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GC-MS and FTIR analyses of oils from Hibiscus sabdariffa, Stigma maydis and
Chromolaena odorata leaf obtained from Malaysia: Potential sources of fatty
acids

Article · April 2019

DOI: 10.1016/j.cdc.2019.100200

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Data Article

GC–MS and FTIR analyses of oils from Hibiscus sabdariffa,

Stigma maydis and Chromolaena odorata leaf obtained from
Malaysia: Potential sources of fatty acids
Oluwaseun Ruth Alara∗, Nour Hamid Abdurahman
Centre of Excellence for Advanced Research in Fluid Flow (CARIFF), Universiti Malaysia Pahang, Lebuhraya Tun Razak, 26300, Gambang,
Pahang, Malaysia

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

Article history: Fatty acids are reduced carbon chains mostly found in nature with different usages in the
Received 29 November 2018 industrial feedstock, pharmaceutical and food industries. Plants are embodiments of sub-
Revised 6 February 2019
stantial amounts of fatty acids. In this study, gas chromatography-mass spectrometry (GC–
Accepted 12 February 2019
MS) analysis was employed to identify the chemical compositions of oils from Hibiscus
Available online 13 February 2019
sabdariffa flower, Stigma maydis; Chromolaena odorata leaf extracted through microwave-
Keywords: assisted hydrodistillation method. In addition, the oils from the three plant samples were
Microwave-assisted hydrodistillation characterized using Fourier transform infrared spectroscopy (FTIR) analysis to evaluate the
Gas chromatography-mass spectrometry fingerprints. A total number of 16, 13 and 13 chemical compounds were identified in the
Fatty acid oils from H. sabdariffa flower, S. maydis and C. odorata leaf, respectively. The main identified
Hibiscus sabdariffa compounds were fatty acids and esters. Moreover, the FTIR characterization reflected the
Stigma maydis presence of hydroxyl group, cellulose-fatty acids, methyl carboxylic acid, nucleic acid, and
Chromolaena odorata leaf carbohydrate. This finding has fully demonstrated that the oils from H. sabdariffa flower, S.
maydis and C. odorata leaf can serve as the potential sources of fatty acids.
© 2019 Elsevier B.V. All rights reserved.

Specification Table

Subject area: Natural product research

Data category: Chemical composition, functional group fingerprinting
Data acquisition: Mass spectrometry, Functional group characterization
Format: Figures, Tables
Data type: Analyzed
Procedure: The chemical compositions and function groups in the oils of Hibiscus sabdariffa; Stigma maydis; Chromolaena odorata leaves
were analyzed using gas chromatography-mass spectrometry and Fourier transform infrared, respectively.

1. Rationale

Oils from plants are widely utilized in aromatherapy since ages. This might suggest that they potentially possessed other
beneficial health properties in conjunction with their pleasant fragrances. There are a few unsaturated fatty acids that the
human body cannot generate unless obtained from foods. Double bonds after 3 to 6 carbon chains cannot be obtained from
animal fat, however, they can be acquired from plants [1]. Plants can synthesize omega-6 and omega-3 fats which are called

∗
Corresponding author.
E-mail address: ruthoalao@gmail.com (O.R. Alara).

https://doi.org/10.1016/j.cdc.2019.10 020 0
2405-8300/© 2019 Elsevier B.V. All rights reserved.
2 O.R. Alara and N.H. Abdurahman / Chemical Data Collections 20 (2019) 100200

