Pulp Oil Characterization
Pulp Oil Characterization
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Physico-chemical and quality characterization of pulp oil from two varieties of
pili (Canarium ovatum Engl.) from Bicol, Philippines
1,2
Tugay, M.M.D.R., 1Mopera, L.E., 3Esguerra, E.B. and 1*Castillo-Israel, K.A.T.
1
Institute of Food Science and Technology, College of Agriculture and Food Science, University of the
Philippines Los Baños, College, Laguna, 4031
2
College of Industrial Technology, Catanduanes State University, Calatagan, Virac, Catanduanes, 4800
3
Postharvest Horticulture Training and Research Center, College of Agriculture and Food Science,
University of the Philippines Los Baños, College, Laguna, 4031
Article history:
Abstract
Received: 1 May 2020
Received in revised form: 3
June 2020
This study aimed to characterize and compare pili (Canarium ovatum Engl.) pulp oil from
Accepted: 8 June 2020 two different varieties of pili fruits in Bicol, Philippines namely M. Orolfo and Orbase
Available Online: 29 July varieties for possible utilization into oil-based products. The effects of varietal differences
2020 in pili fruits on physical, chemical and quality characteristics of its pulp oil were
Keywords:
determined. These two oils were also compared with control oils, commercially available
Pili pulp oil, coconut oil and extra virgin olive oil. Pili pulp oil from M. Orolfo had dark color while
M. Orolfo variety, Orbase had color close to extra virgin olive oil. The two varieties did not significantly
Orbase variety, differ from each other in terms of refractive index, moisture and volatile matters, acid
Fatty acid profile,
Coconut oil, value, iodine value, saponification number and percent unsaponifiable matter but
Extra virgin olive oil significantly differed from coconut oil and extra virgin olive oil. On the other hand, the
two varieties significantly differed from each other in terms of peroxide value, Vitamin A
DOI:
https://doi.org/10.26656/fr.2017.4(6).203
and α-tocopherol contents. In terms of fatty acid profile, high amounts of palmitic acid
were determined in both pili varieties (19-25%) compared with coconut oil (6.34%). Oleic
acid in Orbase was 71.5% while M. Orolfo had 58.1%, which are comparable with extra
virgin olive oil (77.9%). Pili pulp oils from M. Orolfo and Orbase can be utilized into oil-
based products because its chemical and quality characteristics are within the standard.
Both can be stored for a longer period of time and healthier in terms of fatty acid
composition and natural antioxidant content.
Pili fruit is the most important nut-producing species Pham and Dumandan (2015), reported that it has
and an indigenous fruit in the Philippines belonging to dark green color and the major fatty acids present in it
family Burseraceae. It is commonly known as a nut but are palmitic (23.96%), palmitoleic (4.66%), stearic
is actually a drupe that is egg-shaped to oblong-shaped (2.64%), oleic (60.93%) and linoleic (6.63%). They also
that weighs from 15.7 to 45.7 grams. Its pulp contains reported that the lipid molecular species present in the
73% moisture and is about 64.5% of the weight of the unsaponifiable matter of the said oil are carotenoids
fruit. It contains a relatively high amount of fat, 33.6% (141.79 mg/100 g oil), tocopherols (92.44 mg/100 g oil)
based on the dry weight basis per 100 grams (Coronel, and sterols (1,009.61 mg/100 g oil).
1996).
On the other hand, Coronel (1996), described PPO
Pili pulp oil (PPO) is a newly discovered source of differently as clear oil with greenish yellow color
vegetable oil in Bicol, Philippines that is now slowly containing 56.7% oleic glycerides, 13.5% linoleic
making its way into the oil industry. It is very similar to glycerides and 29.3% saturated fatty acids.
olive oil in its chemical and nutritional properties;
however, it contains more beta-carotene and carotenoids Llenaresas (1989) extracted oil from fruit pulp of
that make it more nutritious than olive oil (Asuncion, two pili varieties (Mabunga and Tree #2) and
2006). It is an inexpensive option to olive oil since its characterized them in terms of specific gravity, refractive
index, saponification value, iodine number, hydroxyl
*Corresponding author. eISSN: 2550-2166 / © 2020 The Authors. Published by Rynnye Lyan Resources
Email: kcisrael@up.edu.ph
1938 Tugay et al. / Food Research 4 (6) (2020) 1937 - 1946
value and amount of unsaponifiable matter. Results show extraction in Figure 1 using 1:3 w/w of pulp to water
that pili pulp oil have a specific gravity of 0.9001-0.993, ratio.
a refractive index of 1.4520-1.4625, a saponification
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matter, acid value, peroxide value, Vitamin A and has a C* value that is significantly higher than that of
Vitamin E content were determined according to AOAC refined coconut oil.
methods (2016).
