Jurnal ILMU DASAR, Vol.20 No.

2, Juli 2019 : 67-74 67

Essential Oil Composition of Rose Flowers from Karangpring Village

Jember District Extracted by Distillation and Enfleurage
Komposisi Minyak Atsiri Bunga Mawar dari Desa Karangpring Kabupaten
Jember yang diekstrak melalui Distilasi dan Enfleurasi
Ika Oktavianawati1*), Nanda Letisya1, Priscillia Citra1, Dwi Purwita Utari1, I Nyoman Adi
Winata1, Wuryanti Handayani1, Ari Satya Nugraha2
1
Dept. Chemistry, Faculty of Mathematics and Natural Sciences, University of Jember
2
Faculty of Pharmacy, University of Jember
*
E-mail: [email protected]
ABSTRACT
Karangpring is one tourist destination villages in Jember district which is popular with beautiful
large rose field areas. Therefore, this area grows to be a leading producer of rose flowers in Jember
district. However, the bulky presence of these flowers made its price becomes lower in regular
days. Local community only uses and sells these fresh flowers as the flower for funeral. The rose
flower has a great potency to be explored as a source of rose essential oil production. To date,
there is no previous research on studying rose flowers from Karangpring village for its potency on
the essential oil production. In this research, rose flowers were subjected to be extracted of its
essential oil using two extraction methods, distillation, and enfleurage. Hydrodistillation resulted
two phases of distillates, above part formed a cloudy white phase as a normal essential oil
extracted from plants, and the lower phase was an aqueous phase containing rose hydrosols. Both
phases of these condensates were analyzed using GCMS. Data explained that above phase, with a
yield oil of 0.07%, only contains long-chain hydrocarbons such as n-nonadecane, n-heptadecane,
9-nonadecene, and eicosane, while the lower phase only contains 2-phenylethyl alcohol. On the
other hand, enfleurage of fresh rose flowers resulted in 0.06% oil yield. GCMS analysis of this oil
shows that 2-phenylethyl alcohol, eugenol, and phenylacetic acid are three major compounds
which take more than 85% of total rose absolute. The results show that enfleurage is a better
method for extracting rose oil in better quality than using the distillation method, in term of the
variety of volatile components. Meanwhile, hydrodistillation is still benefiting from producing
rose water that is qualified as an industrial additive agent for food and cosmetic productions or
even a new potent of agromedicine products.
Keywords: rose, rose oil, rose water, rose absolute, distillation, enfleurage.
INTRODUCTION from rose flowers which attracts the attention
of the world is the production of rose
Rose flower has an economic and social value
oil,known as rose otto, in flavor and fragrance
in the world, especially the Indonesian
industry (Kovats, 1987). Since rose oil is one
community. Some communities regularly use
of the most expensive essential oil in the world
the flower as cut roses for many special events,
market today, we proposed the way on the
such as birthday and wedding parties, also for
diversification product of rose flower as
funeral and cemetery flowers. Karangpring
essential oil production in this research
village is a leading producer and supplier for
(Agaoglu, 2000; Kovacheva et al. 2010).
rose flowers in Jember district (Derap Desa,
The main flavor component on the scent of
2010; Arifin, 2017b). Local communities in
Karangpring village frequently use rose rose flowers are  -damascone and  -
damascenone (Pal, 2013). Nevertheless, it is
flowers only as formal flowers for cemetery
also known that characteristic odor of rose
and funeral aim. Some also produce healthy
flowers came from 2-phenylethyl alcohol
labeled juice from rose flowers, or even as rose
which being a principal component in rose
candies, teas, and crackers (Arifin, 2017a).
Others also use rose water in cooking as a water (Watanabe et al. 2001; Sakai et al. 2007;
natural coloring agent (Saati et al. 2011), Sakai et al. 2008; Kumar et al. 2014; Gunes,
2005; Hirata et al. 2016). Previous researches
flavoring agents on desserts and many meat
explained that bioactive molecule of 2-
dishes (Karizaki et al. 2016; Alalwan et al.
phenylethyl alcohol inside rose flowers is in
2017). However, another valuable product

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68 Essential Oil Composition of Rose Flowers … (Oktavianawati, dkk)

the form of 2-phenylethyl -D-glucopyranoside dimethyl ketone, acetaldehyde, sulfides,

