Industrial Crops & Products 129 (2019) 488–494

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Industrial Crops & Products

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Refining process for production of refined palm-pressed fibre oil T

A.W. Nur Sulihatimarsyila , Harrison L.N. Lau, K.M. Nabilah, I. Nur Azreena
⁎

Energy and Environment Unit, Engineering and Processing Research Division, Malaysian Palm Oil Board, 6, Persiaran Institusi, Bandar Baru Bangi, 43000, Kajang,
Selangor, Malaysia

ARTICLE INFO ABSTRACT

Keywords: Palm-pressed fibre oil (PPFO) is rich in natural phytonutrients such as carotenes and tocotrienols (vitamin E),
Red fibre oil which makes it worth further development to enhance its quality. Crude PPFO is currently extracted using
Degumming solvents without further refining. This study aimed to refine crude PPFO using a combination of processes
Bleaching including degumming, bleaching, and deacidification. Various doses of hot distilled water at 0.5, 1.0, 2.0, 3.0,
Phytonutrient
4.0, 5.0, and 6.0 v/v% were applied during water degumming to remove soluble and hydratable gummy ma-
Phosphorus content
terials in crude PPFO. Degumming with acids at doses ranging from 0.1 to 1.0 wt% were tested to obtain oil with
low phosphorus content. Bleaching earth doses ranging from 0.1 to 1.0 wt% were used to absorb trace metals
and other impurities. The bleached PPFO was subjected to deacidification to remove free fatty acid (FFA). The
optimum refining conditions were using 5.0 v/v% of hot distilled water at 90 °C for 20 min for water degum-
ming, 1.0 wt% of phosphoric acid at 90 °C for 10 min for acid degumming, 0.1 wt% of natural bleaching earth at
105 °C for 15 min during bleaching, and deacidification at 110 °C at 0.1 mtorr. The refined PPFO (RPPFO)
showed a 98% reduction of phosphorus content (from 565 ppm to 13 ± 2 ppm) and FFA removal of 97% (from
5.94% to 0.15%), while deterioration of bleachability index (DOBI) increased by 44% (from 1.99 to
2.87 ± 0.17). In addition, RPPFO was rich in carotenoids (1208 ± 23 ppm) and vitamin E (904 ± 8 ppm) that
can be developed into high value products. The RPPFO meets the quality specifications of refined, bleached, and
deodorised palm oil (RBDPO) while maintaining the heat-sensitive phytonutrients.

1. Introduction supplement that contains carotenes, tocopherols and tocotrienols (vi-

Malaysia is the world’s second largest palm oil producer after
Indonesia (Kushairi et al., 2018). The oil palm industry in Malaysia
processed about 103.94 million tonnes of fresh fruit bunches (FFB) into
19.92 million tonnes of crude palm oil (CPO) in 2017 (Kushairi et al.,
2018). At the same time, 14.55 million tonnes of palm-pressed meso-
carp fibre (PPMF) were generated. PPMF is a by-product produced from
the extraction of oil palm FFB in palm oil mills which contains 5% to
7% residual oil (on a dry weight basis) or 0.3% to 0.5% in terms of oil
extraction rate. Conventionally, PPMF is burnt as a fuel to produce
steam and electricity for mill operations. Techniques to recover palm-
pressed fibre oil (PPFO) include solvent extraction, supercritical carbon
dioxide extraction, and water screw-pressed technology, etc. (Choo
et al., 1996; Lau et al., 2006; Luiz and Angela, 2008; Goh, 2014 and
Vijaya et al., 2013). The commercial extraction method of PPFO from
PPMF is solvent extraction using hexane. Based on the FFB processed in
2017, an estimated 728,000 tonnes of PPFO can be recovered from 454
palm oil mills per year.
PPFO has been known as a potential source for dietary health
tamin E), squalene, and phytosterol (Choo et al., 1996, 2003, 2004; Lau
et al., 2008, 2007a; Chandrasekaram et al., 2009 and Rusnani et al.,
2012; Phoon et al., 2018). The reported deterioration of bleachability
index (DOBI) of the unrefined PPFO ranges from 1.3 to 2.0 while the
free fatty acid (FFA) ranges from 5.0% to 7.0% (Lau et al., 2017).
Nevertheless, PPFO is rich in natural phytonutrients such as carotenes
(1,200-2,500 ppm) and tocotrienols (1,200-2,000 ppm). In fact, almost
all previous studies suggested that PPFO has a wide range of applica-
tions in nutraceutical, supplementation, and cosmetics. In addition,
PPFO was also found to contain high amounts of water-soluble com-
pounds, i.e., phenolics with excellent antioxidant activities (Lau et al.,
2007b; and Valeria et al., 2017). Apart from the normal acylglycerides
content, PPFO also contains 31.5% lauric oil due to broken kernels in
the mesocarp fibre (Neoh et al., 2011 and Lau et al., 2006), thus making
it a suitable ingredient in food applications. With proper refining, PPFO
has the potential to generate additional income for the palm oil in-
dustry. Currently, PPFO is sold to animal feed suppliers as a supple-
mentary ingredient for feed formulation.
No specific studies on the refining process of crude PPFO have been

