minyak kelapa dara

UNIVERSITI
SAINS
MALAYSIA - Ruj . Kami 2008/074 (U0060)
: 9 September 2011
Tarikh
Prof. Ir. Mohd. Omar Ab. Kadir
Pusat Pengajian Teknologi Industri
Universiti Sains Malaysia
11800 USM
PULAU PINANG
Pejabat Pengurusan Dan Kreativiti Penvelidil<an
I Research Creativity and Management Office
Canse lori,
Unive rsiti Sains Malaysia
Ara s 6, Bangunan Canselori
11800, USM Pu lau Pinang
T : (6)04-65331 08/3178/3988/5019
F : (6)04-6566466/8470
: (6)04-653 2350
L : www.resea rch.usm.my
Tuan,
LAPORAN AKHIR GERAN PENYELIDIKAN UNIVERSITI PENYELIDIKAN (RU )
TAJUK PROJEK : ENHANCING OIL YIELD AND OPTIMIZATION OF OIL MEDIUM CHA IN
TRIGL YCERIDES (MCTS) CONTENT IN SUPERCRITICAL CARBON DIOXIDE
EXTRACTION OF COCONUT OIL FROM FRESH COCONUT (Cocos nucifera L.)
NO. AKAUN
1001 1 PTEKIND 181401 3
Dengan hormatnya perkara di atas dirujuk.
2.
Terlebih dahulu saya ucapkan terima kasih atas penghantaran laporan akhir Geran RU seperti
tajuk di atas. Bersama-sama ini dilampirkan komen penilaian daripada Dekan Penyelidikan Pelantar
Kejuruteraan & Teknologi untuk perhatian tuan.
3.
Memandangkan projek ini telah selesai, Pejabat ini akan menutup projek ini dan seterusnya pihak
Jabatan Bendahari diminta untuk memproses penutupan akaun projek ini selepas semua urusan tuntutan
dan bayaran dalam tempoh projek dijalankan diselesaikan.
4.
Selanjutnya , tuan diminta untuk mengambil tindakan seperti dinyatakan di bawah :
a)
b)
c)
d)
Merakamkan penghargaan kepada Universiti Sains Malaysia. Sila pastikan nama Universiti
ditulis/ditaip dengan penuh/lengkap iaitu 'Un iversiti Sains Malays ia'.
Tiga salinan penerbitan berkaitan mesti dikirimkan ke Bahagian Penyelidikan dan Inovasi
untuk tindakan selanjutnya.
USM mempunyai opsyen pertama untuk menerbitkan bahan yang dihasilkan melalui projek
ini. Ini akan dilakukan melalui Penerbit USM dan keputusan untuk menerbitkan bahan ini
akan dibuat dalam tempoh en am bul an.
Bahagian ini akan mengagihkan semula peralatan yang telah dibeli menggunakan peruntukan
geran ini sea ndainya terdapat penyelidik lain yang memerlukan peral atan tersebut.
5.
Bahagian ini mengucapkan tahniah di atas kejayaan tuan selaku Ketua Penyelidik menyelesaikan
projek dengan jayanya. Tuan akan dihubungi oleh Pejabat Inovasi untuk perkembangan selanjutnya
has ii/outcome daripada geran ini sekiranya terdapat harta intelek/pengkom ersialan hasil geran yang boleh
diketengahkan.
Sekian , terima kasih .
"BERKHIDMAT UNTUK NEGARA"
'Memastikan Kelestari an Hari Esok'
(H AZL ~N
AB DU L HA
)
Ketua Penolong Pendaftar
Pejabat Pengurusan & Kreativiti Penyelidikan
Bahagian Penyelidikan & Invovasi
- -bAPORAN AKHIR-GERAN PENYELIDIKAN tJNIVERSITI PENYELIDIKAN (RU)
TAJUK PROJEK : ENHANCING OIL YIELD AND OPTIMIZATION OF OIL MEDIUM CHAIN
TRIGL YCERIDES (MCTS) CONTENT IN SUPERCRITICAL CARBON DIOXIDE
EXTRACTION OF COCONUT OIL FROM FRESH COCONUT (COCONUT
NUCIFERA L.)
NO. AKAUN
1001 / PTEKIND 1814013
s.k.
Dekan Penyelidikan
Pelantar Kejuruteraan & Teknologi
Pejabat Pelantar Penyelidikan
USM Kampus Kejuruteraan
Dekan
Pusat Pengajian Teknologi Industri
Universiti Sa ins Malaysia
Pengarah
Pejabat Inovasi
Universiti Sains Malaysia
Timbalan Dekan
(Pengajian Siswazah & Penyelidikan)
Pusat Pengajian Teknologi Industri
Universiti Sa in s Malaysia
Ketua Pustakawan
Hamzah Sendut
~ Universiti Sains Malaysia
r)"'::;;~Perpustakaan
Ketua Penolong Sendahari
Seksyen Kewangan Penyelidikan
Jabatan Sendahari
Universiti Sains Malaysia
Pegawai Sains
Pelantar Kejuruteraan & Teknologi
Pejabat Pelantar Penyelidikan
USM Kampus Kejuruteraan
HAH/aihat
Laporan Akhir - MohdOmarAbKadir (U0060)
}
Disampaikan satu salinan
laporan akhir projek untuk
simpanan Perpustakaan
}
Sila ambil tindakan menutup
akaun projek dan kemukakan
satu salinan penyata
kewangan terakhir ke
Sahag ian ini
=
UNIVERSITY RESEARCH G
FINAL REPORT
0)Geran Penyelidikan Univ
Laporan Akhir
UNIVERSITI SAINS MALAYSIA
A.