‘essential’ fatty acids. Essential fats are in abundance in a diet of vegetables, fruits and starches [2]. Furthermore, oil from
the plant has no cholesterol, toxic waste, lead, mercury, and other heavy metals as compared to fishes [3]. In addition,
plants are excellent sources of not only essential fatty acids but also fibres, minerals, vitamins, proteins, and carbohydrates
[1]. Therefore, oils from plants are being consumed in recent times due to their unmeasurable health benefits.
Hibiscus sabdariffa belongs to the family Malvaceae are annual shrub commonly grown in tropical Africa, it can also be
found in India, Thailand and Malaysia [4]. It comprises of a reddish stem that can grow up to 3.5 m high, the leaves are
long-petiolate with red to dark green colour. The flowers are reddish in colour; they are mostly consumed as flavoured,
hot or tart cold beverages. Several studies had been carried out on H. sabdariffa. Previous studies had reported that the
presence of two specific anthocyanins (cyanidin-3-sambubioside and delphinidin-3-sambubioside) contributed wholly to its
reddish pigment of calyces [5]. The gas chromatography-mass chromatography (GC–MS) analysis of oil from H. sabdariffa
flower obtained from Nigeria showed the presences of linoleic acid (22.7%) and hexadecenoic acids of 64.3% [4]; the seed oil
from Austria showed oleic acid (24.7%), linoleic acid (43.2%) and palmitic acid (17.3%) as the major chemical compositions
[6]. However, α -terpineol and linalool dominated the seed oil from Cuba [7]. It can be observed that there is no uniformity
in the chemical compositions of the oil, it varied based on geographical locations. Thus, geographical location places an
important role in influencing the chemical compositions of plant extracts or oils.
Moreover, corn silk (Stigma maydis) is the stigmas maize (Zea mays) flower. It is thread-like strands from female maize
and yellow-brown or light green in colour. Corn silk is one of the major wastes from maize cultivation. It is readily available
every time in Malaysia because maize is cultivated throughout the year. The reports had shown that corn silk is being used
in traditional medications to treat kidney stones, urinary infections, oedema, cystitis, and obesity in France, Turkey, China,
and United States [8]. El-Ghorab et al. reported that Egyptian corn silk extract comprised of cis-sabinene hydrate (2.28%),
citronellol (16.18%), cis-R-terpineol (24.22%), trans-pinocamphone (5.86%), 6,11-oxidoacor-4-ene (18.06%), neo-iso-3-thujanol
(2.59%), and eugenol (4.37%) [9]. The extract showed antioxidant activity. The previous study investigated that the extract
was not hematotoxic and can be utilized for treating coronary heart ailments at the reported doses [10].
Chromolaena odorata is another perennial shrub that grows in Asia, Africa, and some parts of Europe [11]. Traditionally,
the extract had been utilized to treat colds, wound healing, coughs, and as antiseptic agent [12]. The extracted oils had been
reported to possess varied chemical compositions depending on the geographical locations. In India, pregeijerene, cubebol,
epi-cubebol, 10-epi-γ -eudesmol, cis-sabinene hydrate, germacrene-D-4-ol, germacrene D, δ -cadinene, geijerene, 10-epi-γ -
eudesmol, cyperene, khusimone, and α -muurolol were reported as the main chemical compositions of C. odorata leaf oil.
Only p-cymene and α -pinene were reported for the oil obtained from C. odorata grown in Congo and Cameroon [13].
In the extraction oil from plant sample, several techniques are employed which include conventional and modern meth-
ods. Microwave-assisted hydrodistillation extraction (MAHE) method was used in this study for extracting oils from H. sab-
dariffa flower, S. maydis and C. odorata leaf. This is due to cost effectiveness and ability to recover higher oil yield in shorter
extraction time in relation to the conventional techniques. In addition, MAHE is mostly employed in recent time to extract
oil due to its efficient start-up, spontaneous energy transfer and effective heating [14].
In view of the importance of essential oils from plants as the potential sources of fatty acids, this study investigated the
microwave-assisted hydrodistillation extraction of essential oils from H. sabdariffa flower, S. maydis and C. odorata leaf. Gas-
chromatography-mass spectrometry (GC–MS) and Fourier transform infrared (FTIR) analyses were employed to tentatively
identify the chemical compositions and functional characteristics of the extracted oils.

2. Procedure

2.1. Plant materials and preparations

The H. sabdariffa flowers used in this study were purchased in dry form from a local seller at Kuala Lumpur, Malaysia.
The H. sabdariffa flowers were further dried under shade for two weeks before pulverized. Moreover, fresh sweet corns were
purchased from Giant Hypermarket, Kuantan, Malaysia, the silks were carefully removed and dried under shade for two
weeks. The fresh leaves of C. odorata were obtained from the premises of Universiti Malaysia Pahang, Gambang, Malaysia.
The fresh leaves were rinsed in distilled water and dried under shade for a period of two weeks. All the three samples were
pulverized using a grinder and screened with a mesh of 0.105 mm particle size. The moisture contents of the samples were
approximately 10% prior to the extraction processes.