⁎
Corresponding author.
E-mail address: nursulihati@mpob.gov.my (A.W. Nur Sulihatimarsyila).

https://doi.org/10.1016/j.indcrop.2018.12.034
Received 27 July 2018; Received in revised form 14 November 2018; Accepted 10 December 2018
Available online 15 December 2018
0926-6690/ © 2018 Elsevier B.V. All rights reserved.
A.W. Nur Sulihatimarsyila et al.
reported. Traditionally, CPO is refined into refined, bleached, and
deodorised palm oil (RBDPO) for downstream applications.
Conventional refining destroys the natural carotenoids in CPO due to
the high processing temperature of 260 °C during the deacidification
and deodorisation steps (Bonnie and Choo, 1999). The process is car-
ried out at high temperature ranging from 150 °C to 260 °C and under
high pressure. This tends to degrade the natural carotenoids by thermal
oxidation during the deodorisation step. In order to preserve the car-
otenoids (≈ 70%) in palm oil, the FFA and volatile oxidation products
such as peroxides can be removed through short path distillation which
uses high vacuum and low temperature in the refining process.
Goncalves et al. (2016) reported on the deacidification process of palm
oil through solvent extraction which could produce refined palm oil
with high carotenoid content. However, chemical deacidification using
a polar solvent is not preferable for use in food industries due to safety
issues. Lau et al. (2006) studied simultaneous extraction, degumming,
and deacidification of PPFO using supercritical carbon dioxide. The
degummed and deacidified PPFO fulfilled the specifications of the
RBDPO with preserved and value-added phytonutrients in the refined
PPFO (RPPFO).
In the conventional CPO refining process, phospholipids are re-
moved through degumming and bleaching steps. Phospholipids or gums
are considered as undesirable substances because they could cause pi-
peline and equipment fouling at high temperature processing.
Therefore, an additional pre-treatment process for the removal of
phospholipids in crude PPFO is required due to the high phosphorus
content (> 500 ppm) in the oil. There are two types of phospholipids,
namely hydratable and non-hydratable phospholipids in palm oil. The
hydratable phospholipids can cause formation of gum deposits during
oil storage. In order to overcome the circumstances, water degumming
has been adopted to remove the hydratable phospholipids through
precipitation by water hydration. Whereas for non-hydratable phos-
pholipids, a normal acid degumming step is introduced in the process
(Kanamoto et al., 1981). Lamas et al. (2016) studied water degumming
that obtained drastic reduction of high phosphorus content in de-
gummed sunflower oil. The phosphorus content achieved was lower
than 10 ppm and improves physicochemical parameters of the de-
gummed oil. Zufarov et al. (2008) studied a maximum phospholipid
retention reduction to 10 ppm in pressed rapeseed and sunflower oils by
combining water and acid-based approaches which indicate better de-
gumming efficiency. Hydratable phospholipids can be removed from
crude algal oil by water degumming which reported only a 19.4% re-
duction of the phospholipids. Therefore, acid-degumming was required
for non-hydratable phospholipids in algae that led to an 83% reduction
(Paisan et al., 2017). More and Gogate (2018a,b,More and Gogate,
2018c studied intensification of degumming of vegetable oil using ul-
trasound in combination with sulphate based oxidising agent which
resulted in a 94% phospholipid reduction. More and Gogate
(2018a,b,More and Gogate, 2018c also studied the removal of the total
phospholipid content of crude soybean oil using hydrodynamic cavi-
tation reactor in intensified degumming. The results showed that ca-
vitation-based degumming in intensified soybean oil presented sig-
nificant reduction in phospholipids in less processing time. As an
alternative to conventional degumming approaches, enzymatic de-
gumming processes have also been reported (Lamas et al., 2016; Qu
et al., 2016; Lamas et al., 2014). More and Gogate (2018a,b; More and
Gogate, 2018c investigated enzymatic degumming of crude soybean oil
by ultrasound and reported that 93% phospholipid separation was
achieved. Elina et al. (2017) investigated phospholipid removal by
enzymatic treatment and reported a decreased amount of phospholipids
