 n-Dodecane 1197 AH – – – Benzenoid/Phenylpropanoid B/Ph 6.15 7.15 2.48
37 n-Decanal 1203 A 0.04 0.06 0.02 compound
38 Citronellol 1226 OM 36.15 31.05 13.37 Aldehyde A 0.43 0.42 0.08
39 Nerol 1231 OM – 0.13 – Fatty Acid FA – – 1.08
40 Neral 1238 OM – – – Ester E 0.93 1.48 0.3
41 Carvone 1242 OM – – – Total 99.31 99.31 99.04
42 Geraniol 1255 OM 4.45 3.67 0.32
43 Geranial 1268 OM – – – RI, Retention Index; HD, Hydrodistillation; OAHD, Ohmic assisted hydrodistillation; SFME,
44 2-Phenyl ethyl acetate 1256 E – – 0.04 Solvent free microwave-assisted extraction; C/G ratio, Citronellol/Geraniol; MH, Monoterpene
45 Citronellyl formate 1273 OM 0.06 0.07 0.02 Hydrocarbon; OM, Oxygenated Monoterpene; SH, Sesquiterpene Hydrocarbon; OS,
46 Bornyl acetate 1284 E – 0.54 0.04 Oxygenated Sesquiterpene; AH, Aliphatic Hydrocarbon; B/Ph, Benzenoid/
47 Thymol 1291 OM 0.04 0.65 0.2 Phenylpropanoid compound; A, Aldehyde; FA, Fatty Acid; E, Ester.
48 Carvacrol 1301 OM – 0.53 0.44
49 Geranyl formate 1301 OM 0.05 – –
50 Methyl geranate 1322 OM 0.14 0.16 0.06 extracted EOs physically, it is suggested that SFME and OAHD could be
51 Citronellyl acetate 1352 E 0.45 0.52 0.22 considered as extraction procedures that do not alter the physical
52 Eugenol 1355 B/Ph 1.52 1.81 0.14 properties of the EOs significantly when extraction is performed on the
53 Neryl acetate 1364 E 0.18 – –
damask rose.
54 α-Copaene 1373 SH – – 0.07
55 β-Bourbonene 1382 SH – – 0.1
56 Geranyl acetate 1382 E 0.3 0.42 –
57 β-Elemene 1389 SH 0.1 0.14 0.12 3.5. Effects of extraction methods on essential oil components
58 Methyl eugenol 1404 B/Ph 2.23 2.47 1.25
59 (E)-Caryophyllene 1416 SH 0.25 0.43 0.2 This research analyzed the EOs and demonstrated that fluctuations
60 α-Guaiene 1436 SH 0.26 0.33 0.2
may occur in the chemical profile of the damask rose with respect to the
61 α-Humulene 1450 SH 0.22 0.33 0.17
62 Germacrene D 1478 SH 0.59 0.91 0.55 quantity of their constituents because of the extraction method. The
63 n-Pentadecane 1497 AH 0.68 0.53 0.56 structure of extracted molecules may also be modified as a result of the
64 α-Bulnesene 1503 SH 0.22 0.27 0.18 extraction procedure, which affects the properties of the EOs, de-
65 α-Cadinene 1520 SH – – – pending on the extraction method. Components were identified in the
66 (E)-Nerolidol 1561 OS 0.06 0.12 –
67 Spathulenol 1576 OS – 0.11 0.64
EOs of damask rose petals, as extractions were performed by methods of
68 Caryophyllene oxide 1580 OS 0.03 0.21 0.98 SFME, OAHD and HD (Table 2 and Fig. 2). A total of 99 components are
69 2-Phenyl ethyl tiglate 1582 AH 0.03 0.06 – reported in Table 2 which constitute a percentage exceeding 99.3% of
the overall GC peak zones. Similar compositions were observed in the
EOs extracted through the conventional methods and by the green

79
R. Manouchehri et al.
Fig. 2. Hierarchical cluster analysis of chemical composition in damask rose essential oil
obtained through HD, OAHD and SFME. FAD, n-Octanol, Ethyl palmitate, Ethyl linoleate,
Ethyl stearate; BAL, Benzaldehyde, Benzyl alcohol, Benzene acetaldehyde, Benzyl
benzoate; PHE, Phenyl ethyl alcohol, 2-Phenyl ethyl acetate; EUG, Eugenol, Methyl eu-
genol; GER, Geraniol, Geranyl formate, Methyl geranate, Geranyl acetate; NER, Nerol
oxide, Nerol, Neryl acetate; CIT, Citronellal, Citronellol, Citronellyl formate, Citronellyl
acetate; TER, α-Terpinene, γ-Terpinene, Terpinolene, Terpinene-4-ol, α-Terpineol; MON,
α-Pinene, Camphene, Sabinene, β-Pinene, Myrcene, p-Cymene, Limonene, (Z)-β-
Ocimene, (E)-β-Ocimene, cis-Sabinene hydrate; OXM, 1,8-Cineole, trans-Linalool oxide,
Linalool, trans-Rose oxide, Camphor, Thymol, Carvacrol; BOR, Borneol, Bornyl acetate;
SES, α-Copaene, β-Bourbonene, β-Elemene, (E)-Caryophyllene, α-Guaiene, α-Humulene,
Germacrene D, α-Bulnesene; OXS, (E)-Nerolidol, Spathulenol, Caryophyllene oxide, b-
Eudesmol, (Z, Z)-Farnesol; ALD, Heptanal, 6-methyl-5-Hepten-2-one, n-Octanal, n-
Nonanal, n-Decanal; COS, 1-Eicosene, n-Eicosane, 10-Heneicosene, n-Heneicosane, n-
Docosane, 1-Tricosene, n-Tricosane, n-Tetracosane, n-Pentacosane; DEC, n-Pentadecane,
n-Hexadecane, n-Heptadecane, (E)−7-Octadecene, n-Octadecane, 1-Nonadecene, n-
Nonadecane; ALK, n-Heptanol, 3-Octanone, 2-Phenyl ethyl tiglate, Salvial-4(14)-en-1-
one, Phenyl ethyl octanoate; HD, Hydrodistillation; OAHD, Ohmic assisted hydro-
distillation; SFME, Solvent free microwave-assisted extraction.