(Eikani et al. 2005; Watanabe et al. 2002). ammonia and methanol (Soe’eib et al. 2016;
However, most publications only mention the Muchtar et al. 2013; Yulianingsih et al. 2007;
finding on aglycon part of it, i.e. 2- Oktavianawati et al. 2017).
phenylethylalcohol. It was assumed that instead Various rose extracts depending on the way
of the presence of  -glucosidase inside the they were extracted, have their names. Rose oil
plant (Watanabe et al. 2001; Sakai et al. 2008), is normally obtained from the upper phase of
applying various pretreatment and extraction distillate from steam, steam-water, and
methods could hydrolyze the glycoside as well hydrodistillation methods. Rose concrete is
to produce 2-phenylethyl alcohol. obtained by solvent extraction of rose flowers
Some efforts have been made to extract and has a smooth like semi-solid performance,
rose oil with higher quality, meaning that it has while rose absolute is derived from rose flower
a high content of rose alcohol, but low or even extraction using ethanol as solvent. Rose water
free of ester, higher alkanes, and fat (Eikani et is collected from the lower phase of distillate
al. 2005). Various methods to extract rose oil which also contains a valuable oxygenated
are distillation (Najem et al. 2011; Hosni et al. compound which is responsible for the great
2010; Agarwal et al. 2005), solvent extraction odor of rose flowers (Ulusoy et al. 2009).
(Rusanov et al. 2011; Watanabe et al. 2001; To date, there was no previous
Kurkeuoglu and Baser, 2003), enfleurage investigation on exploring essential oil from
(Yulianingsih et al. 2007), and supercritical rose flowers in Jember district. Then, this
CO2 (Reverchon et al. 1997). Kumar et current paper will discuss the potency of rose
al.(2016) have applied distillation of Damask essential oil production and compare the oil
rose flowers with saline water containing 75 g quality, in terms of GCM analysis data,
NaCl/kg of rose flowers to increase about 42% because of applying different extraction
higher of rose oil content compared to methods.
distillation in water only. But there is a special METHODS
consideration on applying this method in a
significant scale process due to the Materials
adverseeffect of salt on damaging steel Fresh rose flowers were obtained from a rose farmer
community, Sumber Mawar, in Karangpring village,
apparatus in a longer period.
Jember district, from May to July 2018. Rose
Most of all, the use of hydrodistillation in plantsthat were used in this research has been
kinds of literature is quite widespread for identified by Lembaga Ilmu Pengetahuan Indonesia
extracting rose oil from fresh rose flowers. It (Indonesian Institute of Sciences) Balai Konservasi
has been known that hydrodistillation product Tumbuhan Kebun Raya Purwodadi as Rosa hybrida
market value is higher than other product from Hort.
different extraction methods, by the fact that Extraction Procedures
the total number of essential oil components in Hydrodistillation
hydrodistillation is over (Pal 2013). Research The whole flower of roses was used in new
by Karmous et al. (2004) mentioned that conditions and extracted by hydrodistillation method
hydrodistillation has a drawback that the effect using a Clevenger apparatus for 4 hours. The
of boiling floral material and water at the same condensate formed two phases of distillate. The
time could lead a light burned odor in the final upper phase was collected as rose oil, while the
product of essential oil. Since hydrodistillation lower phase was rose water. Rose oil was subjected
is also quite easy and inexpensive, then this to further analysis using GCMS. Rose water was
extracted using diethyl ether to obtain rose concrete
method became economical for essential oil and then was run for GCMS analysis as well.
production and suitable to be applied to the
Enfleurage
local community as a kind of home industry.
Chasis (50x50x7) was smeared with 500 grams of
Enfleurage also becomes a popular shortening (white butter). 200 grams of fresh rose
extraction method to produce absolutely flowers were placed on the top of fat from
because it applies a low temperature for shortening for five days. The flowers were changed
extraction. Hence, enfleurage prevents the in every 24 hours and substituted with the new fresh
hydrolysis of essential oil component during one in a similar weight. After five days, the fat
extraction that can be occurred at high containing essential oil was extracted using alcohol
temperature process, and creates an unpleasant in a ratio of 2:1. Then the mixture was kept in 0-5C
odour because of the presence of acetic acid, during 24 hours. Filtration of this mixture results
inpomade and extrait. Extrait was evaporated for its
Jurnal ILMU DASAR, Vol.20 No. 2, Juli 2019 : 67-74 69