PARTICULARS OF RESEARCH I MAKLUMAT PENYELJDIKAN:
(i)
Title of Research:
Tajuk Penyelidikan: Enhancing Oil Yield & Optimization of Oil Medium Chain Triglycerides ( MCTs)
Contents in Supercritical Carbon Dioxide Extraction of Coconut Oil from Fresh Coconut (Cocos nucifera L)
(ii)
Account Number:
Nombor Akaun: 10011PTEKINDI814013
B.
PERSONAL PARTICULARS OF RESEARCHER / MAKLUMA T PENYELIDIK:
(i)
Name of Research Leader:
Nama Ketua Penyelidik:Prof Mohd Omar Ab Kadir
Name of Co-Researcher
Nama Penyelidik Bersama:
Prof. Dr Nik Norulaini Nik Ab. Rahman
En. Wahyu B. Setianto
En. Abu Hanipah Nawi
(ii)
Schoolllnstitute/Centre/Unit
Pusat Pengajian IlnstitutlPusatlUnit : Pusat Pengajian Teknologi Industri
C.
Research Platform (Please tick (/) the appropriate box):
Pelantar Penyelidikan (Sila tanda (I) kotak berkenaan):
D
D
A.
D
C.
D
D
D
D
D. SQcial Transformation
Life Sciences
Sains Hayat
B. Fundamental
Fundamental
Engineering & Technology
Kejuruteraan & Teknologi
Transformasi Sosial
E.
Information & Communications Technology (ICT)
Teknologi Maklumat & Komunikasi
F.
Clinical Sciences
Sains Klinikal
G.
Biomedical & Health Sciences
Bioperubatan Sains Kesihatan
© Divi sion of Research & Innovation - Unjversi'ti Sains Malaysia - Mal'eh 201 0
D.
Duration of this research:
Tempoh m?Isa penyelidikan ini :
*DUration: =-:-:-3 tanun .....
Tempol? :
Oktober 2007
E.
=.....
September 2010
From
To
Dari:
Ke:
ABSTRACT OF RESEARCH
(An abstract of between 100 and 200 words must be prepared in Bahasa Malaysia and in English.
This abstract will be included in the Annual Report of the Research and Innovation Section at a later date
as a means of presenting the project findings of the researcherls to the University and the community at
large)
Abstrak Penyelidikan
(Perlu dised iakan di ant ara 100 - 200 perkat aan di da lam Bahasa Malaysia dan juga Bahasa
lnggeris .
Abstrak ini akan dimuatkan dalam Laporan Tahunan Sahagian Penyelidikan & Inovasi sebagai satu
cara untuk menyampaikan dapatan projek tuan/puan kepada pihak Universiti & masyarakat luar).
Minyak kelapa yang disari dari isi kelapa segar dikenali sebagai minyak kelapa dara
(l\I.lKD). Minyak kelapa dara adalah sumber semulajadi trigliserida rantai sederhana (IRS) yang
mana telah dikenali sebagai minyak sihat. Sehingga ke hari ini, penyelidikan berkaitan penyarian
l\IlI<D menggunakan karbon dioksida lampau genting (C0 2 - LG) dari segi dasar pengekstrakkan
masih lagi kurang. Objektif kajian ini adalah untuk menentukan kesan faktor-faktor pengekstrakan
l\IlI<D menggunakan (C02- LG), dan mengkaji keterlarutan minyak tersebut dalam (C02- LG) .
Penilaian
kesan-kesan
interaksi
bagi
parameter
pengekstrakan
telah
dilakukan
menggunakan Kaedah Iindakbalas Permukaan (RSlVI). Kajian ini telah dijalankan berdasarkan
reka bentuk Box-Behnken. Iekanan (20.7 - 34.5 MPa), suhu (313 - 353 K) dan jumlah
penggunaan karbon dioksida (10 - 60 g) telah dipilih sebagai parameter. Respon yang terlibat
adalah hasil pengekstrakan dan kandungan IRS dalam minyak yang diekstrak. Hasil
pengekstrakan dikira melalui kaedah gravimetrik dan analisis kandungan IRS dilakukan
menggunakan analisis gas kromatografi (GC). Satu hubungkait telah dibangunkan dengan p value untuk kedua-dua respon pada 95% aras keyakinan. Pengukuran keterlarutan dijalankan
menggunakan kaedah dinamik pada julat tekanan dari 20.7 hingga 34.5 :NlPa dan suhu dari 313
© Di vision of Research & Innovation - Uni versiti Sains Malaysia - March 2010
hingga 353 K. Analisis keterlarutan minyak dilakukan secara gravimetrik dan analisis lengkung.
Keterlarutan minyak meningkat dengan suhu pada tekanan di antara 31.0 dan 34.5 IvIPa dan
berkurang dengan suhu pada tekanan di antara 20 .7 dan 24.1 MPa.
Data keterlarutan yang
diperolehi daripada eksperimen dikolerasikan menggunakan model Chrastil dan del valle-
Aguilera iaitu berdasarkan ketumpatan karbon dioksida (C02). Keterlarutan kawasan-lintasan
boleh diperhatikan dalam julat tekanan 27.5 hingga 30.5 Mpa dan pada sekitar 29 MPa, yang
menunjukkan keterlarutan MKD dalam CO2- LG tidak dipengaruhi oleh suhu secara praktikalnya.
Kesahihan data keterlarutan telah dilakukan melalui perbandingan dengan data keterlarutan
trigliserida tulen dalam CO 2- LG yang pernah dilaporkan dan ujian ketekalan-diri dilakukan
dengan kaedah lvJendez-Santiago dan Teja.