in addition to less oil retention which improved oil yield.
The new refining method of treating crude PPFO will then make it
easier to overcome the limitation in handling oil with high amounts of
phospholipids. In addition, to preserve the nutrient content in crude
PPFO such as carotenes and vitamin E during the process, low tem-
perature deacidification was used in the study. The high quality RPPFO
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Industrial Crops & Products 129 (2019) 488–494
with desired nutritional content will be discussed in this paper.
2. Materials and methods
2.1. Materials
Solvent-extracted crude PPFO samples were collected from two
palm oil mills located in Perak and Johor, Malaysia. The crude PPFO
was freshly collected from solvent extraction plants before being
transferred to storage tanks. The crude PPFO samples were collected in
January during the dry season to avoid high FFA in the oil. During the
rainy season, the crude PPFO quality deterioration results from wet
conditions which cause hydrolysis and oxidation that could be asso-
ciated to higher FFA value. The oil was kept in a chiller at 6 °C prior to
the refining process. The crude PPFO sample collected from Perak was
used to investigate the effect of water dosage on phosphorus content in
water degumming, effect of acid dosage on phosphorus content in acid
degumming, and effect of bleaching earth dosage on phytonutrient
content in bleaching. Meanwhile, the crude PPFO sample from Johor
was used to study the properties of RPPFO under optimum conditions
for the refining process.
Sodium hydroxide (NaOH), phosphoric acid, and citric acid (ana-
lytical grade) were purchased from Merck KGaA, Darmstadt, Germany.
Natural bleaching earth (NBE) and activated bleaching earth (ABE)
were purchased from Taiko Bleaching Earth Sdn. Bhd., Parit Buntar,
Perak, Malaysia.
2.2. Refining process
Crude PPFO was refined using a combination of processes including
two-step water degumming, acid degumming, bleaching, and deacidi-
fication. One litre of crude PPFO was heated to 90 °C in a three-neck
round bottom flask while agitated using a magnetic stirrer (2.5 in.
length) under a nitrogen blanket. A two-step water degumming process
was applied to remove any soluble and hydratable gum in the crude
PPFO by adding 5 ml of hot distilled water at 90 °C for 20 min (coded as
WD1). The water layer was then separated from the oil phase by cen-
trifugation at 3000 rpm for 15 min. The second step of water degum-
ming was conducted by adding 5 ml of hot distilled water into WD1 at
90 °C for 20 min (coded as WD2) followed by separation by cen-
trifugation. Varying amounts of hot distilled water that ranged from 0.5
to 6.0 v/v% was used to investigate the effect of water degumming on
phosphorus removal in crude PPFO. For acid degumming, 1 ml of acid
was added into the water-degummed PPFO at 90 °C for 10 min. The
acids used were citric and phosphorus acid at a concentration of 20%
with doses that ranged from 0.1 to 1.0 wt%. The acid-degummed PPFO
was then neutralised by a NaOH solution followed by washing with
warm water prior to drying. In bleaching, 10 g each of NBE and ABE
was added separately into the acid-degummed PPFO at 105 °C and
maintained for 15 min under a nitrogen blanket. The NBE and ABE that
were added ranged from 0.1 to 1.0 wt%. The oil and bleaching earth
mixture was then filtered under a vacuum in a Buchner funnel with
Whatman filter paper no.1. The bleached PPFO was subjected to dea-
cidification to remove FFA and residual oxidation products at 110 °C
and 0.1 mtorr via a short path distillation system. The resulting water-
and acid-degummed PPFO, bleached PPFO, and RPPFO were char-
acterised for their phosphorus content, DOBI, FFA, carotene and vi-
tamin E content, and metal content. All the experiments were carried
out in 5 replicates. Use of hot distilled water and bleaching earth do-
sages will depend on the properties of crude PPFO collected from palm
oil mills. This study can be applied as a guideline to refine oil with high
phosphorus content.
2.3. Analysis of oil
The water- and acid-degummed PPFO, bleached PPFO, and RPPFO
A.W. Nur Sulihatimarsyila et al.
Table 1
Properties of crude palm-pressed fibre oil (PPFO).
Properties Crude PPFO from A
Phosphorus content (ppm) 815 ± 23
Free fatty acid, FFA (%) 6.07 ± 0.13
Carotene content (ppm) 1249 ± 17