alcohol content which then produced a rose absolute. also known as stereoptanes, including n-
Rose absolute was also analyzed for its volatile nonadecane, n-heptadecane, 9-nonadecene, and
content using GCMS. eicosane. In this term, the form of rose oil as a
Identification of Volatile Components wax-like material is possibly originating from
Volatile compounds of the essential oil extracts were the protective coatings of flowers which then
analyzed by GCMS-QP2010S Shimadzu with Rtx 5 makes the fat hardens and solidifies at room
MS column (length 30 m; ID 0.25 m; film 0.25 um),
temperature (Sterrett 1962). The presence of
Helium gas as a carrier, EI 70 Ev. Column oven
this stearopten guarantees the durability of the
temp.70C, injector temp. 300C, pressure 12 kPa,
total flow 27.3 mL/min, column flow 0.49 mL/min, scent (Dobreva et al. 2013).
ion source temp. 250C, interface temp.305C, Table 1. Chemical components in rose oil from
solvent cut time 3 min, detector gain +0.00 kV. MS Karangpring rose flowers
table, start time 3.20 min, end time 70 min, scan
speed 1250, event time 0.50 sec. The constituents of Retention
No Compound Names %
the oils were identified based on their chromatogram time
and by comparing their mass spectral data with those 1 33.509 9-nonadecene 11.64
from Wiley mass spectral database. 2 34.167 n-heptadecane 26.52
3 34.419 7-hexadecyne 1.00
RESULTS AND DISCUSSION 4 35.426 1-octadecene 0.59
5 35.708 Z-7-hexadecene 0.09
Hydrodistillation is a kind of distillation 6 37.427 10-heneicosene 1.59
method that boils the sample together with 7 38.292 n-nonadecane 38.52
water at the same time. Water molecules will trans-1,4-
diffuse into plant tissues and carry out essential 8 38.476 0.23
dihydroxycyclohexane
oil from oil glands to evaporate and condense. 9 41.502 E-5-octadecene 4.43
The oil will naturally be separated from the 10 41.735 eicosane 10.81
aqueous phase in the distillate. In this current 11 43.877 stearaldehyde 1.40
research, the expected rose oil from 12 45.546 tridecanaldehyde 0.08
hydrodistillation method was presented in the 13 48.178 n-hexatriacontane 2.84
14 50.982 octadecyl chloride 0.16
above phase of distillate and was separated
from rose water to yield 0.07% oil. The This result research was relevant with the
performance of this rose oil was in semisolid result of Moein et al. (2010) mentioning that
form with a white transparent waxy look when Rosa damascena Mill. from South of Iran
it was cooled at 0-5C or even at room contains nonadecane, heneicosane,
temperature. However, the odor of this rose oil docosaneand 9-nonadecene in a total amount of
does not represent the fragrance of rose 92.06% of the rose oil, while the rest comprises
flowers. citronellol and germacrene-D. Our result
showed a relative big different on the
composition of rose essential oil from other
research that also used hydrodistillation to
extract rose oil. Babu et al. (2002) confirmed
that damask rose oil from the western
Himalayas contains rose alcohols (such as
citronellol, nerol, and geraniol) up to 68.13%
and long-chain hydrocarbons including
nonadecane, heptadecane, 9-eicosene, and
docosane for about 21.23% of the total oil.
Figure 1. A chromatogram of rose oil from Dobreva et al. (2013) also enlighten the major
hydrodistillation method volatile contents of three genotypes of oil-
Chromatogram of this rose oil can be seen bearing roses in Kazanluk are mostly consist of
in Figure 1, while the name list of those citronellol, geraniol, nerol and nonadecane.
volatile compounds can be seen Table 1. Phenylethyl alcohol, as a marker compound of
GCMS analysis showed that this rose oil only rose flower, is also obtained from this research
contains saturated and unsaturated aliphatic though , in trace quantity, 0.26-1.31% of total
long chain hydrocarbon compounds, which is rose oil since it is a polar compound and more
soluble in water.