***
Coconut (Cocos nucifera) oil which is extracted from fresh coconut flesh is known as
virgin coconut oil (YCO). The oil is a natural source of medium chain tryglycerides (MCTs)
which has been well known as healthy oil. It is remarkable that very few reports on the extraction
of the YCO using SC-C02 have been published hitherto the fundamental insights on the SC-C02
extraction processes of the coconut oil are much lacking. The objectives of this work are
evaluating the parameters etTects of YCO extraction using SC-C02 and examination of the oil
solubility in SC-C02.
The assessment of interaction effects of extraction parameters was performed using a
Response surface methodology (RSM). The study was carried out according to Box-Behnken
design. Pressure (20.7 - 34.5 MPa), temperature (313 - 353 K) and CO2 consumption (10 - 60 g)
were chosen as the parameters. _T he responses were the extraction yield and the MGT s content of
extracted oil.
The yield was calculated by gravimetric and the MCTs content analysis "vas
performed using GC analysis. A correlation was established with p -value for both responses at
I
95% confident level. The Solubility meaS1..1rement was performed by dynamic method at the
© Di vision of Research & Innovation - Uni versiti Sains Malays ia - M;u'ch 20 I 0
pressures and temperatures range of 20.7 to 34.5 NIPa and 313 to 353 K respectively. Oil
solubility analysis was performed using gravimetric and curve analysis. The' oil solubility
Increases with temperature at pressures between 31.0 and 34.5 MPa and decreases with
temperature at pressures between 20.7 and 24.1 MPa. The solubility experimental data obtained
was correlated with Chrastil and del Valle-Aguilera model, which are based on the C02 density. A
solubility cross-over region was observed in the pressure range of27.5 to 30.5 MPa and at around
29 MPa, the solubility ofVCO in SC-C02 is practically independent of temperature. The validity
of the solubility data was performed by its comparison with previous reported data of pure
triglyceride solubility in SC-C0 2 and performing a self-consistency test with the method of
Mendez-Santiago and Teja.
F.
SUMMARY OF RESEA RCH FINDINGS
Ringkasan dapatan Projek Penyefidikan
The extraction of coconut oil was performed using SC-C02 at various pressures,
temperatures and CO 2 consumption levels. This process can successfully be performed, and
extracting about 99% ofthe total oil. The extraction yield and the MCTs content of the extracted
oil varied with the extraction conditions. A mathematical model based on statistical analysis was
established. The correlation between the extraction conditions and the extraction yield as well as
the MCTs content applied in this study may be remarkable and should be considered for scalingup the VCO extraction process.
Solubility of virgin coconut oil (VCO) in supercritical carbon dioxide was examined with a
dynamic method. The solubility data could be well-correlated with a density based model. The oilCO2 system exhibited a cross-over region that could be described by the density based model. The
solubility data validation confirms its reliability. The comparison of the solubility of pure
triglycerides in SC-C02 with the measured VCO solubilities shows that the latest value are
intermediate to lighter and heavier triglycerides solubility in SC-C02 that was reported in the
literatures. The data examination using the self-consistency test proposed by Mendez-Santiago
and Teja resulted that the data was consistent.
(9 .oi vi sion of R ~searcb & Innovation - U ni versiti Sains Mala ys ia - March 20 to
1- - - -1
G.
COMPREHENSIVE TECHNICAL REPORT
Laporan TeknikaJ Lengk8(J
Applicants are required to prepare a comj:lrehensive technical report explainingJhe project.
(This report must be attached separately)
Siia secjiakan laporan teknika! lengkap yan~l rnenerangkan keseluf'u!wfl projek inL
[laporan ini mesH dikepilkanj
Please see attachment.
List the key words that reflectour research:
Senarai/(an kata kunci yang mencerminkan penyelicfikan andcl.
English
Bahasa Malaysia
Virgin coconut oil
Minyak kelapa muda
Medium chain triglycerides
Rantai trigliserida sederhana
Supercritical CO2
Takat genting CO 2
© Division of RcS"IU'C iJ & innovation - Un iversiti Sa ins Malaysia - March 20 10
-
H
a)
Results/Benefits of this research
Hasil Penyelidikan
-
No.
Bil:
Category/Number:
Kqtegoril Bilangan:
Research Publications
(Specify target journals)
Penerbitan Penyelidikan
(Nyatakan sasaran jurnal)
Human Capital Development
a. Ph. D Students
b. Masters Students
c. Undergraduates (Final Year
Project)
d . Research Officers
e. Research Assisstants
f. Other: Please specify
1.
2.
Achieved
-
3
,
1
1
2
2
Patents
Paten
3.
•
---
Promised
-
4.
Specific / Potential Applications
SpesifiklPotensi aplikasin
5.
Networking & Linkages
Jaringan & Jalinan
6.
Possible External Research Grants
to be Acquired
Jangkaan Geran Penyelidikan Luar
Diperoleh
Developing of new
extractor system using a
new view ce ll and
repa iring of the old others
system part (High
pressure pump and
ch iller) . The system also
suitable for clinica l waste
sterilizati on.
Japan counterpart (Toyo
Koatsu) and loca l
cou nterpart (Sime Darby)
Sime Darby gro up (RM
3.9 Million) - (potentia l)
Kindly provide copies/evidence for Category 1 to 6 .
b) Equipment used for this research.
Perala tan yang telah digunakan dalam penye/idikan ini.
Items
Perkara
Specialized
Equipment
Peralatan
khusus
Approved Equipment
Approved Requested Equipment
Location
Lab 131, Tingkat 1,
Bangunan G07, Pusat
Pengajian Tek. Ind. , USM
Penang.
Extractor with view window
Gas flow meter
High pressure valve
modification
Facility
Kemudahan
-
Infrastructure
Infrastruktur
~
Please attach append ix if necessa ry .
