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Research Article
Received: 2 September 2017 Revised: 11 December 2017 Accepted article published: 18 December 2017 Published online in Wiley Online Library: 23 February 2018

(wileyonlinelibrary.com) DOI 10.1002/jsfa.8839

Stability evaluation of quality parameters for


palm oil products at low temperature storage
Nur Aainaa Syahirah Ramli,* Mohd Azmil Mohd Noor, Hajar Musa
and Razmah Ghazali

Abstract
BACKGROUND: Palm oil is one of the major oils and fats produced and traded worldwide. The value of palm oil products is
mainly influenced by their quality. According to ISO 17025:2005, accredited laboratories require a quality control procedure
with respect to monitoring the validity of tests for determination of quality parameters. This includes the regular use of internal
quality control using secondary reference materials. Unfortunately, palm oil reference materials are not currently available. To
establish internal quality control samples, the stability of quality parameters needs to be evaluated.

RESULTS: In the present study, the stability of quality parameters for palm oil products was examined over 10 months at low
temperature storage (6 ± 2 ∘ C). The palm oil products tested included crude palm oil (CPO); refined, bleached and deodorized
(RBD) palm oil (RBDPO); RBD palm olein (RBDPOo); and RBD palm stearin (RBDPS). The quality parameters of the oils [i.e.
moisture content, free fatty acid content (FFA), iodine value (IV), fatty acids composition (FAC) and slip melting point (SMP)]
were determined prior to and throughout the storage period. The moisture, FFA, IV, FAC and SMP for palm oil products changed
significantly (P < 0.05), whereas the moisture content for CPO, IV for RBDPO and RBDPOo, stearic acid composition for CPO and
linolenic acid composition for CPO, RBDPO, RBDPOo and RBDPS did not (P > 0.05). The stability study indicated that the quality
of the palm oil products was stable within the specified limits throughout the storage period at low temperature.

CONCLUSION: The storage conditions preserved the quality of palm oil products throughout the storage period. These findings
qualify the use of the palm oil products CPO, RBDPO, RBDPOo and RBDPS as control samples in the validation of test results.
© 2017 Society of Chemical Industry

Keywords: palm oil products; storage; stability; quality parameters; control sample

INTRODUCTION and the Malaysian Palm Oil Association (MPOA).4,5 Furthermore,


Palm oil is the most extensively used edible oil as a result of its ver- the identity characteristics of palm oil, palm olein and palm stearin
satility and competitive price compared to other edible oils. The are specified by Malaysian Standards MS 814, MS 816 and MS 815,
consumption of palm oil is increasing because of a growing global respectively.6–8 The quality of CPO is greatly influenced by the
demand driven largely by economic development.1 Malaysia is methods used during the harvesting, handling and processing of
one of the leading producers and exporters of palm oil and palm oil. The quality of palm oil products can be appraised through the
oil products worldwide. This accounts for 12% of oil and fat pro- inspection of physical and chemical properties of the palm oils. The
duction, as well as 27% of the export of oils and fats.2 Palm oil properties include moisture content, free fatty acid (FFA) content,
is obtained from the mesocarp of the palm fruits via the milling iodine value (IV), fatty acids composition (FAC) and slip melting
process for further end-user applications. Crude palm oil (CPO) point (SMP). The quality parameters of palm oil products deter-
is refined to remove impurities such as an undesirable odor, fla- mined are used to confirm whether the oils have been produced,
vor and colour, at the same time as retaining the beneficial com- processed, refined and stored properly.
ponents such as anti-oxidants and vitamins.3 CPO is processed Water is one of the most common impurities in palm oil products.
into refined products, including refined, bleached and deodorized Controlling the moisture content within the permissible limit is
palm oil (RBDPO); refined, bleached and deodorized palm olein important because a high moisture content will influence the
(RBDPOo); and refined, bleached and deodorized palm stearin hydrolytic stability of the palm oil products.5 FFA content is an
(RBDPS). These refined palm oils are utilized in various applica-
tions. For example, RBDPO is used to produce margarine, shorten-
ing and ice cream; RBDPOo is used in cooking oils; and RBDPS is ∗ Correspondence to: NAS Ramli, Quality and Environmental Assessment
used in the manufacture of soaps, fuels and emulsifiers.3 Unit, Advanced Oleochemical Technology Division, Malaysian Palm Oil
Important aspects relating to the quality and stability of palm Board (MPOB), Persiaran Institusi, Bandar Baru Bangi, Selangor, Malaysia.
E-mail: aainaa.syahirah@mpob.gov.my
oil products have to be considered because they are the main fac-
tors influencing market acceptability and value. All palm oil prod- Quality and Environmental Assessment Unit, Advanced Oleochemical Technol-
ucts in Malaysia are traded in accordance with the specifications ogy Division, Malaysian Palm Oil Board (MPOB), Persiaran Institusi, Bandar
3351

developed by Palm Oil Refiners Association of Malaysia (PORAM) Baru Bangi, Selangor, Malaysia

J Sci Food Agric 2018; 98: 3351–3362 www.soci.org © 2017 Society of Chemical Industry
10970010, 2018, 9, Downloaded from https://onlinelibrary.wiley.com/doi/10.1002/jsfa.8839 by Universite Du Quebec A Chicout, Wiley Online Library on [15/12/2022]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License
www.soci.org NAS Ramli et al.