2.2. Extraction of oil

Essential oils from the three considered samples (H. sabdariffa flower, S. maydis and C. odorata leaf) were extracted using
an Ethos X microwave (Milestone, Italy). A 20 g of the powdered sample was extracted at a microwave power of 500 W
for 120 min using 200 mL of distilled water. Then, separating funnel was used to separate the essential oil by adding a few
drops of dichloromethane. The essential oil was dried over anhydrous sodium sulphate and stored at 4 °C until further use.
In addition, the oil yield was evaluated using Eq. (1).
V olume o f the extracted oil
Oil yield (% v/w ) = (1)
Mass o f plant sample
 O.R. Alara and N.H. Abdurahman / Chemical Data Collections 20 (2019) 100200 3

Fig. 1. Total ion current plot of H. sabdariffa flower oil from GC–MS analysis.

2.3. Gas chromatography-mass spectrometry (GC–MS) analysis

The GC–MS analysis was done using an Agilent 7890A gas chromatography (Agilent, CA, USA) coupled with a DB-1MS
column (30 m × 0.25 mm × 0.25 μm) that was at first hand joined to a 5975-mass spectrometer (Agilent) and autosampler.
The extracted oils were diluted using absolute ethanol and filtered through a 0.45 μm membrane filter to obtain a ratio of
1:20 v/v. The injection volume was 1 μL. By utilizing helium at a flow rate of 1.0 mL/min as a carrier gas, the operating
conditions were: the split injection ratio of 1:10, initial oven temperature stabilized at 60 °C for 4 min and ramped at
6 °C/min to 230 °C, detector temperature of 260 °C, injector temperature of 230 °C, 70 eV of ionization voltage, column flow
rate of 0.8 mL/min, and total run time of 48 min. The volatile chemical compounds in the oils were identified and estimated
by comparing the mass spectra with the NIST 05a library database.

2.4. Fourier transform infrared spectroscopy (FTIR) analysis

FTIR was performed with a Nicolet iS5 iD7 ATR (Thermo Scientific, Germany) apparatus coupled with OMNIC software.
The analysis range was selected between 40 0 0 and 50 0 cm−1 using a revolution of 4 cm−1 [15,16]. The generated IR spec-
troscopy was tentatively assigned based on the wavelength.

2.5. Analysis of data

The experimental trials were repeated thrice, and average values for oil yields were recorded as mean ± standard devia-
tion using Microsoft Excel 2013® .

3. Data, value and validation

3.1. Essential oil yields and tentative identification of the chemical compounds using GC–MS analysis

In recent time, there have been a lot of changes in the way of life. These have brought about changes in the quality of
food ingested and concerns about the safety of products being produced industrially on human health. This is because most
of the consumer products are being produced from synthetic chemicals which are being reported daily to pose side effects
on human health. However, efforts are being made to find an alternative by using natural-based raw-materials in place of
the synthetic ones. In this regard, essential oils are mostly utilized daily as food or folk medicine, causing higher demands
as compared to synthetic additives.
The extracted essential oils from H. sabdariffa flower, S. maydis and C. odorata leaf yielded 2.60 ± 0.2, 6.25 ± 0.15 and
2.10 ± 0.10% v/w, respectively. The GC–MS analysis was employed to tentatively identify the volatile chemical compounds
in the essential oils of H. sabdariffa flower, S. maydis and C. odorata leaf (Figs. 1–3). Supplementary materials (Tables S1-3)
summarize the volatile compounds identified in the essential oils. Generally, there are significant differences in the chem-
ical compositions of the three considered plant samples. It can be observed that 16, 13 and 13 chemical compounds were
4 O.R. Alara and N.H. Abdurahman / Chemical Data Collections 20 (2019) 100200

Fig. 2. Total ion current plot of S. maydis oil from GC–MS analysis.