DOBI 1.38 ± 0.04
Vitamin E (ppm) 1205 ± 11
Note: A = Palm oil mill is located in Perak, northern region of
Peninsular Malaysia.
The crude PPFO was collected from a solvent extraction plant in Perak,
Malaysia.
Results are mean values ± standard deviation (n = 3) of oil samples.
samples were analysed for phosphorus content using MPOB Test
Method p2.8 Part 1(b): 2004 (MPOB, 2005). FFA was analysed using
MPOB Test Method p2.5: 2004 (MPOB, 2005) while DOBI was analysed
using MPOB Test Method p2.9: 2004 (MPOB, 2005). Carotenoid con-
tent was analysed using UV–vis Spectrometer (U-2001, Hitachi
Instruments Inc., Tokyo Japan) at a maximum absorbance of 446 nm
(MPOB Test Method p2.6: 2004 (MPOB, 2005). Vitamin E content was
analysed by high-performance liquid chromatography (HPLC) with
fluorescence detector (Agilent Technologies, Palo Alto, CA) using C18
column (150 mm x 4.6 mm i.d.) and mobile phase of acetonitrile/me-
thanol (50:50, v/v) at a flow rate of 1.0 ml per min. Iron and copper
concentrations were analysed according to AOAC 984.27 and AOAC
999.11 Test Method, respectively. All analyses were carried out in tri-
plicates and average results were reported.
3. Results and discussion
3.1. Effect of water dosage on phosphorus content
The hydratable gums or phospholipids in crude PPFO need to be
removed to improve the oil quality. The phospholipids are ester of
glycerol, fatty acid, and other alcohols that differ from triglycerides in
Fig. 1. Effect of water dosage on phosphorus reduction during two-step water degumming (WD1, WD2).
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Industrial Crops & Products 129 (2019) 488–494
being surface-active and mostly used in food products as emulsifiers.
Phospholipids are present ranging from 20 to 80 ppm in CPO. Removal
of phospholipids is one of the toughest steps in the refining process.
Hydratable gums are formed when phospholipids bind with water,
causing hydration of some of the phosphatides which then become non-
oil-soluble. Therefore, hydrating the gums and removing the hydrated
gums from the oil via hot water degumming is necessary before pro-
cessing the oil to prevent formation of gum deposits. Table 1 shows the
properties of the solvent-extracted crude PPFO from a solvent extrac-
tion plant located in Perak, which were analysed for phosphorus con-
tent, FFA, carotene content, DOBI value, and palm vitamin E content.
The DOBI of the crude PPFO was 1.38. Due to its low DOBI value, the
crude PPFO is classified as sludge oil. The low DOBI is due to the co-
extraction of phospholipids or gum found in the bilipid membrane layer
of the plant cells. Phospholipids absorb UV light at 269 nm, which is the
wavelength used in DOBI calculation. In this study, two steps of water
degumming were performed to efficiently reduce the phosphorus con-
tent. It was found that phosphorus content in crude PPFO was reduced
with increasing water dosage (Fig. 1). The phosphorus content dropped
from the initial 815 ppm to 95 ppm with 5.0 v/v% of hot distilled water
used in the first water degumming step. From the first water degum-
ming step where the temperature and time was set at 90 °C and 10 min
respectively, water dosage was increased from 0.5 to 1.0 v/v% which
gave a significant increment of phospholipids removal. However, it was
slightly reduce when more than 2 v/v% of water was used. The addition
of 0.5–6.0 v/v% hot distilled water to the water-degummed PPFO
(WD1) in the second step of water degumming prior to acid degumming
helped to further reduce the phosphorus content in the PPFO by 30% to
50%. The degumming efficiency in WD1 was 10% to 40% as compared
to 32% to 45% in WD2. The amount of water had a significant effect on
water degumming. During water degumming, the water is dispersed in
the oil to provide an oil/water interface that enables the hydratable
phospholipids were hydrated gums to be moved into the water phase
via centrifuge. Therefore, water significantly improves the reduction of
phospholipids in oil. The hydratable gums in oil are coagulated by
water allowing them to become more easily absorbed by NBE (Howes
et al., 1991). These results are similar to those reported by previous
studies that use the same approach (Manjula et al., 2011; Lamas et al.,
A.W. Nur Sulihatimarsyila et al. Industrial Crops & Products 129 (2019) 488–494