important indicator for quality of palm oil products because it is


Table 1. Quality parameters of CPO, RBDPO, RBDPOo and RBDPS
allied with the economic value of the edible oils.9,10 During storage, from COA by Sime Darby Jomalina
FFA is released from the hydrolysis reaction of oil.5 A high level of
FFA content implies that the palm oil product is very rancid and of Quality parameters
poor quality. IV is used to measure the unsaturated fatty acids or Palm oil Moisture FFA IV FAC SMP
double bonds in the palm oil products, which can react with the products (%) (%) (g 100 g –1 oil) (%) (∘ C)
iodine compound. Furthermore, IV reflects the vulnerability of the
oil sample to oxidation. CPO 0.17 3.070 53.11 ND ND
Fatty acids are categorized by their degree of saturations, com- RBDPO 0.02 0.051 51.90 ND 37.0
prising saturated, monounsaturated, and polyunsaturated fatty RBDPOo 0.04 0.051 57.74 ND 22.6
acids. The information on FAC of palm oil products is important in RBDPS 0.03 0.032 35.20 ND 52.8
the development and marketing of new products. This is because
ND, not determined.
the proportions and positions of fatty acids on the glycerol back-
bone influence the physicochemical and nutritional characteris-
tics of the oils.9 Meanwhile, the SMP of the palm oil products is
defined as the temperature at which the solidified oil becomes Table 2. Initial moisture, FFA, IV and SMP of CPO, RBDPO, RBDPOo
sufficiently fluid to slip in an open capillary tube.11 The SMP can and RBDPS
be a good indicator of the general behavior of the palm oil prod-
Quality parameters
ucts at various temperatures, including cool, ambient and elevated
temperatures.9 In addition, the SMP is useful in the formulation of Palm oil Moisture IV
new products and the consistency of a finished product can be products (%) FFA (%) (g 100 g –1 oil) SMP (∘ C)
envisaged.9
CPO 0.12 ± 0.01 3.170 ± 0.00 53.49 ± 0.03 36.0 ± 0.00
In parallel with the storage time, factors such as storage condi-
RBDPO 0.04 ± 0.00 0.045 ± 0.00 52.69 ± 0.15 37.2 ± 0.00
tions and packaging materials can also affect the quality of palm
RBDPOo 0.01 ± 0.00 0.054 ± 0.00 57.67 ± 0.28 22.0 ± 0.00
oil products, edible oils and other vegetable oils.10,12–20 Appropri-
RBDPS 0.03 ± 0.01 0.041 ± 0.00 34.92 ± 0.02 51.4 ± 0.00
ate storage conditions and packaging materials can help prevent
the oils from being exposed to factors that cause oxidation and
hydrolysis reactions. In a storage stability study, CPO showed faster
deterioration when stored at a temperature > 30 ∘ C compared to conditions for the purpose of establishing internal quality control
when stored at a temperature < 20 ∘ C.13 Furthermore, the changes samples. As a result of the stability of a reference sample being ver-
in quality parameters of RBDPO in storage at 60 ∘ C experienced a ified because the sample is stored in darkness and at a controlled
greater degree of deterioration than the oil system at a room tem- temperature of between 0 and 8 ∘ C,27 the palm oil product samples
perature of 28 ± 1 ∘ C.12 Moreover, it was reported that the oxida- were stored in a transparent glass bottle and in a dark cold room at
tive properties of palm oil after 4 months of storage were best 6 ± 2 ∘ C within the specified storage period. Several quality param-
preserved under refrigerating conditions.16 The effects of different eters were chosen and evaluated; moisture content, FFA content,
packaging materials on the quality of palm oil products and edible IV, FAC and SMP. The present study will confirm whether the qual-
oils have been evaluated. The packaging materials include glass ity of the palm oil products, stored under the specified conditions,
bottles, polyethylene terephthalate (PET) bottles, amber glass bot- is stable throughout the storage period. The suitability of the palm
tles and laminated pouches.10,14,21–24 oil products for use as control samples throughout the 10 months
Palm oil products with a maintained and preserved quality is determined by examining the stability of their quality parame-
throughout the specified storage condition and storage period ters within the specified control limits.
can be employed as secondary reference materials or control
samples. According to ISO 17025:2005, accredited laboratories
require a quality control procedure for monitoring the validity MATERIALS AND METHODS
of tests. This includes the regular use of internal quality control Materials
using secondary reference materials. The use of a control sample The palm oil products; CPO, RBDPO, RBDPOo and RBDPS were
allows an assessment of the instrument’s performance, calibration, purchased from Sime Darby Jomalina (Selangor, Malaysia). Mois-
analytical procedure and analyst, as well as the influences of ture content, FFA content, IV, FAC and SMP of the palm oil
environmental conditions.25 To be considered as control samples, products shown in Table 1 were obtained from the certificate
palm oil products must have several properties, including stability. of analysis (COA) provided by Sime Darby Jomalina. Meanwhile,
According to ISO Guide 30, the stability of a reference sample can all of the chemicals and solvents used for the analyses were
be defined as the ability to maintain the quality within specified of analytical grade. The equipment used in the present study
limits for a specified storage period.26 The stability of a reference comprised an oven (model ULM 500; Memmert, Schwabach,
sample is verified because the sample is stored in darkness and at Germany), analytical balance (model HR 250A; AD Instruments,
a controlled temperature of between 0 and 8 ∘ C.26,27 In a stability Sydney, Australia), hot plate (Cimarec, model SP 131320-33;
study, the limits are set at ±3𝜎 (SD). If the values were found to Thermo Scientific, Waltham, MA, USA), gas chromatograph (HP
be outside the pre-defined limits, corrective action is taken to 6890 Series, capillary column HP-88; Agilent Technologies Inc.,
correct the problem and to prevent incorrect results from being Santa Clara, CA, USA), capillary tube for SMP (Microhematocrit;
reported.28 length 75 ± 0.02 mm, inner diameter 1.1–1.2 mm, outer diameter
The present study aimed to evaluate the quality parameters 1.3–1.4 mm, wall 0.2 ± 0.02 mm; Fisherbrand, Fisher Scientific
of several palm oil products (CPO, RBDPO, RBDPOo and RBDPS) Co., Pittsburgh, PA, USA) and a waterbath (model F34; Julabo,
3352

within a storage period of 10 months under specified storage Seelbach, Germany).

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Table 3. Initial FAC (%) OF CPO, RBDPO, RBDPOo and RBDPS

Fatty acids composition


Palm oil products C14:0 C16:0 C16:1 C18:0 C18:1 C18:2 C18:3

CPO 1.0 ± 0.00 44.1 ± 0.03 0.2 ± 0.01 4.2 ± 0.01 39.5 ± 0.00 9.7 ± 0.02 0.3 ± 0.00
RBDPO 1.0 ± 0.00 43.9 ± 0.01 0.2 ± 0.00 4.3 ± 0.00 39.7 ± 0.01 9.8 ± 0.01 0.2 ± 0.00
RBDPOo 1.0 ± 0.00 39.4 ± 0.03 0.2 ± 0.00 4.0 ± 0.01 43.4 ± 0.01 10.8 ± 0.03 0.2 ± 0.00
RBDPS 1.2 ± 0.00 58.4 ± 0.00 0.1 ± 0.00 5.0 ± 0.01 28.7 ± 0.00 5.6 ± 0.01 0.1 ± 0.00

where M is the mass (g) of the dish, Mb is the mass (g) of the dish
Table 4. Changes in moisture content (%) of CPO, RBDPO, RBDPOo
and RBDPS during storage and oil, and Md is the mass (g) of the dish and oil after drying.