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70 Essential Oil Composition of Rose Flowers … (Oktavianawati, dkk)

Figure 2. A chromatogram of rose water Figure 3. A chromatogram of rose absolute

extracted with diethyl ether from five days enfleurage of fresh
rose flowers.
It has been discussed before that upper
phase of distillate, rose oil, contains only Enfleurage method is chosen as an
aliphatic hydrocarbons, while the lower phase alternative method to extract essential oil from
only contains one polar and soluble compound fresh rose flowers instead of hydrodistillation.
in water, 2-phenylethyl alcohol (see Enfleurage applies cold fat as an adsorbent of
chromatogram in Figure 2). This marker volatile compounds deliberated by flowers.
compound of rose oil was obtained when the This research used a white butter or shortening
lower distillate, as we knowas a hydrosol, was as an adsorbent.
extracted using diethyl ether.Evaporation of Table 2. Chemical components of rose absolute
diethyl ether resulted in a clear colorless liquid from enfleurage of fresh rose flowers
form of rose concrete. The odor of this extract
represents the right fragrance of rose flowers No.
Retention
Compound Names %
with a pleasant odour. In our research, we do time
not find any other volatile compounds that 1 3.448 2-propenoic acid 0.96
could be extracted from this rose water, like 2 3.889 glycolamide 3.56
3 13.857 Phenylethyl alcohol 40.48
other research which are conducted by
4 17.948 phenylacetic acid 12.91
Kurkeuoglu & Baser (2003), Eikani et al 5 20.789 eugenol 35.16
(2005),Najem et al (2011), Agarwal et al 6 22.793 -caryophillene 5.21
(2003) and Babu et al (2002), using various 7 23.778 -selinene 0.63
solvents ofn-hexane, n-butylacetate,pentane, 8 28.541 9-heptadecanone 1.09
and dichloromethane, respectively, to isolate
citronellol, geraniol, nerol, linalool and Enfleurage of fresh rose flowers for five
eugenol, instead of obtaining 2-phenylethyl days resulted in a0.06% oil yield with ‘a light
alcohol. yellow liquid majorly containing 2-phenylethyl
This current research confirmed that alcohol, eugenol and phenylacetic acid (Figure
hydrodistillation method is not a suitable 3 and Table 2). Research of Yulianingsih et al.
method to extract the true rose oil since it does (2007) shows that seven days enfleurage on
not contains any marker compound of rose similar adsorbent, i.e white butter, of Middle
flower, i.e 2-phenylethyl alcohol, or even any Java red roses brings about 0.239% of rose
other highly polar and water-soluble absolute containing 2-phenylethyl alcohol,
compound, while the rose water contains. citronellol, geraniol, nerol and also eugenol.
Thus, the distillation method could be chosen Although that we did not obtain any citronellol,
as the right method to produce valuable rose geraniol and nerol in our rose oil, we found that
water or hydrosol because of a big content of it also contains phenylacetic acid. Although
2-phenylethyl alcohol. This rose hydrosol was Watanabe et al. (2002) have explained that one
proven to be a safe material or additive in way of biogenesis of 2-phenylethyl alcohol
aromatherapy, cosmetics, andflavoring agents (route c) was from phenylacetic acid
since it did not contain any lipophilic intermedietthe presence of phenylacetic acid in
compounds that could interact and react with this research result was mostly predicted to
body tissues in topical application method became from the oxidation of 2-phenylethyl
(Adams et al. 2005). alcohol during enfluerage process. The
Jurnal ILMU DASAR, Vol.20 No. 2, Juli 2019 : 67-74 71

presence of natural oxidators such as rose Beside, rose water showed a mature content of
oxides and acids in enfleurage and defleurage rose flower marker compound, 2-phenylethyl
process could influence the stability of 2- alcohol, making this aromatic water to be a
phenylethyl alcohol. Moreover, possibility of precious candidate of flavor and aromatherapy
the presence of microbes inside chassis and the agent obtaining from the distillation process.
fat, such as Acetobacter acetic, will oxidize 2-
phenylethyl alcohol into corresponding acid ACKNOWLEDGEMENT
and aldehyde (Gandolfi et al. 2004).
We would like to acknowledge DRPM and the
Nevertheless, the rose absolute
University of Jember for providing research
performance from enfleurage is quite
and community engagement grant in 2017. We
impressive with a light yellow color oil and
also thankful to rose farmer community in
pleasant odor effect. There was no fat left from
Karangpring village, Jember district, for
adsorbent to be the presence in the rose
supplying the sample for research.
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