Malaysian
Journal of Analytical Sciences Vol 22 No 6 (2018): 973 - 983
DOI:
10.17576/mjas-2018-2206-07
EXTRACTION OF
SQUALENE FROM Aquilaria malaccensis
LEAVES USING DIFFERENT EXTRACTION METHODS
(Pengekstrakan
Skualena daripada Daun Aquilaria malaccensis
Menggunakan Kaedah Pengekstrakan yang Berlainan)
Wan Nurul Diyana Ramli1,2, Mohd Azizi Che Yunus1,2*,
Lee Nian Yian1, Zuhaili Idham1, Ahmad Hazim Abdul Aziz1,2, Noor Aiysah Aris1,2,
Nicky Rahmana Putra1,2, Shahid Kamar Sham2
1Centre of Lipids Engineering & Applied Research (CLEAR),
Ibnu Sina Institute for Scientific and Industrial Research
2Faculty of Chemical
and Energy Engineering
Universiti Teknologi Malaysia, 81310 UTM Johor Bahru,
Johor, Malaysia
*Corresponding
author: azizi@cheme.utm.my
Received: 16
April 2017; Accepted: 18 November 2018
Abstract
Nowadays deep sea sharks species have been hunted for its liver oil as
the major source of squalene because of its importance in medical field
especially as an antioxidant and anticancer compound. Studies have proved the
existence of squalene compound in the Aquilaria
malaccensis leaves. Supercritical carbon dioxide (SC-CO2)
extraction was done to study the effect of SC-CO2 operating
parameters (pressure and temperature) on the oil yield as well as percentage
yield of squalene compound in the oil extracted from the leaves. Both the oil
yield and the squalene percentage obtained by using SC-CO2
extraction method were compared with conventional Soxhlet extraction technique.
For SC-CO2 extraction, the temperature used were 45 °C, 60 °C and 75 °C while the operating pressures were 100 bar, 200 bar
and 300 bar. Each extraction process was carried out for 60 minutes with carbon
dioxide flow rate of 8 g/min. Meanwhile for Soxhlet extraction, six types of
solvents were used (methanol, ethanol, ethyl acetate, n-hexane, acetone and
water). Soxhlet extraction gave higher oil yield (45.66%) by using ethanol as
solvent compared to SC-CO2 (13.22%) at 300 bar and 60 °C. However, Soxhlet gave lower squalene percentage in
the oil extract (0.78%) by using n-hexane as solvent when compare with SC-CO2
(3.97%) at 200 bar and 60 °C. These findings
reveal that SC-CO2 extraction is a preferable technique used to
extract oil with high percentage of squalene compared to conventional Soxhlet
extraction technique with shorter extraction time and higher selectivity on
squalene.
Keywords: Aquilaria
malaccensis, supercritical carbon dioxide, squalene, gas chromatography
analysis
Abstrak
Pada masa
kini spesies jerung laut dalam diburu kerana minyak hatinya sebagai sumber
utama skualena disebabkan kepentingannya dalam bidang perubatan terutama sekali
sebagai sebatian antioksida dan antikanser. Kajian telah membuktikan kewujudan
sebatian skualena di dalam daun Aquilaria
malaccensis. Pengekstrakan karbon dioksida lampau genting (SC-CO2)
telah dijalankan untuk mengkaji kesan parameter operasi SC-CO2
(tekanan dan suhu) terhadap hasil minyak bersama peratusan hasil sebatian
skualena di dalam minyak yang diekstrak daripada daun tersebut. Kedua-dua hasil
minyak dan peratusan skualena yang didapati menggunakan kaedah pengekstrakan
SC-CO2 telah dibandingkan dengan kaedah pengekstrakan Soxhlet
konvensional. Untuk pengekstrakan SC-CO2, suhu yang digunakan adalah
45 °C, 60 °C dan 75 °C manakala tekanan operasi pula adalah 100 bar, 200 bar
dan 300 bar. Setiap proses pengekstrakan telah dijalankan selama 60 minit
dengan kadar aliran karbon dioksida sebanyak 8 g/min. Manakala bagi
pengekstrakan Soxhlet, enam jenis pelarut telah digunakan (metanol, etanol,
etil asetat, n-heksana, aseton dan air suling). Pengekstrakan Soxhlet
memberikan hasil minyak yang lebih tinggi (45.66%) dengan menggunakan etanol
sebagai pelarut berbanding pengekstrakan SC-CO2 (13.22%) pada 300
bar dan 60 °C. Walau bagaimanapun, Soxhlet dengan menggunakan n-heksana sebagai
pelarut memberikan peratusan skualena yang lebih rendah di dalam ekstrak minyak
(0.78%) apabila dibandingkan dengan SC-CO2 (3.97%) pada 200 bar dan
60 °C. Hasil penemuan ini mendedahkan bahawa pengekstrakan SC-CO2
adalah kaedah yang lebih baik untuk mengekstrak minyak dengan peratusan
skualena yang tinggi dengan masa pengekstrakan yang lebih singkat dan pemilihan
yang lebih tinggi terhadap squalene berbanding kaedah pengekstrakan Soxhlet
konvensional.
Kata kunci: Aquilaria
malaccensis, karbon dioksida super genting, skualena, analisis
kromatografi gas
References
1.
Robert,
A. B., Jurgens J. A. and Heuveling van Beek H. (2015). Growing aquilaria and
production of agarwood in hill agro-ecosystems. Akansha Publishing House,
Delhi: pp. 66-82.
2.