Palm oil products Determination of FFA


Storage period The MPOB test method, MPOB p2.5:200429 was employed to
(month) CPOa RBDPOb RBDPOob RBDPSb determine the FFA content in the palm oil products. The FFA
content was expressed as the percentage of palmitic acid. The
0 0.12 ± 0.01 0.04 ± 0.00 0.01 ± 0.00 0.03 ± 0.01 melted and homogenized oil sample was weighed into a conical
1 0.08 ± 0.01 0.05 ± 0.00 0.02 ± 0.00 0.04 ± 0.00 flask. Next, 50 mL of the neutralized isopropanol was added to
2 0.11 ± 0.01 0.08 ± 0.01 0.07 ± 0.01 0.04 ± 0.01 the flask, followed by a few drops of phenolphthalein. Then, the
3 0.12 ± 0.01 0.04 ± 0.01 0.03 ± 0.00 0.02 ± 0.00 conical flask was placed on a hot plate at 40 ∘ C. The flask was
4 0.09 ± 0.01 0.01 ± 0.00 0.02 ± 0.00 0.02 ± 0.00 gently swirled at the same time as being titrated with sodium
5 0.12 ± 0.01 0.02 ± 0.00 0.02 ± 0.00 0.01 ± 0.00 hydroxide (NaOH) standard solution until the appearance of the
6 0.10 ± 0.01 0.01 ± 0.00 0.05 ± 0.01 0.03 ± 0.01 first permanent pink colour. The FFA content was expressed as:
7 0.10 ± 0.01 0.06 ± 0.02 0.05 ± 0.01 0.01 ± 0.00
8 0.06 ± 0.01 0.04 ± 0.01 0.04 ± 0.01 0.05 ± 0.01 25.6 × M × V
FFA as palmitic acid (%) = (2)
9 0.11 ± 0.00 0.05 ± 0.01 0.04 ± 0.02 0.07 ± 0.02 m
10 0.13 ± 0.00 0.06 ± 0.00 0.08 ± 0.00 0.05 ± 0.00
where M is the molarity (mol L –1 ) of standard NaOH solution, V is
a No significant change (P > 0.05). the volume (mL) of the standard NaOH solution used and m is the
b Significant change (P < 0.05).
mass (g) of the oil sample.

Determination of IV
Storage conditions
The IV of the palm oil products was determined in accordance with
Upon receipt, the palm oil products were stirred well before
the procedure specified in AOCS method: AOCS Cd 1d-92.30 The
transferred into several 60 mL clear glass bottles with a screw cap.
oil sample was melted, homogenized, filtered, allowed to achieve
Then, the oil samples were placed in desiccators and stored in
a temperature of 68–71 ∘ C and then weighed into a conical flask.
a dark cold room at 6 ± 2 ∘ C. This storage condition was chosen
Next, 15 mL of cyclohexane:acetic acid (1:1) solution and 25 mL of
because the stability of a reference sample is tested when the
Wijs solution were added to the conical flask. The contents were
sample is stored in darkness and at a controlled temperature of
mixed thoroughly and stored in a dark place at room temperature
between 0 and 8 ∘ C.27 All oil samples were analyzed for moisture
for 1 h. Then, 20 mL of 10% potassium iodide (KI) solution was
content, FFA content, IV, FAC and SMP prior to and throughout the
added, followed by 100 mL of distilled water. The mixture was then
storage period. The analyses were conducted in accordance with
titrated with 0.1 mol L –1 sodium thiosulfate (Na2 S2 O3 ) standard
the Malaysian Palm Oil Board (MPOB) and American Oil Chemists’
solution until the yellow color almost disappeared. Starch indicator
Society (AOCS) standard methods. Data were collected monthly for
solution (1–2 mL) was added to the mixture and the titration was
10 months.
continued until the blue colour disappeared. The blank sample
was titrated in the same manner as described herein. The IV was
Determination of moisture content
computed using:
The determination of moisture content in the palm oil products
( )
was carried out using a MPOB test method: MPOB p2.1:2004.29 12.69 × C × V1 − V2
The method consisted of heating the oil sample in an oven at IV (g 100 g–1 oil) = (3)
m
103 ± 2 ∘ C, until moisture and volatile substances were completely
eliminated. The oil sample was weighed (approximately 10 g to the where C is the molarity (mol L –1 ) of the Na2 S2 O3 solution, V 1 is the
nearest 0.001 g) into a Petri dish that had previously been dried volume (mL) of Na2 S2 O3 solution used for the blank test, V 2 is the
and cooled in desiccators. The Petri dish with the oil sample was volume (mL) of Na2 S2 O3 solution used for the sample test and m is
placed in an oven at 103 ∘ C for 2.5 h and then allowed to cool to the mass (g) of the oil sample.
room temperature (23–25 ∘ C) in a desiccator for 30 min, followed
by weighing. This step was repeated until a constant weight was Determination of FAC
obtained. The moisture content was calculated in accordance with: The AOCS test methods were applied to determine the FAC of
Mb − Md the palm oil products. AOCS Ce 2-66 was used in the prepara-
3353

Moisture (%) = × 100 (1) tion of fatty acid methyl esters (FAME), whereas AOCS Ce 1-62
Mb − M

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10970010, 2018, 9, Downloaded from https://onlinelibrary.wiley.com/doi/10.1002/jsfa.8839 by Universite Du Quebec A Chicout, Wiley Online Library on [15/12/2022]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License
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0.18 CPO RBDPO


UCL 0.12 UCL
0.15

Moisture content (%)


Moisture content (%)

0.08
0.12

0.09
0.04

0.06
LCL LCL
0.00
0.03

0 1 2 3 4 5 6 7 8 9 10 0 1 2 3 4 5 6 7 8 9 10
Storage period (month) Storage period (month)

RBDPOo 0.12
RBDPS
0.12
UCL
UCL

0.08
Moisture content (%)

Moisture content (%)