Fig. 3. Effect of extraction methods on the main essential oils components of damask
rose; HD, Hydrodistillation; OAHD, Ohmic assisted hydrodistillation; SFME, Solvent free
microwave-assisted extraction.
methods studied herein. This study reports that the extracted EOs ex-
hibited the same components when extractions were performed by the
different methods. The compounds were namely citronellol
(13.37–36.15%), geraniol (0.32–4.45%), n-nonadecane
(19.03–30.36%), n-henicosane (9.25–17.54%) and phenyl ethyl alcohol
(PEA) (0.73–2.63%) (Fig. 3). Previous reports approve of the fact that
the most abundant components in the EOs of damask rose are also the
main components found here in this research (ISO, 9842, 2003; Verma
et al., 2011; Rusanov et al., 2011; Rusanov et al., 2012; Karami et al.,
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Sustainable Chemistry and Pharmacy 8 (2018) 76–81
2012). Furthermore, some components present in the extracted EO
were different in their quantity when the HD was used and when the
SFME and OAHD were used. The results of EO analysis indicated con-
siderable variations in EOs compounds achieved using SFME method
compared with with OAHD and HD. The major oil components obtained
by the extraction methods were citronellol, geraniol, n-nonadecane and
n-henicosane. The results showed HD and OAHD produced yields with
higher amounts of citronellol and geraniol, C/G ratio, PEA, while lower
amounts of n-nonadecane and n-henicosane were observed. It was
found that the oil obtained from the petals extracted by HD and OAHD
exhibited a higher percentage of typical constituents of rose oil as well
as a suitable ratio of C/G. However, SFME increased the C/G ratio
(Table 2). On the other hand, extraction methods were observed in this
study to have significant effects on C/G ratio, and therefore could alter
oil quality. Previous studies on rose oil claim the unbalanced rate of C/
G originated by extended storage and distillation time of the flowers
(Baydar et al., 2008; Baydar and Baydar, 2005; Mirzaei et al., 2016).
The main components in the EO extracted from rose flowers were ci-
tronellol and nonadecane. Furthermore, nonadecane is the richest hy-
drocarbon present in rose oil (Mohamadi et al., 2013). Considerably
greater hydrocarbons values exist the EO of rose flowers extracted by
SFME, compared to the EOs extracted using OAHD and HD (30.36%
versus 19.03% and 19.93%, respectively). While a low content of hy-
drocarbons is not expected to be seen in high quality rose oil (Baydar
and Baydar, 2005; Mohamadi et al., 2013), high contents quantified
here are relatively natural. Moreover, oil of rose is specified by great
percentages of perfume-diffusing alcohols involving geraniol, ci-
tronellol, and phenyl ethyl alcohol. In the present study, geraniol, ci-
tronellol, and phenyl ethyl alcohol percentages in the oils obtained by
SFME were lower compared to oils obtained by HD and OAHD. Eugenol
is usually reported as a component present in rose oil odor, whereas
methyl eugenol has negative side-effects on human health and is not
safe to be available in amounts more than a certain concentration
(Rusanov et al., 2012; Baydar and Baydar, 2005; Mohamadi et al.,
2013). As seen from Table 2, using SFME instead of HD and OAHD for
distillation of rose flowers caused a considerable decrease in the re-
lative contents of methyl eugenol and eugenol. The antioxidant activ-
ities differed in EOs of Tetraclinis articulata obtained by different ex-
traction methods including solvent extraction, HD, and SFME (Herzi
et al., 2013). In addition, the EO extracted by SFME was more active
than the oil extracted by HD, when considering their response to Gram-
positive and negative bacteria. It seems that the higher contents of
oxygenated compounds generate high antibacterial and antifungal
properties (Okoh et al., 2010). The composition of EOs extracted by the
different methods are comparable, meaning that the relative con-
centrations of identified compounds could be different, which causes
differences in oil attributes. Therefore, the type of extraction must be
decided upon in relation to the EO intended for extraction (Stratakos
and Koidis, 2016).
4. Conclusion
The EOs extracted compositions by all techniques were alike; hence,
components obtained through conventional techniques were observed
in the green procedures. In addition, meaningful differences were ob-
served among some components’ quantities obtained via HD and those
extracted via SFME and OAHD. The results of EO analysis indicated
considerable alterations in EOs compounds gained through new and
green method (SFME and OAHD) in comparison with HD. As compared
with conventional techniques, SFME noticeably reduces the extraction
time and increases EO yields. In other words, compared to HD extrac-
tion technique, SFME and OAHD could be regarded as examples of
green technology as they consume notably less energy amounts for
operation. Such privileges can make SFME and OAHD preferable ex-
traction methods that are unconventional for the optimum extraction of
EOs. Consequently, extraction of EO from rose flowers with SFME and
R. Manouchehri et al.
OAHD present crucial benefits over traditional HD concerning saving
time of extraction, energy, and extraction yield. Nevertheless, a notable
increase was observed in percentages of hydrocarbon and decrease in
percentages of monoterpene alcohol when using the SFME method for
EO extraction, a drawback from a qualitative perspective. The conclu-
sions of this study are in accordance with prior studies relevant to green
technology and its applications.
Acknowledgments
We would like to thank Shiraz University (Grant no:
93GCU3M154198) for providing the grant of this research.
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