It is also shown in Table 1 that all of the oil samples
2.4 Experimental design have negative a* value and positive b* values. This
This study employed a complete randomized design means that the hue value of all these samples is within
(CRD). Each treatment was triplicated while each of the green (-a*) and yellow (+b*) zone. This implies the
analysis for each treatment was conducted in two trials. presence of carotenoid and chlorophyll pigments in the
oil samples. Gandul-Roxas et al. (2016) and Minguez-
2.5 Statistical treatment of the data Mosquera et al. (1990) reported that carotenoids and
chlorophyll are mainly responsible for the color of virgin
In a completely randomized design, Analysis of olive oils. Mounts (1981) also reported the presence of
Variance (ANOVA), utilizing STAR software 2.0.1.2014
chlorophyll and a more prevalent and most important
system, was used to determine if significant difference provitamins pigments in soybean oil, β-carotene. The
among mean scores exists and LSD was used to locate
said author also reported that the latter pigment is
the differences among means. Q-test was used to responsible for the red color of palm oil when present in
determine the outlier.
higher concentration. Sahari et al. (2004) also attributed
to the presence of carotenoids in the intensely yellow
3. Results and discussion color of tea seed oil. Moyano et al. (2008) determined
3.1 Physical characteristics the relationship of color of virgin olive oils with their
chlorophyll and carotenoid indices. Pearson coefficients
Physical characteristics of different types of oil are (r*), revealed that that the best correlations are between
shown in Table 1. As shown, physical characteristics, in the carotenoid index and the C* (r* = 0.801) values and
terms of color, specific gravity and refractive index, of b* (r* = 0.802) values. When compared with PPO,
different types of oil vary among each other, except for however, this high positive correlation is not evident. It
the L* values of extra virgin olive and PPO from M. can be observed in Table 4 that pulp oil from M. Orolfo
Orolfo, and refractive indices of the two PPO samples. variety has higher carotenoid (Vitamin A) content than
that from Orbase variety but based on Table 1, the
Varietal differences in pili fruits affect its pulp oil
former has lower C* and b* values than the latter. This
color in terms of lightness (L*), chroma (C*) and hue
indicates how other pigments, aside from carotenoid,
angle (oH). When compared to that from Orbase variety,
affect the C* and a* values in PPO samples. Figure 2
PPO from M. Orolfo variety has lower L* value, C*
shows the actual appearance of the PPO and other oils.
value and oH value. This implies that the latter has a
Darkest color was obtained from M. Orolfo while Orbase
darker and less intense color than that from Orbase
was almost similar in appearance to extra virgin olive oil.
variety. PPO from M. Orolfo variety has an L* value that
Meanwhile, Gandul-Roxas and Minguez-Mosquera
is not significantly different from that of extra virgin
(1996) reported that aside from variety, ripening degree
olive oil but significantly lower than that of refined
of fruit affects the chlorophyll and carotenoid pigments
coconut oil. It has a C* value that is significantly lower
present in nine varieties of virgin olive oils from main
than that of extra virgin olive oil but significantly higher
Spanish producing regions. They further reported that
than that of refined coconut oil. Its oH value is
pheophytin (44-58%) was the predominant pigment in all
significantly higher than that of extra virgin olive oil but
of the oils studied, followed by lutein (18-38%) and β-
significantly lower than that of refined coconut oil.
carotene (6-17%). Psomiadou and Tsimidou (2001) also
On the other hand, PPO from Orbase variety has an reported that pheophytin a was the main pigments in all
Table 1. Physical characteristics of different types of oil
Physical Characteristics
Types of Oil Color Specific Refractive
L* a* b* C* o
H Gravity index at 25oC
Refined coconut oil 78.87a -1.38b 14.18d 14.30d 95.47a 0.9158a 1.4551c
Extra virgin olive oil 66.63c -0.42a 70.63b 70.60b 90.35d 0.9102d 1.4674a
Pili pulp oil (M. Orolfo variety) 66.13c -1.68c 41.33c 41.38c 92.37c 0.9115b 1.4663b
Pili pulp oil (Orbase variety) 73.53b -5.17d 71.87a 72.07a 94.12b 0.9110c 1.4663b
Means followed by the same letter in a column are not significantly different from each other by LSD at α=0.05
eISSN: 2550-2166 © 2020 The Authors. Published by Rynnye Lyan Resources
1940 Tugay et al. / Food Research 4 (6) (2020) 1937 - 1946
of 52 samples of virgin olive oils from various regions of unsaturation of fatty acid, molecular weight and degree
Greece. of conjugation (Ibeto et al., 2012). The higher the
molecular weight of oil and length and degree of
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oil oil (M. orolfo variety) (Orbase variety)
Caproic (C6) 0.543 ND ND ND
Caprylic(C8) 6.65 ND 0.046 ND
Capric (C10) 5.2 ND ND ND
Lauric (C12) 46.9 0.092 0.127 0.078
Myristic (C14) 19.9 0.025 0.183 0.132
Myristoleic (C14:1) ND ND ND ND
Palmitic (C16) 9.67 10.5 25.6 19.4
Palmitoleic (C16:1) ND 0.96 5.61 2.76
Stearic (C18) 3.13 3.6 1.22 1.74
Oleic (C18:1) 6.34 77.9 58.1 71.5
Linoleic (C18:2) 1.61 5.81 7.8 3.96
Linolenic (C18:3) 0.027 0.552 1.23 0.349
Erucic (C22:1) ND 0.7 0.039 0.019
Legend: ND = None Detected
for a longer period since it is less prone to rancidity. oxygen.