0.08

0.04
0.04

LCL LCL
0.00 0.00

0 1 2 3 4 5 6 7 8 9 10 0 1 2 3 4 5 6 7 8 9 10
Storage period (month) Storage period (month)

Figure 1. Control chart of moisture content stability for CPO, RBDPO, RBDPOo and RBDPS (UCL: upper control limit at +3𝜎, LCL: lower control limit at –3𝜎).

was performed for quantitative analysis of FAC. The preparation


of FAME is necessary to improve volatility of the methyl ester
Table 5. Changes in FFA content (%) of CPO, RBDPO, RBDPOo and
derivatives. Gas chromatography (model 6890; Agilent Technolo- RBDPS during storage
gies Inc.) equipped with a flame ionization detector (FID) was used
to determine the FAC of the tested palm oil products. The col- Palm oil products
umn used was capillary column HP-88 (60 m × 250 μm × 0.2 μm), Storage
with a flow rate of 0.8 mL min –1 . The injector temperature and period (month) CPOa RBDPOa RBDPOoa RBDPSa
FID temperature were both set at 250 ∘ C. The oven temperature
was initially set at 150 ∘ C, and then programmed to 210 ∘ C for 0 3.17 ± 0.00 0.045 ± 0.00 0.054 ± 0.00 0.041 ± 0.00
10 min at a rate of 3 ∘ C min –1 . The injection volume was 1 μL 1 3.12 ± 0.01 0.049 ± 0.00 0.056 ± 0.00 0.042 ± 0.00
and the total run time was 30 min. The peaks from the gas chro- 2 3.23 ± 0.01 0.049 ± 0.00 0.057 ± 0.00 0.042 ± 0.00
matogram were distinguished based on the retention times using 3 3.08 ± 0.00 0.051 ± 0.00 0.058 ± 0.00 0.044 ± 0.00
FAME standards. 4 3.18 ± 0.00 0.051 ± 0.00 0.056 ± 0.00 0.056 ± 0.00
5 3.19 ± 0.00 0.053 ± 0.00 0.058 ± 0.00 0.058 ± 0.00
Determination of the SMP 6 3.18 ± 0.00 0.058 ± 0.00 0.053 ± 0.00 0.058 ± 0.00
The SMP of the palm oil products was measured by applying 7 3.22 ± 0.00 0.055 ± 0.00 0.060 ± 0.00 0.059 ± 0.00
the AOCS test method: AOCS C c3-25.30 This method follows the 8 3.23 ± 0.02 0.053 ± 0.00 0.058 ± 0.00 0.053 ± 0.00
open capillary tube technique. The melted and homogenized oil 9 3.26 ± 0.00 0.054 ± 0.00 0.061 ± 0.00 0.055 ± 0.00
sample was filtered at 60 ∘ C in oven and then left in the oven 10 3.27 ± 0.00 0.053 ± 0.00 0.060 ± 0.00 0.070 ± 0.00
for 10 min. Three capillary tubes were dipped into the melted oil a Significant change (P < 0.05).
sample until the oil rises approximately 10 mm high in the tube.
3354

Then, the tubes containing the oil sample were chilled until the

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CPO 0.070 RBDPO


3.4 UCL UCL
0.063
3.3

FFA content (%)


FFA content (%)

0.056

3.2
0.049

3.1
0.042 LCL
LCL
3.0
0.035

0 1 2 3 4 5 6 7 8 9 10 0 1 2 3 4 5 6 7 8 9 10
Storage period (month) Storage period (month)

0.070 RBDPOo RBDPS


0.090
UCL
UCL
0.065 0.075
FFA content (%)

FFA content (%)

0.060 0.060

0.045
0.055

LCL 0.030 LCL


0.050

0.015

0 1 2 3 4 5 6 7 8 9 10 0 1 2 3 4 5 6 7 8 9 10
Storage period (month) Storage period (month)

Figure 2. Control chart of FFA content stability for CPO, RBDPO, RBDPOo and RBDPS (UCL: upper control limit at +3𝜎, LCL: lower control limit at –3𝜎).

sample solidified by holding the tubes against ice. These tubes


were placed in a beaker and held in refrigerator at 10 ± 1 ∘ C for Table 6. Changes in IV (g 100 g –1 oil) of CPO, RBDPO, RBDPOo and
RBDPS during storage
16 h. After 16 h, the tubes were removed from the refrigerator and
attached to thermometer using rubber band. The thermometer Palm oil products
was suspended in a 400-mL beaker containing distilled water. The
Storage period
starting bath temperature was adjusted to 8–10 ∘ C below the
(month) CPOb RBDPOa RBDPOoa RBDPSa
expected SMP of the oil sample. The water bath was stirred with
a magnetic stirrer and heat was then applied to increase the water 0 53.49 ± 0.03 52.69 ± 0.15 57.67 ± 0.28 34.92 ± 0.02
bath temperature at a rate of 1 ∘ C min –1 then reduced to 0.5 ∘ C 1 53.18 ± 0.03 52.61 ± 0.11 57.71 ± 0.10 35.25 ± 0.06
min –1 as the SMP approached. The temperature at which each 2 53.15 ± 0.08 52.69 ± 0.08 57.89 ± 0.11 35.02 ± 0.26
column rises was observed and the average temperature of all 3 53.20 ± 0.11 52.58 ± 0.08 57.63 ± 0.18 35.33 ± 0.04
capillary tubes was recorded as the SMP. 4 53.66 ± 0.07 52.77 ± 0.06 57.59 ± 0.08 35.51 ± 0.06
5 53.59 ± 0.17 52.73 ± 0.27 57.69 ± 0.12 35.82 ± 2.16
Statistical analysis 6 53.71 ± 0.18 52.71 ± 0.16 57.53 ± 0.04 35.60 ± 0.11
All analyses were conducted in duplicate. In the statistical anal- 7 53.41 ± 0.23 52.47 ± 0.11 57.36 ± 0.04 35.40 ± 0.01
ysis, the data obtained from the duplicate tests were within the 8 53.70 ± 0.05 52.72 ± 0.13 57.51 ± 0.15 35.39 ± 0.08
repeatability limit of the respective analysis. The results relating 9 53.43 ± 0.20 52.52 ± 0.04 57.40 ± 0.18 35.43 ± 0.05
to the quality parameters of oil samples were expressed as the 10 53.26 ± 0.14 52.49 ± 0.29 57.38 ± 0.11 35.32 ± 0.01
mean ± SD. Data were subjected to one-way analysis of variance a No significant change (P > 0.05).
using XLSTAT (Addinsoft, New York, NY, USA). P ≤ 0.05 was consid- b Significant change (P < 0.05).
3355

ered statistically significant. The control charts were established

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54.5 CPO RBDPO


53.0 UCL
UCL
54.0
52.8
IV (g/100g oil)

IV (g/100g oil)
53.5
52.6

53.0
LCL 52.4
LCL

52.5
52.2

0 1 2 3 4 5 6 7 8 9 10 0 1 2 3 4 5 6 7 8 9 10
Storage period (month) Storage period (month)