Angela,
B., Anak, N. A., Mulliken, T. and Song, M. (2000). Heart of the matter:
Agarwood use and trade and CITES implementation for Aquilaria malaccensis. Unpublished note. Cambridge, TRAFFIC.
3.
Popa,
O., Babeanu, N. E., Popa,I., Nita, S. and Dinu-Pârvu, C. E. (2015). Methods for
obtaining and determination of squalene from natural sources. BioMed Research International, 2015:
1-16.
4.
Simandi,
B., Kery, A., Lemberkovics, E., Oszagyan, M., Ronyai, E., Mathe, I., Fekete, J.
and Hethelyi, E. (1996). Supercritical fluid extraction of medicinal plants. High Pressure Chemical Engineering, 12:
357-362.
5.
Tapsell,
L. C., Hemphill, I., Cobiac, L., Patch, C. S., Sullivan, D. R., Fenech, M.,
Roodenrys, S., Keogh, J. B., Clifton, P. M., Williams, P. G., Fazio, V. A. and
Inge, K. E. (2006). Health benefits of herbs and spices: The past, the present,
the future. The Medical Journal of
Australia, 185(4): 4-24.
6.
Norzafneza,
M. A., Saripa, S. S. A. A., Hasimah, A., Ramli, I., Mohd, A. H. M. S., Mat, R.
M. and Abdul, H. A. H. (2010). Chemical constituents of leaves from Aquilaria Crassna Pierre (Karas) and
their biological activities. Proceedings
of the Seminar on Medicinal and Aromatic Plants: pp. 111-120.
7.
Khalil,
A. S., Rahim, A. A., Taha, K. K. and Abdallah, K. B. (2013). Characterization
of methanolic extracts of agarwood leaves. Journal
of Applied and Industrial Sciences, 1(3): 78-88.
8.
Selva,
M. and Perosa, A. (2008). Green chemistry metrics: A comparative evaluation of
dimethyl carbonate, methyl iodide, dimethyl sulfate and methanol as methylating
agents. Green Chemistry, 10(4):
457-464.
9.
Villén,
J., Blanch, G. P., Ruiz del Castillo, M. L. and Herraiz, M. (1998). Rapid and
simultaneous analysis of free sterols, tocopherols, and squalene in edible oils
by coupled reversed-phase liquid chromatography-gas chromatography. Journal of Agricultural and Food Chemistry,
46(4): 1419-1422.
10.
Özkal,
S., Salgın, U. and Yener, M. (2005). Supercritical carbon dioxide extraction of
hazelnut oil. Journal of Food
Engineering, 69(2): 217-223.
11.
Yunus,
M. A. C., Zhari, S., Haron, S., Arsad, N. H., Idham, Z. and Ruslan, M. S. H.
(2015). Extraction and identification of vitamin E from Pithecellobium jiringan seeds using supercritical carbon dioxide. Jurnal Teknologi, 74(7): 29-33.
12.
Xiao,
J. B., Chen, J. W. and Xu, M. (2007). Supercritical fluid CO2 extraction of essential oil from Marchantia convoluta: Global yields and
extract chemical composition. Electronic
Journal of Biotechnology, 10(1): 141-148.
13.
Peterson,
A., Machmudah, S., Roy, B. C., Goto, M., Sasaki, M. and Hirose, T. (2006).
Extraction of essential oil from geranium (Pelargonium
graveolens) with supercritical carbon dioxide. Journal of Chemical Technology and Biotechnology, 81(2): 167-172.
14.
Ibrahim,
A., Al-Rawi, S., Majid, A. A., Rahman, N. A., Abo-Salah, K. and Ab Kadir, M.
(2011). Separation and fractionation of Aquilaria
malaccensis oil using supercritical fluid extraction and the cytotoxic
properties of the extracted oil. Procedia
Food Science, 1: 1953-1959.
15.
Rezaei,
K. and Temelli, F. (2000). Using supercritical fluid chromatography to
determine diffusion coefficients of lipids in supercritical CO2. The Journal of Supercritical Fluids,
17(1): 35-44.
16.
Mohd
Azizi, C. Y. (2007). Extraction, identification and separation of vitamin E and
djenkolic acid from Pithecellobium
jiringan (jack) prain seeds using supercritical carbon dioxide. PhD Thesis.
Universiti Sains Malaysia.
17.
Long,
C. X. (2014). Extraction of squalene from palm oil mesocarp using supercritical
carbon dioxide. Thesis of Master Degree. Universiti Teknologi Malaysia.
18.
Blanks,
R. F. and Prausnitz, J. (1964). Thermodynamics of polymer solubility in polar
and nonpolar systems. Industrial and
Engineering Chemistry Fundamentals, 3(1): 1-8.
19.
Ikushima,
Y., Saito, N., Arai, M. and Arai, K. (1991). Solvent polarity parameters of
supercritical carbon dioxide as measured by infrared spectroscopy. Bulletin of the Chemical Society of Japan,
64(7): 2224-2229.
20.
Vieillescazes,
C., Sierra, I. and Morante-Zarcero, S. (2012). Separation techniques. In
conservation science for the cultural heritage Springer: pp. 15-35.
21.
Mohd,
A. C. Y., Nur, H. A., Salman, Z., Zuhaili, I., Siti, H. S. and Ana, N. M.
(2012). Effect of Supercritical carbon dioxide condition on oil yield and
solubility of Pithecellobium jiringan
(Jack) prain seeds. Jurnal Teknologi,
60: 45-50.
22.
Yunus,
M. A. C., Idham, Z. and Morad, N. A. (2015). Optimisation of squalene from palm
oil mesocarp using supercritical carbon dioxide. 10th Asian Control Conference: pp.1-6.