:\) Division of Research & [nl1ovatiol1 - Uni versiti Sains Malaysia - March 20 10
.
-
I.
BUDGET f BAJET
Total Approved Budget
Additionai Budget- - - -
: RM 257,450 .00
:RM -
Grand Total of Approved Budget
: RM 257, 450.00
--I--~I --rotal
Yearly Budget Distributed
Year 1
:RM122,100.00
Year 2
Year 3
: RM 91,350.00
: RM 44,000.00
Additional Budget Approved
Year 1
: RM
Year 2
Year 3
: RM
: RM
Total Expenditure
: RM 259,912.77
Balance
: RM -3 ,107.21 (deficit)
•
Please attach final account statement from Treasury
5-4-2011
Signature of Researcher
Penyelidik
~~-~:randatan§an
Date
Tarikh
Professor Ir. Moh. Omar Ab. Kadlr, Ph I)
$chooloftndustriaJTechn~y
Universiti Sains Malaysia
11800 Penanq
(9 Div.is.ion
ofR~search &
lnnovation - Uni versiti Sains Ma laysia - March 2010
H.
COMM ENTS OF PTJ'S RESEARCH COMMITTEE
KOMEN JAWATANKUASA PENYELIDIKAN PERINGKAT PTJ
General Comments :
Ulasan Umum:
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?'l\13r " a t F~' ~'a
Tim b[1 1an lJekan
Pe n gaj ian S is wa'lah & : (, ~yelid.ika~
P u sat Pe n gaj ian Tekn"lcg 1 In,ci ustIl
Prc fes"T
Universiti Sains Ma l aYSia
11800 Pulau Pinang
Signatu
d Sta
Chairperson of PTJ's Evaluation Committee
Tandatangan dan Cop Pengerusi Jawatankuasa Penilaian PTJ
t.~. . /t..(?C!..f (
Date : .....
Tarikh :.. .... ... ..................... ... .... .. ......... ..
Signature and Stamp of Dean! Director of PTJ
;;;;:taT:;!y7(Deka~/~engarah PTJ
P
rcSOR
ROZM/~N
HJ. DIN
DEKAN
PUSAT PENGAJI AN TEKNOLOG I INDUSTRI
11 800, USM. PENANG
(9 Division ofRl!search & Innovation - ti ll iversiti Sains Ma lays ia - M;u'ch 20 10
G. COMPREHENSIVE TECHNICAL REPORT
Laporan TekniJ<al LengJ<.ap
Effects of Extraction ParametersonYield and Medium-Chain Triglycerides
(MCTs) Content
Qualitative analysis of the sample was performed using GC-MS. The sequence of the
peak for all fatty acids which existed in the extracted oil was confirmed by performing
GC-MS analysis. Peak scan analysis using MS was performed to indentify the peah. The
analysis showed that fatty acid elution depended on the fatty acids molecular weight.
Lighter fatty acids (lower molecular weights) were eluted first, followed by the heavier
fatty acids .
Spectrophotometric analysis gave the following identification: time (minutes)
1.02; 147; 2. 31 ; 4.38; 7.69; 1147; 15 .61 ; 1599; 16.85 are n-Hexane (solvent for
analysis); caprylic acid methyl ester; capric acid methyl ester; lauric acid methyl ester;
myristic acid methyl ester; palmitic acid methyl ester; linoleic acid methyl ester; oleic
acid methyl ester; stearic acid methyl ester respectively.
As discussed previously, fatty acids that were obtained in the extracted oil were
caprylic (C8 :0), capric (CI0 :0), lauric (C1 2:0), myristic (C14:0), palmitic (C16:0),
linoleic (C18 :2), oleic acid (C18: 1) and stearic acid (CI8 :0). The target compounds of the
extraction were the MCTs. MCTs content ofthe extracted oil were defined as the
medium fatty acid (C 8 :0 - C 12 :0 ) present in the oil.
To determine the effects of interactions between the parameters (pressure,
temperature and CO2 consumption) to the extraction yield and the MCTs content of the
extracted oil, the response surface methodology (RSM), a statistical analysis was applied
(Palma and Taylor, 1999, Myers and lVIontgomery, 2002) . The experimental data were
obtained, according to the response surface methodology RSM experiment design as
given in Table 1.1.
The design of experiment (DOE) was performed according to Box-Behnken
design. Throughout the RSM analysis the unit of temperature was expressed in degree
celcius CC).
Table 1.1 : Experimental Program and Results of The Box-Behnken Design of Extraction
Yield and Extracted Oil MCTs Content in The Extraction Using SC-C02 .
(Weight %)
MCTs
content
(weight %)
35
94. 56
5947
40
35
96.25
57.99
80
35
40 .29
67 27
Pressure
Temperature
(MPa)
(0C)
CO2
consumption
(g)
( Xl)
( x2 )
(X3 )
1
20.7
40
2
34.5
20.7
Standard
order
..,
j
© Di vision of Research & [llnovatioll - Uni vers iti Sains Malays ia - March 20 10
Yield
4
34.5
80
35
99.4-1
59.07
5
20.7
60
10
30.2 1
65.49
34.5
60
10
93.37
62.00
7
20.7
60
60
92.37
60.39
8
34.5
60
60
99.08
56.71
9
27.6
40
10
73.69
62.40
10
27.6
80
10
63 .30
64.27
11
27.6
40
60
95.64
58.94
12
27.6
80
60
99.32
58 .07
13
27.6
60
35
98.28
59.12
14
27.6
60
35
97.30
59.49
15
27.6
60
35
97.08
56.76
16
27.6
60
35
97.64
56.35
17
27.6
60
35
96.55
56.35
6
A second-order polynomial model was applied to express the responses as a
function of the chosen variables.
y, represents the dependent variables (extracted yield and the IvICTs content),
Xs
represents the independent variables (pressure, temperature and CO2 consumption) and
bs represents the coefficients. Multiple regression analysis was performed to determine
the regression coefficients of the model (Table 1.2).