RBDPOo RBDPS
58.25 36.5
UCL
UCL
58.00
36.0
IV (g/100g oil)

IV (g/100g oil)

57.75
35.5
57.50

35.0
57.25
LCL LCL
57.00 34.5

0 1 2 3 4 5 6 7 8 9 10 0 1 2 3 4 5 6 7 8 9 10
Storage period (month) Storage period (month)

Figure 3. Control charts of IV (g 100 g –1 oil) stability for CPO, RBDPO, RBDPOo and RBDPS (UCL: upper control limit at +3𝜎, LCL: lower control limit at –3𝜎).

by applying the upper and lower control limits +3𝜎 and –3𝜎, analytical methods when determining the quality parameters,
respectively. as well as other factors, such as the storage time before the
procurement of oils.

RESULTS AND DISCUSSIONS Changes in moisture content


Initial quality parameters of palm oil products Low moisture content is important for controlling the deteriora-
The initial moisture content, FFA content, IV and SMP of CPO, tion of oil samples because the presence of moisture promotes
RBDPO, RBDPOo and RBDPS used in the present study are pre- hydrolysis, which leads to an increase in FFA content. Table 4 shows
sented in Table 2, whereas the FAC of the palm oil products are the moisture content of the palm oil products obtained during
shown in Table 3. The fatty acids include saturated fatty acids storage. There was no significant change in moisture content for
myristic (C14:0), palmitic (C16:0) and stearic (C18:0); monoun- CPO (P > 0.05). On the other hand, the moisture content for RBDPO,
saturated fatty acids palmitoleic (C16:1) and oleic (C18:1); and RBDPOo and RBDPS was observed to vary significantly (P < 0.05)
polyunsaturated fatty acids linoleic (C18:2) and linolenic (C18:3). over 10 months. A study carried out on CPO, which was packaged
The values in Tables 2 and 3 are obtained from the analyses. in different containers and stored at room temperature, found a
The quality parameters of the palm oil products before stor- significant change in the moisture content (P < 0.05), with values
age were within the range specified by MPOA, PORAM and from 0.39% to 0.56% being recorded after 3 months of storage.14
Malaysian Standards.4–8 The range of quality parameters of Meanwhile, Augustin et al.13 reported a moisture content for CPO
the palm oil products by MPOA, PORAM and Malaysian Stan- of 1.15% and 0.25%. A moisture content of CPO higher than the
dards is provided further below. The initial quality parameters norm of 0.25–0.30% was probably attributed to the accumulation
of the palm oil products determined after being received of water at the bottom of storage tank. This condition led to an
(Table 2) were significantly different (P < 0.05) from the COA increase in the moisture content of CPO obtained from the bot-
3356

(Table 1). The difference is probably a result of the use of different tom of storage tank.13 Furthermore, it is important to note that the

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Table 7. Changes in FAC (%) of CPO, RBDPO, RBDPOo and RBDPS during storage