The iodine value of pili pulp oil (M. Orolfo variety) Findings of Sahari et al. (2004) on the characteristics
is lower but very close to the values reported by of tea seed oil in comparison to olive oil are different
Llenaresas (1989). On the other hand, iodine value of pili from this study. The iodine value of tea seed oil was
pulp oil from Orbase variety lies in between the values significantly higher than olive oil, though the
obtained by Llenaresas (1989) and Pham and Dumandan saponification value of the two mentioned oils was
(2015). The former reported a value ranging from 70.2- similar to each other.
70.3 while the latter reported a value of 74.57. This
variation can be attributed to varying methods of oil Unsaponifiable matters are hydrophobic components
extraction and differences in variety among pili fruits. that are stable towards bases and do not volatilize at
100oC like sterols, hydrocarbons, alcohols, mineral oils,
Saponification number is the number of mg of KOH carotenoids and the like (Baltes, 1964). Percent
needed to neutralize and saponify the free and esterified unsaponifiable matter in pili pulp oil samples is
organic acids, respectively in one gram of fat or oils significantly higher than refined coconut oil but
(Baltes, 1964). It indirectly accounts the average significantly lower than extra virgin olive oil (Table 2).
molecular weight of the triglycerides of fat and oil The lower amount of unsaponifiable matter obtained
(Bockisch, 1998). Saponification number of different from refined coconut oil is attributed to the refinement
types of oil is shown in Table 2. Pili pulp oil samples process undergone by this oil. Bleaching, as part of oil
have significantly lower saponification number than refinement processes, removes a wide range of different
extra virgin olive oil and refined coconut oil. This impurities like pigments and some oxidation products.
indicates that there are more triglycerides, which consist Originally it was only used to reduce the oil color but
of fatty acids with longer carbon chain, present in pili nowadays, this step is done to get rid of or convert
pulp oil samples than that from the other two oils. When detrimental by-products to safe ones (Zschau, 2001). It
compared with other studies, saponification numbers of usually improved the quality of oil with respect to color,
pili pulp oil samples are higher than that reported by oxidative stability and initial and aged flavor (Mounts,
Pham and Dumandan (2015) which is equivalent to 178 1981). Moreover, lower amount of unsaponifiable
mg KOH/g and are within, though not equal to the range matters in pili pulp oil than in olive oil implies higher
of values (167-437 mg KOH/g) obtained by Llenaresas purity of the former than the latter.
(1989) from pili pulp oil extracted from different
varieties of pili fruits by different solvents. This implies The amount of unsaponifiable matter obtained from
that the method of oil extraction affects the fatty acid pili pulp oil samples (Table 2) is way lower than that
composition and as well as saponification number of oil. obtained by Pham and Dumandan (2015) and Llenaresas
Moreover, Llenaresas (1989) pointed out also that aside (1989). The former reported a mean value equivalent to
from extracting solvents, the extent of oxidation or 1.69% while the latter reported values ranging from
rancidity of oil also affects saponification value of pili 1.12% to 1.88% of unsaponifiable matters in pili pulp oil
pulp oil as carboxylic acids are produced when double samples while for the samples is 0.4783% - 0.5283%.
bonds present in fatty acids of oils are attacked by This result is attributed to the solvent used in the
isolation of unsaponifiable matters. For this study,
hexane is used as extracting solvent in the determination Llenaresas (1989) reported a value from 69.4-80.6 for
of unsaponifiable matters while the other mentioned the percentage of oleic acid from different pulp oil
researchers use diethyl ether. Solvents that are samples from different varieties by different solvents.