Fig. 3. Total ion current plot of C. odorata leaf oil from GC–M– analysis.

identified in the oils from H. sabdariffa flower, S. maydis and C. odorata leaf, respectively. The main chemical composi-
tions of the H. sabdariffa flower oil were fatty acids (71.73%), Thiol (21.31%), sesquiterpene (2.27%), acyclic diterpene alcohol
(3.49%), and phenolic monoterpenoids (1.01%). Meanwhile, S. maydis oil comprised of fatty acids (55.10%), ketone (24.23%),
flavone (14.66%), acyclic diterpene alcohol (1.50%), and alkaloid (1.28%). The C. odorata leaf oil contained fatty acids (44.28%),
monoterpenes (24.11%), sesquiterpenes (19.45%), acyclic diterpene alcohol (11.02%), and alkene (1.04%). These indicated that
the extracted oils contained larger quantities of fatty acids. They are essential for the human survival because essential fatty
acids can lower blood pressure, minimise lipoprotein-cholesterol, avert platelet aggregation, possesses anti-inflammatory
property, cytoprotective activity, initiate telomerase, and ameliorate homocysteine adverse effect [17].
The major chemical compounds in H. sabdariffa flower essential oil are fatty acids that amount to 71.73%, the fatty acids
include 4-methoxy-2-thiophenecarboxylic acid (18.04%), cyclopentane carboxylic acid (16.86%), n-Hexadecanoic acid (10.19%),
9,12-Octadecadienoic acid (Z,Z)- (8.14%), Oleic acid (5.54%), dodecanoic acid (4.54%), 4-pentenoic acid ethyl ester (3.28%), 9-
Octadecenoic acid (Z)- (3.11%), and n-Nonanoic acid (2.03%). The analysis of oil from H. sabdariffa flower obtained from Cuba
reflected the presence of 81 chemical compositions whereby the amount of fatty acid was 12.4% [7]. However, the study
 O.R. Alara and N.H. Abdurahman / Chemical Data Collections 20 (2019) 100200 5

Fig. 4. FTIR analysis of H. sabdariffa flower oil.

carried out on H. sabdariffa flower from China showed the presence of 50.564% of fatty acids and 31.898% ester compounds
as the main chemical compounds [18]. The obtained results showed that H. sabdariffa flower from Malaysia is endowed and
rich in fatty acids.
Furthermore, the result from this finding had reflected that 55.10% of fatty acids were present in the extract of S. maydis
from Malaysia. Previous findings had reported that Egyptian S. maydis mainly comprised of citronellol and α -terpineol which
belongs to terpenoid class [9]. The occurrence of 4H-pyran-4-one (14.66%) and 4-hepten-3-one (24.23%) had been previously
reported as the main chemical compounds in five different species of maize genotypes [9]. In addition, the methanol extract
of S. maydis from Nigeria was investigated to contain a higher quantity of fatty acids [19].
The results obtained clearly showed that C. odorata leaf is an embodiment of fatty acids (44.28%), monoterpenes (24.11%),
sesquiterpenes (19.45%), acyclic diterpene alcohol (11.02%), and alkene (1.04%). However, previous investigation on C. odorata
leaf from Ivory Coast showed that the extract contained geigerene (11.68%), α -pinene (21.15%) and pregeigerene (19.61%);
from Thailand comprised of geigerene (3.1%), α -pinene (20.7%) and pregeigerene (17.6%); from Nigeria comprised of ger-
macrene D (9.7%), α -pinene (42.2%), (E)-caryophyllene (5.4%), β -copaen-4α -ol (9.4%), pregeijerene/geijerene (7.5%), and β -
pinene (10.6%). These previous results showed clear variations in the results of this study whereby α -muurolene (2.32%),
caryophyllene (5.39%), Bicyclo [7.2.0] undec-4-ene, 4,11,11-trimethyl-8-methylene-, [1R-(1R∗ ,4Z,9S∗ )]- (7.43%), germacrene D
(3.89%), β -pinene (23.35%), α -pinene (0.76%), and higher percentage of fatty acids were obtained. This variation might be
due to different geographical locations, climatic conditions, soil type, temperature, climate, collection time, and luminosity
where the plant samples had been acquired.