Table 1.2 : Estimated Coefficients of Second-Order Response Models for SC-C02
Extraction ofVCO.
intercept
~_
Extraction yield
Extracted oil MCTs content
(%)
(%)
-77.2497
88.4694
9.9870
-1.6310
Di vision of R esearch &. [nnovation - Ulliversiti SaiJ]s \lIaJa ysia - NJaJ'ch 20 J0
-~--..........-~-.
~'fmi<:
_
x1
-1.9022
-0.0206
x_
3.4872
-0 .2067
XI XI
-0 .1993
0.0374
.1: 2 .1: 2
-0.0131
0.0039
X3X3
-0.0146
0.0028
X1X2
0.1040
-0.0122
X1X3
-0 .0818
-0.0003
X2X3
0.0070
-0.0014
J
The effects of pressure, temperature and CO2 consumption on extraction yield and
MCTs content can be seen in the sample graph (Figure 1.6). In Figure 1.6a, it was
observed that at pressures lower than 28.3 "NIPa, the extraction yield decreased with
increase in temperature, while at higher pressures (greater than 28.3 l\1Pa), the yield
increased with temperature. This was most likely due to the solubility cross-over
phenomenon, which often occurs in solute-C02 systems. The phenomenon is discussed in
the section of solubility examination.
Figure 1.6b shows a contour plot of the interaction of the pressure and the CO 2
consumption. It is clear that the increase in CO2 consumption resulted in an increase in
the yield. At a constant temperature (60 QC) and certain CO2 consumption level,
increasing pressure provided higher extraction yields (Fig. 1.6a. The MCTs content
increased with increasing temperature, while it decreased with increasing pressure (Fig.
1.6c). The increase in CO2 consumption reduced the MCTs content of the extracted oil
(Fig. 1.6d) . The trend of the MCTs content was contrary to that of the yield. This might
be due to the shorter chain triglycerides that were extracted more easily than the longer
chain triglycerides; consequently, the oil extracted earlier in the process has a higher
MCTs content than the fractions extracted later.
(9 Division of R.:search & Inn ovat ion - Universiti Sains Malaysia - M:u'ch 20 10
'""
Yield (%)
80.-~~--~~,-~--,---~
Yie ld
(%)~~
~~- 60,---~--------~====--~
70
48
0
~
.!:!!
~
"'0
(J)
:J
+'
~
CfJ
60
:J
(1)
35
N
0
0.
E
(1)
0
I-
50
23
40
10
21
24
28
31
21
35
24
Pressure (MPa)
31
35
(b)
(a)
80
28
Pressure (MPa)
MCTs content (%)
60
70
MCTs content (%)
48
0
~
2.?
~
:J
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::l
0.
0 '"
(1)
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E
35
0
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I-
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23
40~----,L----.-----,-L-~
21
24
28
31
35
21
24
28
Pressure (MPa)
Pressure (MPa)
(c)
(d)
31
35
Figure L 6 :~ftects of parameters on yield and NIGT-s content of extracted oil. (a) Effects
of pressure and temperature on extraction yield using 35 g CO2 . (b) Effects of pressure
and CO 2 consumption on extraction yield at 60°C. ( c) Effects of pressure and
temperature on extracted oil MCTs content using 35 g CO 2 . (d) Effects of pressure and
CO2 consumption on oil MCTs content at 60
0c.
© Division of R ~searcb & InlJova tion - U lli versili Sains Malaysia - Mru'e h 2010
The analysis of variance (ANOVA) for the extraction yield and the extracted oil
MCTs content is shown in Table 4.3. The calculated values of F were compared to the
tal51e vruue of 0. p- l. n-p .a) . The ANOVA shows that the calculated value of F for the
yield response (20.52) and that of the MCTs content response (6.44) were greater than the
table (experimental) value of F (09,7,005) = 3.68). If the calculated value of F exceeds
the table value of F , the null hypothesis is rejected at the level of significance, and it is
inferred that the coefficient estimates are not all zero (that is, one or more coefficients
convey information about the model) and the variation verified that the model is
significantly greater than the unexplained variation (noise) (Wonnacott and Wonnacot,
1990). Therefore, the p -value for the yield and the MCTs content responses is below
0.05 . Accordingly, it could be constmed that, at the 95% contldence level, the models
were significant for both of the responses. The value of R2 measures the total variation of
the observed values about the mean determined by the fitted model. The values of R2 for
the yield and the MCTs content responses were 0.96 and 0.90, respectively; hence, the R2
value in this study signifies a good correlation between the experimental data and the
predicted values. Therefore, the fitted model obtained can be used to describe the effects
of the factors within the experimental ranges.
Table 1.3 : Analysis of Variance (ANOVA) for Extraction Yield and Extracted Oil MCTs
Content.
Extraction Yield
Source
Degrees of freedom
Regression
Residual
Total
7
9
16
Extracted Oil .MCTs Content
Source
Degrees of freedom
Regression
9
Residual
7
Total
16
Sum of squares Mean Square
7140.38
270.59
7410.98
793.38
38.66
Sum of squares Mean Square
151.84
18.33
170.17
© Di vision of R esearch & Innovation - Univcrsiti Sains Malavsia - Mm'ch 2010
16.87
2. 62
0.0.05)
20. 52 0.96
3.68
R2
0.0.05)
0.90
3.68
F
6.44
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KETUA PRO.EK : PROFESOR MOHO OMAR AS KADIR
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Doi<lJmen
In(
a<iarall cetakan komputer c1an tfada tanc1atangan c1iperJukan
No._
Authors, Year, Title of paper, Name of journal or proceeding, Volume, Page
Number
1.