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matters, % KOH/g fat peroxide/kg sample content, I.U. content, mg/kg
Refined coconut oil 0.0367b 0.27c 0.70d 41.22d 93.59a
Extra virgin olive oil 0.0400b 0.75a 10.38c 165.73b 2.76b
Pili pulp oil (M. Orolfo variety) 0.1000a 0.48b 13.50b 278.36a 125.85a
Pili pulp oil (Orbase variety) 0.0833a 0.43b 14.58a 123.00c 2.45b
Means followed by the same letter in a column are not significantly different from each other by LSD at α=0.05
moisture and volatile matter content of both of the pili Refined coconut oil sample obtained the lowest
pulp oil samples are within the maximum level of 0.2% peroxide value. According to Zschau (2001), bleaching
(Codex Alimentarius Commission, 1999). This implies removes products of oxidation. Also, refined coconut oil
that both of the pili pulp oil samples are in good quality is composed mostly of saturated fatty acid (Table 3)
and that the method used for its extraction is effective. unlike pili pulp oil samples and extra virgin olive oil.
Saturated fatty acids are less prone to oxidation than
Moisture is an important quality parameter for oils unsaturated ones (Sanders, 2003).
because it is one of the reactants in oil hydrolysis. Oil
hydrolysis yields free fatty acids which cause hydrolytic Akinoso et al. (2010) conducted a study on the effect
rancidity. Refined coconut oil in Table 4 has the lowest of moisture on the peroxide value of unrefined sesame
acid value because it has the lowest moisture content and oil. Results revealed that peroxide value increased with
because almost all of the non-fat components had been increasing moisture content. The same result was found
removed during refinement. However, pili pulp oil in this study. It is shown in Table 4 that moisture content
samples which have higher moisture content than extra of two pili pulp oil samples (with higher peroxide
virgin olive oil have lower acid value than the latter. values) is significantly higher than that of refined
Another factor which could affect acid value is the coconut oil and extra virgin olive oil.
method of extraction. Virgin oils are obtained by
pressing and application of heat while cold press oils are In terms of peroxide value, the Codex Standard for
obtained by pressing only. Aside from its reactants and refined coconut oil is up to 10 milliequivalents of active
enzymes, oil requires heat to hydrolyze. Thus, the oxygen per kilogram oil (Codex Alimentarius
application of heat during extraction causes the acid Commission, 2001a), for virgin olive oil, it is up to 20
value of the extra virgin oil sample to increase. Also, milliequivalents of active oxygen per kilogram (Codex
pressing of olive oils is not continuous, that filter mats Alimentarius Commission, 2001b), and for other oils not
could easily become contaminated which leads to the covered by other individual standards, it is up to 15
introduction of fermentation and oxidative defects into milliequivalents of active oxygen per kilogram oil
oils (Vossen, 2007). (Codex Alimentarius Commission, 1999). Therefore, it
can be implied that all of the four oil samples are still in
In terms of acid value, the Codex Standard for good quality.
refined coconut oil is up to 0.6 mg KOH/gram oil
(Codex Alimentarius Commission, 2001a), for virgin When the two pili pulp oil samples are compared, it
olive oil, it is up to 6.6 mg KOH/gram oil (Codex can be observed that the oil sample from M. Orolfo
Alimentarius Commission, 2001b), and for other oils not variety has a lower peroxide value than the other. This
covered by individual standards, it is up to 4.0 mg KOH/ can be explained by the higher amount of unsaponifiable
gram oil (Codex Alimentarius Commission, 1999). matters (Table 2) in M. Orolfo variety compared to the
Therefore, it can be implied that all of the four oil Orbase variety. Important natural antioxidants present in
samples are in good quality. oil like Vitamin A and Vitamin E are unsaponifiable. It
is shown in Table 4 that Vitamin A and Vitamin E
Peroxide value is one of the most important components of M. Orolfo are significantly higher than
properties for determining the level of fat deterioration. Orbase variety. Antioxidants help to reduce oxidation in
It shows the molar equivalent of oxygen, bound as oils. In fact, due to the high content of antioxidant, oils
peroxide, which is present in one kilogram fat (Baltes, with high initial peroxide value may have unpredictably
1964). longer shelf-life (Tsimidou et al., 2003). Thus, it can be
implied that M. Orolfo variety is less prone to oxidation
All of the four oil samples significantly differ among than oil from Orbase variety because of the higher
each other in terms of peroxide value (Table 4). Orbase amount of natural antioxidant (Vitamin A and E) it
fruit variety has the highest peroxide value, followed by contains. Sahari et al. (2004) also attributed to the
M. Orolfo variety and then by extra virgin olive oil. presence of carotenoids and antioxidant activity of tea
seed oil. Kamal-Eldin (2006) reported that the oxidative Helyes et al. (2012) reported that carotenoid content and
stability of vegetable oils is determined by fatty acid composition of tomato fruits were significantly affected
composition and presence of antioxidants, which are by varietal factors and water supply. Kotikova et al.