Table 2
Characteristics of water-degummed PPFO in first step of water degumming (WD1).
Sample Water dosage DOBI FFA Carotene content Vitamin E
(v/v, %) (%) (ppm) (ppm)

Water-degummed PPFO 0.5 1.79 ± 0.01 6.28 ± 0.05 1216 ± 24 1093 ± 15

1.0 1.80 ± 0.01 6.39 ± 0.05 1213 ± 31 999 ± 17
2.0 1.81 ± 0.01 6.40 ± 0.10 1248 ± 15 949 ± 27
3.0 1.83 ± 0.25 6.50 ± 0.01 1117 ± 19 936 ± 16
4.0 1.90 ± 0.25 6.51 ± 0.01 1190 ± 23 893 ± 32
5.0 1.94 ± 0.29 6.68 ± 0.05 1184 ± 13 847 ± 29
6.0 1.94 ± 0.08 6.93 ± 0.03 1189 ± 25 885 ± 23

Note: Crude palm-pressed fibre oil (PPFO) : Deterioration of bleachability index (DOBI) = 1.38; free fatty acid (FFA) = 6.07%; Carotene content = 1249 ppm;
Vitamin E = 1205 ppm.
The crude PPFO was collected from a solvent extraction plant in Perak, northern region of Peninsular, Malaysia.
Results are mean values ± standard deviation (n = 5) of duplicate degumming step.

Fig. 2. Effect of different acid dosage on phosphorus content reduction during acid degumming.