SETIANTO, W. B" NAWI, A. H. & MOHD. OMAR, A. 1<. (2008) Applicati on of Chrastil
Model to The Virgin Coconut and Palm Kernel Oil Solub ility in Supercritica l Carbon
Dioxide. International conference on environmental research and technology. {pp.
921-925}, P. Pinang, Malaysia.
2.
Setianto, W.B" Nik Norulaini, N.A., Abu Hanipah, N" Mohd Zu lhilmi, M . & Mohd
Omar, A. 1<' (2008). Solubi lity examination of virgin coconut oi l in supercritica l carbon
dioxide and its corre lation with existing model. In Proceedings of the 2 nd
In ternational conference on science and technology (pp. 2187-2193), P. Pinang,
Malaysia.
3.
NIK NORULAINI, N. A., SETIANTO, W. B" ZAIDUL, I. S. M. , NAWI, A. H" AZIZI, C. Y. M .
& OMAR, A. 1<. M. (2009) Effects of supercritica l carbon dioxide extractio n
parameters on virgin coconut oil yield and medium -cha in triglyceride content. Food
Chemistry, 116, 193-19. (impact facto r : 2.698)
International Conj'erence on Environmental Research and Technology (ICERT 2008)
Application of Chrastil Model to The Virgin Cocoout and Palm Kernel Oil Solubility in
Supercritical Carbon Dioxide
WahyuB. Setianto*, Abu H. Nawi, Mohd. Omar Ab. Kadir
School of Industrial Technology, Universiti Sains Malaysia, 11800 Minden, Penang, Malaysia
*Corresponding author. Phone: +604 653 2110, Fax: +604 6585435
___~ __ .__ ·___ ~!pil-it~\[email protected]<2.~~m
ABSTRACT
Supercritical carbon dioxide (SC-CO z) extraction has been introduced as a clean technology for extraction process
since it is exclusive of chemical utilization. Application of the SC-COz to vegetable oil extraction became an
attractive technique due to its high solublbty, short extraciton hme, sImple punfiCafiOflanaa osence' of chemical
residue in the oil. The application of SC-C0 2 to virgin coconut oil (VCO) and palm kernel oil (PKO) extraction has
been performed. The equilibrium solubility ofVCO and PKO in supercritical carbon dioxide have been measured by
means of extraction curve' analysis. The measurements were performed in the temperature range from 323 .1 5 K to
353. 15 K and pressures 20. 7 to 34.5 :MPa for VCO and 27.5 to 48.3 "NfPa for PKO. The solubility experimental data
were correlated with Chrastil model, a density solvent base model. The experimental data were well fitted to the
model by average absolute Jlercent deviation 2.20 and 3.84 for VCO and PKO respectively.
Keywords·:-Ghrastil-modeI-,-palIn-kerneLo.il,...solubilit¥,_sup.ercritical _carbon dioxide, virgin coconut oiL
---------1. INTR,Op'UCTlo~-~·· ...· ~--. _
Supercritical .carbon dioxide (SC-C02) extraction is an attractive technology due to its relatively low critical
temperature (31.1 0c) and critical pressure (7.38 :MPa) (McHugh and Krukonis, 1994). In the supercritical state,
liquid-like density is approached, while viscosity is near that of normal gases, and diffusivity is about two order of
magnitude higher than in typical liquid (Brunner, 1994). It makes the fluid become an excellent solvent. As the
solvent is non-polar, the application for triglyceride extraction gives a pramising result. Using SC-CO z sa lvent
allaws extractian pracesses to aperate near ambient temperature. Furthermare, SC-COz is nan-taxic, can be used in
food-grade fann for faad pracessing, and is cansidered to be an environmentally friendly solvent. It shauld be noted
that we are using CO 2 rather than dispasing it. Separation af extracts fram SC-CO z is relatively simple, since the
salute extract can be separated fram the SC-COz solvent by reducing the pressure af the flawing mixture thraugh an
expansian valve.
In this study, the SC-C02 extraction technalogy was applied far the extract ian afvirgin cacanut oil (VCO). and
palm kernel ail (PKO). In the extractian pracess, a single step extraction can be applied, in which the ails can be
extracted directly fram the matrices without further purificatian ar separatian. A report af using af SC-CO z
extraction on caconut ail has been published (Celestino et aI., 2006). The author suggested an ail cantent analysis of
capra using SC-COz. It is reported that within less than ane our, 100% of caconut ail, as referred to. saxhlet
extraction, cauld be extracted from the tissue using the pracess. However, further studies an the extractian, such as
the ail solub ility and mass transfer analysis have not been reported yet. The applicatian af SC-COz an PKO
extraction has been reported in several publicatians (Hassan et aI. , 2000, Nik Namlaini et aI., 2004, Zaidul et ai. ,
2007).The pracess has been described as a clean technalagy due to. the absent af chemical far sa lvent and refining
far the pracess ..
Several vegetab le (such as sunflawer, com, uCJ,mba and babassu) ail salubility in SC-COz have been carrelated
..Eith the madel (Soares et aL, 2007).J{awever, analysis afthe VCO and PKO solubility inSC-C0 2 using the sa lvent
density base madel has nat been reported yet. The abjectives afthe study were to. examine the twa ail so lubility in
SC-C0 2 and to. apply the Chrastil made I (Chrastil, 1982) an the so lubility.