Storage period (month) Fatty acids


CPO C14:0b C16:0b C16:1b C18:0* C18:1b C18:2b C18:3a

0 1.01 ± 0.00 44.10 ± 0.03 0.16 ± 0.01 4.24 ± 0.01 39.49 ± 0.00 9.71 ± 0.02 0.27 ± 0.00
1 1.00 ± 0.01 44.10 ± 0.03 0.15 ± 0.00 4.25 ± 0.01 39.54 ± 0.03 10.07 ± 0.01 0.26 ± 0.01
2 0.98 ± 0.00 43.80 ± 0.05 0.15 ± 0.00 4.27 ± 0.01 39.77 ± 0.01 9.76 ± 0.00 0.27 ± 0.00
3 1.00 ± 0.00 43.99 ± 0.01 0.15 ± 0.00 4.25 ± 0.01 39.66 ± 0.02 9.75 ± 0.01 0.27 ± 0.00
4 1.00 ± 0.01 43.81 ± 0.04 0.15 ± 0.00 4.26 ± 0.01 39.88 ± 0.01 9.68 ± 0.06 0.26 ± 0.01
5 0.98 ± 0.01 43.83 ± 0.01 0.15 ± 0.00 4.26 ± 0.03 39.97 ± 0.02 9.71 ± 0.02 0.26 ± 0.00
6 1.00 ± 0.00 43.95 ± 0.08 0.15 ± 0.00 4.24 ± 0.02 39.85 ± 0.04 9.76 ± 0.02 0.27 ± 0.00
7 1.00 ± 0.00 43.97 ± 0.04 0.15 ± 0.00 4.24 ± 0.03 39.82 ± 0.00 9.72 ± 0.05 0.27 ± 0.00
8 0.98 ± 0.01 43.70 ± 0.07 0.15 ± 0.00 4.29 ± 0.01 40.07 ± 0.07 9.74 ± 0.01 0.27 ± 0.00
9 1.02 ± 0.00 43.97 ± 0.07 0.16 ± 0.00 4.26 ± 0.01 39.72 ± 0.04 9.72 ± 0.02 0.27 ± 0.00
10 1.01 ± 0.00 43.92 ± 0.00 0.20 ± 0.00 4.29 ± 0.01 39.80 ± 0.00 9.70 ± 0.00 0.27 ± 0.00
RBDPO C14:0b C16:0b C16:1b C18:0b C18:1b C18:2b C18:3a
0 1.01 ± 0.00 43.87 ± 0.01 0.15 ± 0.00 4.25 ± 0.00 39.74 ± 0.01 9.75 ± 0.01 0.19 ± 0.00
1 1.01 ± 0.01 43.78 ± 0.01 0.16 ± 0.01 4.25 ± 0.01 39.81 ± 0.03 9.77 ± 0.04 0.19 ± 0.00
2 0.99 ± 0.00 43.67 ± 0.01 0.15 ± 0.00 4.27 ± 0.01 39.90 ± 0.01 9.79 ± 0.01 0.19 ± 0.01
3 1.01 ± 0.00 43.97 ± 0.01 0.15 ± 0.00 4.24 ± 0.00 39.74 ± 0.01 9.75 ± 0.01 0.19 ± 0.00
4 1.02 ± 0.00 43.79 ± 0.03 0.15 ± 0.00 4.24 ± 0.00 40.00 ± 0.01 9.71 ± 0.01 0.19 ± 0.00
5 1.01 ± 0.00 43.79 ± 0.02 0.15 ± 0.00 4.22 ± 0.00 39.94 ± 0.03 9.79 ± 0.01 0.19 ± 0.00
6 1.02 ± 0.01 43.86 ± 0.01 0.15 ± 0.00 4.25 ± 0.00 39.94 ± 0.02 9.74 ± 0.00 0.18 ± 0.00
7 1.01 ± 0.00 43.87 ± 0.01 0.15 ± 0.00 4.23 ± 0.01 39.96 ± 0.01 9.74 ± 0.00 0.19 ± 0.01
8 1.01 ± 0.00 43.57 ± 0.08 0.15 ± 0.00 4.27 ± 0.00 40.14 ± 0.08 9.77 ± 0.01 0.19 ± 0.00
9 1.01 ± 0.00 43.73 ± 0.06 0.19 ± 0.00 4.30 ± 0.02 39.97 ± 0.06 9.70 ± 0.01 0.19 ± 0.00
10 1.02 ± 0.00 43.81 ± 0.01 0.2 ± 0.00 4.28 ± 0.00 39.90 ± 0.00 9.70 ± 0.00 0.19 ± 0.00
RBDPOo C14:0b C16:0b C16:1b C18:0b C18:1b C18:2b C18:3a
0 0.98 ± 0.00 39.37 ± 0.03 0.17 ± 0.00 4.03 ± 0.01 43.35 ± 0.01 10.80 ± 0.03 0.22 ± 0.00
1 0.97 ± 0.00 39.25 ± 0.05 0.20 ± 0.00 4.04 ± 0.01 43.43 ± 0.06 10.81 ± 0.05 0.22 ± 0.01
2 0.97 ± 0.01 39.24 ± 0.04 0.17 ± 0.00 4.05 ± 0.00 43.48 ± 0.03 10.81 ± 0.01 0.21 ± 0.00
3 0.98 ± 0.00 39.39 ± 0.00 0.17 ± 0.00 4.03 ± 0.01 43.42 ± 0.00 10.79 ± 0.01 0.22 ± 0.00
4 0.98 ± 0.01 39.24 ± 0.03 0.18 ± 0.01 4.04 ± 0.01 43.66 ± 0.04 10.70 ± 0.02 0.21 ± 0.00
5 0.98 ± 0.00 39.31 ± 0.03 0.17 ± 0.00 4.02 ± 0.00 43.59 ± 0.06 10.82 ± 0.03 0.21 ± 0.00
6 0.97 ± 0.01 39.25 ± 0.06 0.18 ± 0.01 4.05 ± 0.01 43.62 ± 0.01 10.82 ± 0.06 0.21 ± 0.01
7 0.98 ± 0.00 39.28 ± 0.03 0.17 ± 0.00 4.02 ± 0.00 43.64 ± 0.01 10.80 ± 0.01 0.21 ± 0.00
8 0.96 ± 0.01 38.88 ± 0.08 0.17 ± 0.00 4.08 ± 0.00 43.94 ± 0.06 10.81 ± 0.01 0.21 ± 0.00
9 0.97 ± 0.01 39.16 ± 0.07 0.17 ± 0.00 4.09 ± 0.01 43.68 ± 0.06 10.73 ± 0.01 0.21 ± 0.00
10 0.98 ± 0.01 39.20 ± 0.05 0.20 ± 0.00 4.08 ± 0.01 43.65 ± 0.07 10.70 ± 0.00 0.21 ± 0.00
RBDPS C14:0b C16:0b C16:1b C18:0b C18:1b C18:2b C18:3a
0 1.19 ± 0.00 58.44 ± 0.00 0.09 ± 0.00 4.97 ± 0.01 28.71 ± 0.00 5.57 ± 0.01 0.10 ± 0.00
1 1.18 ± 0.01 58.39 ± 0.00 0.09 ± 0.01 4.99 ± 0.02 28.78 ± 0.00 5.57 ± 0.02 0.09 ± 0.01
2 1.17 ± 0.01 58.24 ± 0.16 0.09 ± 0.00 5.01 ± 0.01 28.88 ± 0.11 5.60 ± 0.04 0.10 ± 0.00
3 1.19 ± 0.00 58.50 ± 0.00 0.09 ± 0.00 4.96 ± 0.01 28.75 ± 0.00 5.58 ± 0.01 0.09 ± 0.01
4 1.18 ± 0.00 58.24 ± 0.04 0.09 ± 0.00 4.99 ± 0.01 29.00 ± 0.03 5.56 ± 0.00 0.10 ± 0.00
5 1.20 ± 0.00 58.56 ± 0.03 0.09 ± 0.00 4.97 ± 0.01 28.80 ± 0.03 5.55 ± 0.00 0.09 ± 0.00
6 1.18 ± 0.00 58.37 ± 0.00 0.09 ± 0.00 4.98 ± 0.01 28.96 ± 0.00 5.56 ± 0.01 0.09 ± 0.01
7 1.18 ± 0.01 58.47 ± 0.02 0.09 ± 0.00 4.99 ± 0.01 28.91 ± 0.02 5.53 ± 0.00 0.09 ± 0.00
8 1.17 ± 0.00 58.02 ± 0.06 0.09 ± 0.00 5.04 ± 0.01 29.18 ± 0.04 5.60 ± 0.00 0.10 ± 0.00
9 1.19 ± 0.00 58.32 ± 0.05 0.09 ± 0.01 5.02 ± 0.01 29.93 ± 0.04 5.56 ± 0.01 0.09 ± 0.00
10 1.19 ± 0.01 58.19 ± 0.05 0.10 ± 0.00 5.04 ± 0.01 29.00 ± 0.00 5.60 ± 0.00 0.10 ± 0.00
a No significant change (P > 0.05).
b Significant change (P < 0.05).

packaging and processing of the oil may also contribute to the vari- RBDPOo and RBDPS, respectively.5 Based on the control charts
ation in moisture content.10 shown in Fig. 1, it is confirmed that the palm oil products were sta-
The changes in moisture content of the palm oil products in the ble for 10 months under the storage condition because the mois-
present study were still below the limit of specifications estab- ture content was still within the upper and lower control limits.
lished by MPOA and PORAM. The maximum permissible mois- Thus, CPO, RBDPO, RBDPOo and RBDPS can be used as control
3357

ture contents are 0.25%, 0.1%, 0.1% and 0.15% for CPO, RBDPO, materials for moisture content analysis of the respective oils.