2016). The phosphorus content was reduced to 60 ppm in degummed
sunflower oil (Lamas et al., 2016). Table 2 shows the characteristics of
water-degummed PPFO (WD1) using various doses of hot distilled
water, which were 0.5, 1.0, 2.0, 3.0, 4.0, 5.0, and 6.0 v/v%. The crude
PPFO with a DOBI value of 1.38 (Table 1) is difficult to be bleached.
After the first water degumming step, the DOBI value of the PPFO had
increased to 1.94 ± 0.8 using 6.0 v/v% of hot distilled water. The
proportion of FFA in the water-degummed PPFO increased as gums
were removed gradually. This is in accordance with the results reported
by Lamas et al. (2016) for sunflower oil. Removal of phospholipids in
crude PPFO by water degumming caused an increase of FFA in the oil.
The increase of FFA detected was a consequence of the hydrolysis of
phospholipids. The moisture content of the water-degummed PPFO was
greater than crude PPFO due to the addition of the hot distilled water
during the process, indicating heat sensitivity to hydrolytic damage
(Vidrih et al., 2010). The water-degummed PPFO showed a decline in
carotene and vitamin E content, dropping from 1249 ppm to
1189 ± 25 ppm and 1205 ppm to 885 ± 23 ppm respectively, at 6.0
v/v% water dosage. It’s possible that the hot water and high tempera-
ture (90 °C) employed had destroyed some of the carotenes and vitamin
E present in PPFO.
3.2. Effect of acid dosage on phosphorus content and other oil properties
Acid degumming is expected to further decrease the phosphorus
content in water-degummed PPFO. Fig. 2 shows a further reduction of
phosphorus content using 1.0 wt% of phosphoric acid and citric acid,
from 95 ppm after the first step of PPFO water-degumming to 24 ppm
and 49 ppm, respectively. Phosphoric acid was found to be more ef-
fective in reducing the phosphorus content of the water-degummed
PPFO compared to citric acid under same dosage. After water degum-
ming, the remaining non-hydratable phospholipids were mainly phos-
phatidic acid bound to Mg2+ or Ca2+. The hydroxyl group in phos-
phoric acid dislodged the Ca2+ bound to phosphatidic acid and
precipitated. As a result, the non-hydratable phospholipids were de-
composed and transformed into insoluble lipid, which could be filtered
during the bleaching step. Acid degumming was required in this study
in order to completely remove phosphorus from PPFO. This is con-
sistent with the results obtained in a previous study that used water-
acid degumming (Chew et al., 2017). Zufarov et al., (2008) reported
that combination of water degumming and acid degumming removed
93% of phosphorus content from rapeseed oil. Table 3 shows the
characteristics of the acid-degummed PPFO. The DOBI of the acid-

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Table 3 3.3. Effect of bleaching earth dosage on phytonutrient content