2.
lVlATERlALS AND METHODS
2.1 Material
The sa lubility af cacanut ail in supercritical CO 2 was measured in this wark, whereas the palm kernel oil
so lubility data was acquired from previaus repart perfarmed by the same research group (Hassan et aI. , 2000).
C leaner cech, concro t, treatment & remediacion cechnique
92 1
SOLUBILITY EXAMINATION OF VIRGIN COCONUT OIL IN
SUPER CRITICAL CARBON DIOXIDE AND ITS CORRELATION
WITH EXISTING MODEL
Wahyu Bahari Setianto U, Nik Norulaini Nik Ab.Rahmanb, Abu Hanipah Nawi a,
Mohd Zulhilmi Mokhtal'U, Mohd Omar Ab. Kadir u
"School at' Industrial Technology, Universiti Sains Malaysia, 11800 Minden, Pulau Pi nang, Malaysia
"School of Distant Education, Universiti Sains Malaysia, 11 800 Minden, Pulau Pinang. Malaysia
Emai l: [email protected]
ABSTRACT. Coconut (Cocos nucijera L.) oil is a source of natural medium chain triglycerides (MCTs) with
approximately 60% of Ihe oil cOn/en/ is ,."JCTs. The MCTs have been reported to have benefiCial eifeci on health
Extraction of the oil has been performed using supercrilical carbon dioxide (SC-CO~. The extraclion technology has
been introduced as a clean lechnology since it is exclusive of chemical utilization. Applicalion of Ihe SC-CO, to
vegelable 011 extraction became an allraClive technique due 10 ils high soll/bilily. shOl'l extraction lime. simple
purification and absence of chemical residue in the oil. In the present work. solubility of virgin coconut oil (VCO) in
SC-CO, was examined. The Solubility examination was performed with dynamic method using a SC-CO, labora/ory
scale extractor and phase behaVIOr examination using a view high-pressure vessel. The measZlremen/s were
pe/formed al temperatures Fom 313.15 10 353./5 K and pressures Fom 20.7 10 34.5 MPa. The solZlbilily
experimental data obtained/i'om dynamIC me/hod examination was correlaled with Chrastil and del Valle-AgUIlera
model which are based on the CO} denSity. while the data Fom phase behavior examination was correlated with
Peng-Robmson equation of state (£OS). The experlmen/al data was well fitted /0 the models by average ab~olllle
percent devialion (AAPD) 0.95 ond 4.02for Ihe Chras/i/ and del Valle-Aguilera model respectively and 2.62/01' Ihe
Peng-Robinson EOS.
1. Introduction
Coconut (Cocos nucifera L.) oil that is extracted from fresh coconut flesh is known as virgin coconut oil
(YCO). The extraction involves a process without employing thermal treatment or food preservatives. Coconut
oil obtained from copra, dried coconut has no taste or fragrance due to the refining process, whereas YCO has a
fragrance and taste of coconut. The absence of heating and chemical usage in the oil makes it tasty and healthy.
The antioxidant activity of YCO is superior to that of regular coconut oil, which is extracted from copra and of
groundnut oil [ I]. Separation of the oil from the water oi l emulsion also can be accomplished by breaking the
emulsion and creating an oil-oil emulsion [2], in which pure coconut oil is needed to be added to the coconut
milk to extract the oil from the emulsion, and then the oil has to be separated from the water and protein with
decantation. The existing mentioned process requires 24 to 48h and gives an oil yield of about 40% oil
available in the coconut.
The oil is a natural so urce of medium chain tryglycerides (MCTs) in terms of fatty acids constituents with
approximately 60% of the total oil content which are regarded as C6 to C12 fatty acids constituents. The MCTs
constituents have been reported to have beneficial for the human health. The MCTs constituents are mainly
utilized as a nutritional supplement for patient suffering from mal absorption caused by intestinal resection and
also as a component of infant feeding tormulation [3] . It is also reported that MCTs constituents have beneficial
effect on weight control and g lucose as well as lipid metabolism [4].
The technology of supercritical carbon dioxide (SC-C0 2) was proposed to enhance the existing production
process of virgin coconut o.il. Supercriti cal fluids are substances at pressure and temperature above their critical
value. [n the supel'cl'itical region of a fluid, the phase state resembles one of the dense gases with properties that
are generally intermediate to those of a gas and liquid. In tbe supercritical state liquid like density--.is
approaclLed, while viscosity is near that of normal gases, and diffusivity is about two order of magnitude higher
than in typical liquid [5]. A specific feature of the supercritical state of a fluid is its dense and highly
compressible nature. This means that properties can be changed greatly with small changes in temperature or
pressure. The tremendous variation in characteristics due to various conditions is causing differences in effects
on solutes within the state conditions [6). The techno logy of SC-C0 2 is an attractive technology applied in
many research activities around the globe due to its relatively low critical temperature (31.1 0c) and critical
pressure (7.38 MPa) [7]. Using SC-C0 2 solvent allows extraction processes to operate near ambient temperature.