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www.soci.org NAS Ramli et al.

were significant changes (P < 0.05) in the FFA content of all palm
Table 8. FAC (%) for palm oil, palm olein and palm stearin by
Malaysian Standards oil products within the storage duration of 10 months. A high FFA
content can ultimately lead to rancidity, which subsequently alters
Palm oil products the sensory and nutritive value of the palm oil products.31 The
Palm oil Palm olein Palm stearin hydrolysis of palm oil products is an autocatalytic reaction, where
Fatty acids (MS 814) (MS 816) (MS 817) the FFA produced from the reaction will continuously increase
with the storage period.5 In previous study, a significant increase
C14:0 (myristic) 0.9–1.5 0.9–1.2 1.1–1.7 to 0.15% and 0.22% (P < 0.05) was observed in the FFA content for
C16:0 (palmitic) 39.2–45.8 38.2–42.9 49.8–68.1 RBDPOo after 52 days of storage at 28 and 60 ∘ C, respectively.12
C16:1 (palmitoleic) 0.0–0.4 0.1–0.3 < 0.05–0.1 Meanwhile, the FFA content for CPO changed significantly from
C18:0 (stearic) 3.7–5.1 3.7–4.8 3.9–5.6 4.46% to 8.03% (P < 0.001) after 3 months of storage at 20 ∘ C13 and
C18:1 (oleic) 37.4–44.1 39.8–43.9 20.4–34.4 increased from 7.0% to 8.30% (P < 0.05) at room temperature.14
C18:2 (linoleic) 8.7–12.5 10.4–12.7 5.0–8.9 The difference in the FFA content for CPO from various stud-
C18:3 (linolenic) 0.0–0.6 0.1–0.6 0.1–0.5 ies is possibly related to the initial quality of the oil palm fruits
from which the oil was extracted, as well as the heaping period
of the fruits.14
Changes in FFA content As specified by MPOA, the maximum FFA content for CPO is
The level of oil deterioration is best expressed by the FFA content. 5%.5 Meanwhile, PORAM specifies that the maximum FFA con-
The changes of FFA content for CPO, RBDPO, RBDPOo and RBDPS tents for RBDPO, RBDPOo and RBDPS are 0.1%, 0.1% and 0.2%,
evaluated in the present study are presented in Table 5. There respectively.5 It is important to note that the FFA contents for CPO,

CPO RBDPO
44.4 44.2 UCL
UCL

44.0
44.1
C16:0 (%)
C16:0 (%)

43.8
43.8
43.6
LCL
LCL
43.5
43.4

0 1 2 3 4 5 6 7 8 9 10 0 1 2 3 4 5 6 7 8 9 10
Storage period (month) Storage period (month)

39.9 RBDPOo RBDPS


59.0
UCL UCL
39.6

58.5
C16:0 (%)

C16:0 (%)

39.3

58.0
39.0 LCL
LCL

38.7 57.5

0 1 2 3 4 5 6 7 8 9 10 0 1 2 3 4 5 6 7 8 9 10
Storage period (month) Storage period (month)

Figure 4. Control chart of palmitic acid (C16:0) composition stability for CPO, RBDPO, RBDPOo and RBDPS (UCL: upper control limit at +3𝜎, LCL: lower
3358

control limit at –3𝜎).

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CPO 40.4 RBDPO


40.4 UCL UCL
40.2

40.0

C18:1 (%)
40.0
C18:1 (%)

39.8
39.6

LCL 39.6 LCL


39.2
39.4

0 1 2 3 4 5 6 7 8 9 10 0 1 2 3 4 5 6 7 8 9 10
Storage period (month) Storage period (month)

44.4
RBDPOo RBDPS
29.5
UCL UCL
44.0
C18:1 (%)

C18:1 (%)

29.0
43.6

43.2 LCL LCL


28.5

42.8
0 1 2 3 4 5 6 7 8 9 10 0 1 2 3 4 5 6 7 8 9 10
Storage period (month) Storage period (month)

Figure 5. Control chart of oleic acid (C18:1) composition stability for CPO, RBDPO, RBDPOo and RBDPS (UCL: upper control limit at +3𝜎, LCL: lower control
limit at –3𝜎).

RBDPO, RBDPOo and RBDPS in the present study were still well in the present study were lower (0.23 g 100 g –1 oil and 0.29 g
below the maximum limit as specified in the standard specifica- 100 g –1 oil, respectively) compared to previous studies, where
tions set by MPOA and PORAM. In addition, the palm oil products CPO and RBDPO were stored at room temperature and 60 ∘ C,12,14
can be used as control samples for FFA content determination in although comparable with RBDPOo stored at room temperature.12
the respective palm oil products, which agrees with the control It is suggested that the rate of oxidation of unsaturated fatty acids
charts shown in Fig. 2. was faster at a higher temperature.
According to Malaysian Standard MS 814, the allowable range
of IV for CPO is 50.1–54.9. Meanwhile, as indicated by PORAM
Changes in IV
specifications, the allowable range of IV for RBDPO is 50–55, the
In addition to the FFA content, the IV of oil sample also discloses minimum IV for RBDPOo is 56 and the maximum IV for RBDPS
the extent of oil deterioration. Table 6 shows the changes of IV for is 48. Compared to the standard specifications for the palm oil
palm oil products examined in the present study. The IV of CPO and products, it can be concluded that the quality of CPO, RBDPO,
RBDPS up to 10 months of storage changed significantly (P < 0.05), RBDPOo and RBDPS, in terms of IV tested in the present study, was
whereas there were no significant changes in the IV of RBDPO preserved during the storage period. Figure 3 shows the control
and RBDPOo (P > 0.05). There are different ranges and limits of IV charts of IV stability for the palm oil products. The IV does not
specified for the palm oil products.5 The lower IV for RBDPS was exceed the upper and lower control limits, thus allowing the use
a result of the higher saturated fatty acid content.32,33 Significant of CPO, RBDPO, RBDPOo and RBDPS as control samples for IV
changes in IV for CPO with respect to 4.17 g 100 g –1 oil have determination in the respective oils.
been reported previously after storage at room temperature for
3 months.14 Gan et al.12 reported significant changes (P < 0.05) in
IV for RBDPOo over 52 days. The changes of IV were 0.34 g 100 g –1 Changes in FAC
oil and 3.67 g 100 g –1 oil for RBDPOo stored at room temperature The changes in the saturated, monounsaturated and polyun-
3359