Characteristics of acid-degummed palm-pressed fibre oil (PPFO).
Sample Acid dosage (wt DOBI Carotene content The minor components retained in the bleached PPFO such as car-
%) (ppm) otenoids and vitamin E were investigated. Bleaching was carried out
using NBE and ABE at three different doses, i.e., 0.1, 0.5 and 1.0 wt%.
Crude PPFO – 1.38 ± 0.04 1249 ± 17
Figs. 3 and 4 show the carotenoid and vitamin E content in the bleached
Water-degummed PPFO – 1.94 ± 0.29 1184 ± 13
Acid-degummed
PPFO. The results showed that 90% of the carotenoids were preserved
PPFO in the bleached PPFO after adsorption by both NBE and ABE. The NBE
Phosphoric acid 0.1 1.79 ± 0.01 1176 ± 25 had less active bonding sites to entrap carotenes compared to the ABE.
0.2 1.86 ± 0.02 1170 ± 19 Carotenes, part of colour pigments, are physically adsorbed by
0.3 1.93 ± 0.01 1163 ± 12
bleaching earth. The ABE was slightly stronger in the removal of car-
0.4 1.97 ± 0.01 1161 ± 19
0.5 1.95 ± 0.07 1163 ± 17 otenes due to an increase in specific surface area and pore volume
0.6 2.10 ± 0.05 1153 ± 9 during the thermal activation process. Table 4 shows the surface
0.7 2.11 ± 0.01 1129 ± 15 characteristics of both the bleaching earths. High specific surface area
0.8 2.31 ± 0.03 1123 ± 24
and pore volume in the ABE had contributed to higher removal of
0.9 2.41 ± 0.07 1113 ± 30
Citric acid 1.0 2.40 ± 0.10 1114 ± 23
carotenes from the crude PPFO compared to the NBE. The crude PPFO
0.1 1.72 ± 0.37 1098 ± 19 with an initial carotene content of 1249 ppm (Table 1) showed a slight
0.2 1.79 ± 0.04 1109 ± 25 reduction to 1138 ppm and 1126 ppm, when using 0.1 wt% of NBE and
0.3 1.81 ± 0.05 1098 ± 13 ABE, respectively (Fig. 3). Increasing the dosage of both types of
0.4 1.85 ± 0.01 1092 ± 33
bleaching earth did not change the carotenoid content significantly.
0.5 1.86 ± 0.05 1082 ± 15
0.6 1.90 ± 0.01 1082 ± 7 Vitamin E level decreased significantly with high doses of NBE and
0.7 1.91 ± 0.05 1077 ± 16 ABE, up to 1.0 wt% (Fig. 4). Degradation of Vitamin E by ABE was
0.8 2.02 ± 0.01 1071 ± 12 greater than NBE. The results showed that 71% and 61% of vitamin E
0.9 2.05 ± 0.08 1170 ± 22 was preserved when 0.5 wt% of NBE and ABE were used, respectively.
1.0 2.13 ± 0.01 1069 ± 27
The graphs show that increasing the bleaching earth dosage did not
Note: Crude palm-pressed fibre oil (PPFO) : Deterioration of bleachability index affect the adsorption of carotenoids and vitamin E. At the same time,
(DOBI) = 1.38; Carotene content = 1249 ppm. the bleaching activity can preserve the natural nutrient content in the
The crude PPFO was collected from a solvent extraction plant in Perak, bleached oil.
northern region of Peninsular Malaysia. Degumming effectiveness can also be measured by analysing trace
Results are mean values ± standard deviation (n = 5) of duplicate degumming metals such as copper and iron in the bleached PPFO as shown in
step. Table 5. The high value of trace metal contamination is due to high
wear and tear of the machineries in palm oil mills. During the pressing
process to extract crude PPFO, addition metal wear occurs, contributing
degummed PPFO were 2.40 ± 0.10 and 2.13 ± 0.01 after treating to the copper and iron contamination. Results indicated better copper
with 1.0 wt% of phosphoric acid and citric acid, respectively. In addi- removal using phosphoric acid. The levels of copper and iron were
tion, the carotenoid content of the acid-degummed PPFO was mostly reduced to less than 0.10 mg kg−1 and 12–15 mg kg−1 respectively
preserved. with increasing phosphoric acid doses from 0.1 to 1.0 wt%. Using
1.0 wt% phosphoric acid, the iron and copper contents were reduced by
78% and 83% respectively. Meanwhile, with 1.0 wt% of citric acid iron

Fig. 3. Carotene content of the bleached palm pressed fibre oil (PPFO).

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Fig. 4. Vitamin E content of the bleached palm pressed fibre oil (PPFO).