3.2. FTIR analysis

FTIR is commonly used for the tentative identification of functional groups. The functional characteristics in the oils of
H. sabdariffa flower, S. maydis and C. odorata leaf are presented in Figs. 4–6. Table S4 (Supplementary materials) extracted
from the previous study was used to categorize the obtained spectra in the oils into their respective functional groups [20].
The infrared spectra observed in the H. sabdariffa flower, S. maydis and C. odorata leaf oils fall within the range of 40 0 0–
500 cm−1 . In the spectra obtained for H. sabdariffa flower, the broad peak at 3328.31 cm−1 suggested the presence of O–H
stretching; the sharp peak at 2979.86 indicates the presence of lipid-carbohydrate; the peaks at 1785.74 and 1724.36 cm−1
refer to the presence of fatty acids (C=O) stretching of esters; peaks at 1696.45 and 1632.36 cm−1 might be due to the
occurrence of protein amide I; the bands that fall between 1399.88 and 1042.72 cm−1 might be due to the presence of CH2 ,
lipids, nucleic acids, and carbohydrate (C–O–C). Moreover, there were five major identified peaks in the oil of S. maydis which
are 3274.19 cm−1 (O–H functional group), 1653.54 and 1635.99 cm−1 (C=O stretching), 1081.29 and 1044.48 cm−1 suggested
the presence of C–O–C of polysaccharides and nucleic acid. In the oil obtained from C. odorata leaves, the observed peak
at 3343.61 cm−1 might be due to the presence of O–H stretching; a peaks at 1785.74 and 1724.36 cm−1 refer the presence
6 O.R. Alara and N.H. Abdurahman / Chemical Data Collections 20 (2019) 100200

Fig. 5. FTIR analysis of S. maydis oil.

Fig. 6. FTIR analysis of Chromolaena odorata leaf oil.

of fatty acids (C=O) stretching of esters; peak at 1642.11 cm−1 can be attributed to the presence of protein amide I; the
peaks observed between 1453.14 and 1043.58 cm−1 might be due the presence of N–H bending, C–N stretching, lipids,
nucleic acids, and carbohydrate (C–O–C). In general, the spectra obtained from the oils indicated the presence of hydroxyl
group showing the presence of phenolic compounds [15]; cellulose-fatty acids v(C=O) stretching of esters, affirming the
occurrence of fatty acids in the oils [21]; protein amide I band mainly v (C=O) stretching; protein δ s (CH2 ) and δ s (CH3 )
bending of methyl carboxylic acid vs(C–O) of COO- groups of carboxylates Lipid δ s (N(CH3 )3 ) bending of methyl; nucleic
 O.R. Alara and N.H. Abdurahman / Chemical Data Collections 20 (2019) 100200 7

acid (other phosphate-containing compounds) vas (>P=O) stretching of phosphodiesters; and carbohydrate v (C–O–C) of
polysaccharides [20]. These results complemented the presence of fatty acids in the oils as presented in the GC–MS results.

4. Conclusion

The potentials of oils from H. sabdariffa flower, S. maydis and C. odorata leaf as sources of fatty acids were examined
through GC–MS analysis. The functional groups in the extracted oils were analysed using FTIR. The results showed that the
oils possessed a total number of 16, 13 and 13 chemical compounds dominated with esters and fatty acids for H. sabdariffa
flower, S. maydis and C. odorata leaf, respectively. In addition, the obtained results from FTIR analysis showed the presence
of hydroxyl group, cellulose-fatty acids, methyl carboxylic acid, nucleic acid, and carbohydrate in the extracted oils. Thus,
the extracted oils from H. sabdariffa flower, S. maydis and C. odorata leaf can serve as the potential source of fatty acids. It
is therefore suggested that the biological activities of the oils be examined in future studies to ascertain the full potentials
of the oils from the three considered plants for food, nutraceutical and pharmaceutical purposes.

Conflict of interest

The authors declare none.

Acknowledgement

We thank Universiti Malaysia Pahang for the financial support through RDU180329.

Supplementary material

Supplementary material associated with this article can be found, in the online version, at doi:10.1016/j.cdc.2019.10 020 0.

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