and 60 ∘ C, respectively. The changes of IV for CPO and RBDPOo saturated FAC of palm oils products over 10 months of storage

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10970010, 2018, 9, Downloaded from https://onlinelibrary.wiley.com/doi/10.1002/jsfa.8839 by Universite Du Quebec A Chicout, Wiley Online Library on [15/12/2022]. See the Terms and Conditions (https://onlinelibrary.wiley.com/terms-and-conditions) on Wiley Online Library for rules of use; OA articles are governed by the applicable Creative Commons License
www.soci.org NAS Ramli et al.

are presented in Table 7. The FAC for CPO exhibited a significant


change (P < 0.05) in the compositions of C14:0, C16:0, C16:1,
Table 9. Changes in SMP (∘ C) of CPO, RBDPO, RBDPOo and RBDPS
during storage C18:1 and C18:2, whereas there was no significant change in the
compositions of C18:0 and C18:3 (P > 0.05). The FAC for RBDPO,
Palm oil products RBDPOo and RBDPS demonstrated the same trend where the
Storage period compositions of C14:0, C16:0, C16:1, C18:0, C18:1, and C18:2 var-
(month) CPOa RBDPOa RBDPOoa RBDPSa ied significantly (P < 0.05), except for the composition of C18:3.
In a study by Gan et al.12 on the storage stability of RBDPOo, the
0 36.0 ± 0.00 37.2 ± 0.00 22.0 ± 0.07 51.4 ± 0.00 composition of linoleic acid decreased, whereas the composition
1 35.9 ± 0.14 37.2 ± 0.07 21.8 ± 0.00 51.4 ± 0.14 of palmitic acid increased over the storage period of 52 days at 28
2 36.0 ± 0.00 37.2 ± 0.00 22.0 ± 0.00 51.6 ± 0.07 and 60 ∘ C. The change in the compositions of unsaturated fatty
3 36.2 ± 0.00 37.0 ± 0.00 21.8 ± 0.00 51.4 ± 0.00 acids is mainly attributed to the oxidation products because the
4 36.2 ± 0.00 37.0 ± 0.00 22.4 ± 0.07 51.2 ± 0.00 double bonds are more susceptible to oxidation.9,12 The FAC of
5 36.2 ± 0.00 36.2 ± 0.00 22.2 ± 0.00 51.2 ± 0.00 palm oil products from different sources may vary significantly as
6 36.2 ± 0.00 37.4 ± 0.21 22.4 ± 0.00 51.6 ± 0.00 a result of several factors, such as the genetic variation, climate
7 37.2 ± 0.00 37.2 ± 0.00 22.5 ± 0.00 51.6 ± 0.00 and season conditions, and soil types.9,34
8 36.2 ± 0.00 37.2 ± 0.00 22.2 ± 0.07 51.4 ± 0.07 During the storage duration, the FAC of CPO, RBDPO, RBDPOo
9 37.2 ± 0.00 36.2 ± 0.00 22.2 ± 0.00 51.4 ± 0.00 and RBDPS was within the range of compositions set by the
10 36.8 ± 0.00 36.2 ± 0.00 22.0 ± 0.00 51.2 ± 0.00 Malaysian Standards: MS 814, MS 816 and MS 815 for palm oil, palm
a Significant change (P < 0.05). olein and palm stearin, respectively (Table 8). The specifications
include the FAC for the respective processed palm oils.6–8 The
control charts of major fatty acids in the palm oil products palmitic

38.4 CPO RBDPO


38.7
UCL
UCL
37.6
37.8
36.8
SMP ( C)

SMP ( C)
o

36.9
36.0

36.0
35.2 LCL
LCL

34.4 35.1

0 1 2 3 4 5 6 7 8 9 10 0 1 2 3 4 5 6 7 8 9 10
Storage period (month) Storage period (month)

23.2 RBDPOo RBDPS


UCL 52.0
UCL
22.8

22.4 51.6
SMP ( C)

SMP ( C)
o

22.0
51.2

21.6 LCL LCL

50.8
21.2

0 1 2 3 4 5 6 7 8 9 10 0 1 2 3 4 5 6 7 8 9 10
Storage period (month) Storage period (month)
3360

Figure 6. Control chart of SMP (∘ C) stability for CPO, RBDPO, RBDPOo and RBDPS. (UCL: upper control limit at +3𝜎, LCL: lower control limit at –3𝜎).

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acid and oleic acid are shown in Figs 4 and 5, respectively. The condition of 6 ± 2 ∘ C in the absence of light has preserved the
control charts certified the stability of CPO, RBDPO, RBDPOo and quality of palm oil products throughout the storage duration of
RBDPS throughout the storage period. Therefore, the palm oil 10 months.
products can be used as control samples for FAC analysis of the
respective oils, particularly palmitic and oleic acid compositions.
ACKNOWLEDGEMENTS
We acknowledge all of the analysts of Analytical Services Labora-
Changes in SMP tory of the Advanced Oleochemical Technology Division (AOTD),
The SMP of an oil sample depends on several factors, such as MPOB, for their technical assistance and services provided with
the chain length of fatty acids, the trans fatty acid content, the respect to the completion of the present study.
unsaturation ratio and the position of the fatty acids in the glycerol
backbone.35 In the present study, the SMP of the CPO, RBDPO, RBD-
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