Table 4 content was significantly reduced by 89% compared to copper content

Surface characteristics of bleaching earth. which was reduced by just 8.3%. Hence, removal of transition metals
Bleaching earth Specific surface Total pore Pore size
economically from PPFO is possible with addition of water and acid.
area volume
(m2 g−1) (cm3 g−1) (nm)
3.4. Properties of RPPFO
Natural bleaching earth, NBE 242 0.363 6.0
Activated bleaching earth, 309 0.483 6.2
ABE Table 6 shows the properties of RPPFO obtained after the refining
process at optimum conditions: 5 v/v% hot distilled water in water
degumming, WD1 and WD2; 1.0 wt% of phosphoric acid in acid de-
gumming; 0.1 wt% of NBE in bleaching; and deacidification at 110 °C
Table 5 and 0.1 mtorr. The final phosphorus content of PPFO was 13 ± 2 ppm,
Trace metals in bleached palm-pressed fibre oil (PPFO). i.e., a 98% reduction. The trace metals in the final oil, i.e., iron and
Sample Acid dosage Copper (Cu) Iron (Fe) copper were less than 0.5 mg kg−1 and 0.1 mg kg−1, respectively. The
(wt %) (mg kg−1) (mg kg−1) undesirable smell caused by peroxides and hydroperoxides was re-
moved during deodorisation of oil. Meanwhile, the DOBI and FFA in the
Crude PPFO – 0.60 68.3
RPPFO were improved compared to the crude PPFO, i.e., from 1.99 to
Water-degummed PPFO – 0.55 16.0
Bleached PPFO
2.87 ± 0.17 and 5.94% to 0.15%, respectively. Carotenoid and vi-
Phosphoric acid 0.1 < 0.10 15.2 tamin E content were preserved after completing the refining process.
0.2 < 0.10 14.7 The optimum refining conditions in this study were selected based
0.3 < 0.10 13.5 mainly on the capability of the process to retain the highest carotene
0.4 < 0.10 13.9
and vitamin E content (89% and 82%, respectively) in RPPFO.
0.5 < 0.10 13.9
0.6 < 0.10 13.3
0.7 < 0.10 13.5
0.8 < 0.10 13.5 4. Conclusions
0.9 < 0.10 13.0
Citric acid 1.0 < 0.10 12.8
0.1 0.55 13.6
The refining process for the production of RPPFO under optimum
0.2 0.63 13.1 conditions has been successfully carried out. Water-degumming with
0.3 0.60 12.4 5.0 v/v% of hot distilled water at 90 °C for 20 min was able to ade-
0.4 0.55 11.8 quately remove hydratable phosphatides and at the same time increase
0.5 0.55 7.5
DOBI value from 2.0 to 2.9. Copper and iron were effectively removed
0.6 0.55 7.5
0.7 0.55 7.6 using both NBE and ABE. More than 80% of carotenoids and vitamin E
0.8 0.55 7.5 were retained under the investigated refining conditions.
0.9 0.53 7.4 Deacidification was recommended to be carried out at 110 °C and 0.1
1.0 0.55 7.4 mtorr via short path distillation process. The RPPFO is a rich source of
carotenes and other phytonutrients that can be further processed into
high value-added products.

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A.W. Nur Sulihatimarsyila et al. Industrial Crops & Products 129 (2019) 488–494

Table 6
Properties of crude palm-pressed fibre oil and refined palm-pressed fibre oil (RPPFO).
Sample Phosphorus DOBI FFA (%) Carotene content Vitamin E
content (ppm) (ppm) (ppm)

Crude PPFO 565 ± 9 1.99 ± 0.03 5.94 1357 ± 19 1106 ± 21

Water-degummed PPFO (WD1) 101 ± 3 2.62 ± 0.01 – 1358 ± 14 1097 ± 15
Water-degummed PPFO (WD2) 63 ± 7 2.65 ± 0.01 – 1323 ± 7 1048 ± 13
Acid-bleached PPFO 64 ± 5 2.58 ± 0.05 – 1317 ± 17 998 ± 25
RPPFO 13 ± 2 2.87 ± 0.17 0.15 1208 ± 23 904 ± 8

Note: The crude PPFO was collected from a solvent extraction plant in Johor, southern region of Peninsular, Malaysia.
Results are mean values ± standard deviation (n = 5) of duplicate refining process.

Acknowledgement Lau, H.L.N., Choo, Y.M., Ma, A.N., Chuah, C.H., 2007a. Production of refined carotene-
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