2 187
Food Chemistry 116 (2009 ) 193-197
_Co ntents~ lists
.:
\
availab le at ScienGeDireGt
Food Chemist ry
----. ~
.
j ourna I h·o m e·p.age.: www.els.evi.er ..co·m / I.ocat.e/fooctche,m
Effects of supercritical carbon dioxide extraction parameters on virgin coconut
oil yield and medium-chain triglyceride content
N.A. Nik Norulaini a .• , W.B. Setianto b, I.S.M. Zaidul c, A.H. Nawi b, C.Y.M. Azizi d, A.K. Mohd Omar b
'Scl1ool oj' Discance Education. Universiti Sains Malaysia. 11800 Minden. 1'. I'inang. Malaysia
b Scl100l oj' Indusnial Technology. UniversiLi Sains Maiaysicl. 11800 Minden. P. Pinang. Malaysia
'DeparoJ1 ent oJ Food Science. Faadey oj' Fo od Science anci Tecl1nology. Universiti Put/'a Malaysia. 43400 UPM. Serdang. Selangor DE. Malaysia
dCl1emical Engineering DeparoJ1ent. Universiti Teknologi Malaysia. 813 10 Skudai.jollOr. Malaysia
ARTICLE
[NfO
Artide history:
Received 9 Decem ber 2008
Received in revised form 7 Jan uary 2009
Accepted 12 February 2009
Keywords:
Virgin coconut oil
Medi um chain lriglyceri des
Supercritica l CO,
Extraction
Response s urface methodology
ABSTRACT
The extraction of coconut oil has been perfo rmed us ing supercritical carbo n dioxide (5C-C0 2 ). The ext ractio ns were performed at pressure and temperature r<l nges of 20.7-34.5 MPa and 40-80 0( . respect ive ly. It
was observed that almost all (mo re tha n 99%) of the total oil could be extracted. Response surface methodo logy (RSM ) was applied to eva lua te the effects of the parameters (pressure. temperature and CO 2 consumpt ion) on the extracti on yie ld and med iu m-cha in trig lyce ri des (MCTs ), in terms of the fa tty acid
content in the ex tracted oil. A corre latio n was established with p-va lues fOT both responses sign ificant
at the 95%co nfide nce level.
© 2009 Elsevier Ltd. All rights reserved.
1. Introduction
Coco nut (Cocos n ll cilera L ) oil is a na tura l source of med iu mcha in t rig lyce rid es (MCTs ) with a pprox imate ly 60% of the total
oi l co nte nt be in g MCfs. The term MCT refers to t riglyceride wh ich
is com posed of a glycero l backbone a nd three satu rated fatty acid s
with cha in length of 6-12 carbons. MCTs have been repotted to be
be neficia l to hum a n hea lt h. MCTs a re m a inl y utili se d as a nut ritional s upplement for patients suffering from ma labsorp tion
caused by in testi na l resect ion a nd a lso as a com po ne n t of infa nt
feedi ng for m ulas (Nandi, Gangop adh yay , & Ghos h. 2005). rVlarten.
Pfeuffer. and Schrezenmei r (2006) reported t hat MCTs have beneficial effects o n weight co n trol and g lucose, as we ll as li pid metabo lis m. Compa red wit h other triglycer ides that ma in ly co nta in
sa tu rate d long cha in fatty acids . MCTs have a lower me ltin g poin t.
s ma ll er mo lecular size, lower sol id ificat ion temperature and lower
e nergy density. These ciistillct chemical properties affect the way s
in which MCTs are abso rbed and metabo li zed. MCfs have a lso bee n
reported as tumoUl' inh ibitors wbe n consumed in a_diet (Cohe n &
Thomson, [987). and. if t hey a re mi xed wit h p hytos te ro l and
high-o leic canola oil. t hey can deCl~ease plasma lipid co ntent in
overweig ht men (Ru dkow ska, Roynelle, Naki1as i, & Jones . 2(06).
Coco nu t oil that is ex tracted from fres h cocon u t fle s h is
known as virgin cocon u t oil (VCO). The extraction invol ves a
• Corresponding author. Tel./ fa x: +6046585435.
F.- mail address: nor1.!i.1in@u~~m.my (N.A. Nik NOfulain i).
0308~81461$ ~ see fro nt matter '9 2009 Elsevier Ltd . /\ 11 righ ts reserved.
doi : 10.1 01 6/j.lclOdch e m. 2009.02.030
process t hat d oes not use the rma l t rea tment or food p rese r vatives. Coconut o il obta ined from copra, dried cocon u t, has no
taste o r fragra nce, due t o the refin ing process. w hereas vco
has the fragra nce a nd taste of coco nu t. The a bse nce of hea lin g
and c hem ical treatm ent in the oil makes it tasty a nd hea lt hy.
The a nti ox id ant activ ity o f VCO is s up eri o r to t ha t of regul ar
coco n ut oil, which is ext racted fro m copra, an d a lso of groundnut oi l (Nevin & Rajamoilan. 2005). The existin g p rocess productio n of VCO bas ically is con ducted thro ugh o il se pa rat io n from
coco nu t m il k (S u kartin & Sitan gga ng, 2005). Coco nu t m ilk can
be obta ine d by e ithe r press ing fres h coco nu t fles h w it ho u t additional water or grat ing the coconut flesh followed by extracting
the water-o il e mul s io n with wate r. The oil can be se parated
fro m the e m ulsi on by means of bo ili ng, fe rm enta tio n. re fr ige ration or m ec han ica l cent rifuge. Separation of the oil from the
water-o il em ul sio n can a lso be acco mpl ished by break ing th e
emulsion and creating an oi l-o il em ul sion . in which pure coconut o il must be adde d to the coco n ut m ilk to extract th e oil
from the emulsion . and the n the oil m usc--be sepaTated from
the wa ter a nd protei n w ith deca n tatio n. The exis ti ng process requ ires 24-48 h and produces an oil yie ld of about 40% of t he oil
ava il ab le in the coco n ut.
Althoug h extractio n of nat ural compounds us ing SC- C0 2 has
been reported as a promising techn ique by ma ny researche rs it is
re marka ble that very few repo rts on the extraction of coco nu t oil
fro m co p ra using SC-C0 2 have bee n publ is hed. Ad d iti o na ll y . tllere
is a lack of fu ndamenta l ins igh ts in to the SC-C0 2 extractio n process