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generally tocopherols and other non-saponifiable (2007) found that carotenoid content in potato tubers was
components. Based on this finding, it is recommended significantly affected by maturity, year of cultivation and
that further study should be made to determine the effect variety.
of fatty acid composition and antioxidant content of pili
pulp oil from different varieties of pili fruits on its shelf- M. Orolfo variety has the highest α-tocopherol
life measured in terms of peroxide value. content that is not significantly different from that of
refined coconut oil. Presence of α-tocopherol in refined
Important antioxidants in oils, Vitamin A and E (as α coconut oil could mean that it is extracted from coconut
-tocopherol), are shown in Table 4. It can be observed meat with its testa. This claim is proven by Dia (2005).
from Table 4 that M. Orolfo variety has the highest In order to prove that α-tocopherol is present in coconut
Vitamin A content, followed by extra virgin olive oil, testa and not in coconut endosperm, the said author
Orbase variety and refined coconut oil, respectively. subjected both coconut testa and coconut milk to
Vitamin A present in refined coconut oil comes from Vitamin E analysis. Results of this investigation revealed
fortification done by the manufacturer. Its label declares that the former contains 732 µg tocopherol while the
that it contains around 61 I.U. of Vitamin A per gram oil. latter did not contain any.
However, a mean value of 41.22 I.U. of Vitamin A per
gram oil has been obtained from the analysis. On the other hand, both Orbase variety and extra
virgin olive oil have a significantly lower content of α-
The varying Vitamin A content between two pili tocopherol than the two other oils. The varying α-
pulp oil samples may be due to varietal differences in pili tocopherol content between two pili pulp oil samples
fruits. Oil from Orbase variety has significantly lower may be due to differences in pili fruit variety. Aside from
Vitamin A content than extra virgin olive oil while that variety, Aguilera (2005) reported that the tocopherol
one from M. Orolfo variety is significantly higher than content of virgin olive oil is affected by environmental
extra virgin olive oil. conditions. The said author reported that the tocopherol
content of virgin olive oil is lower when its fruit sources
The value of Vitamin A from two pili pulp oil were grown in higher altitude. Values of α-tocopherol
samples are way lower than that reported by Pham and content in two pili pulp oil samples are far lower than
Dumandan (2015). These authors reported a value of that reported by Pham and Dumandan (2015) which is
1417.9 µg of carotenoids or 1181.58 I.U. of Vitamin A 924 µg α-tocopherol per gram of pili pulp oil. Possible
per gram of pili pulp oil. This may be due to the reasons for this are different method used in the analysis
difference in the method used in the determination of the of the said component, method of oil extraction, varietal
said component, varietal differences of pili fruits and differences of pili fruits used in the study and sample
method of oil extraction. This study utilized the hexane storage time. Rastrelli et al. (2002) reported a 20% and
distillation method to determine the amount of 92% decrease in α-tocopherol content of olive oil after 2
unsaponifiable matters, wherein samples were refluxed months and 12 months, respectively of storage in the
for almost two hours. The refluxing process may have dark.
degraded some of the carotenoids in oil. Destruction of
carotenoids in crude palm oil increased with both
temperature and duration of exposure to heat (Fabien, et 4. Conclusion
al., 2014). Onyewu et al. (1986) heated 10 g β-carotene Characteristics of pili pulp oil samples from two
o
in glycerol at 210 C for 4 hrs, 1 hr, 15 mins, and 5 mins varieties of pili (M. Orolfo and Orbase) were determined
and results showed that at 210oC, degradation of β- for possible utilization into oil-based products. Physical
carotene was almost complete after 4 hrs and most of the characteristics of pulp oil samples from two different
nonvolatile products were viscous and yellow-brownish varieties of pili fruits vary from each other and from
in color. Less degradation was observed at shorter times commercially available oil samples, except for L* values
(1 hr, 15 mins, and 5 mins). Aside from variety, other of extra virgin olive and PPO from M. Orolfo. Chemical
factors that affect carotenoid content in plant food are characteristics of two pili pulp oil samples do not
genotype, season, geographic location, climate, stage of significantly vary from each other but both significantly
maturity and growing conditions (Kocher et al., 2014). vary from commercially available oil samples, except for
Aherne et al. (2009) reported that differences in type and refractive indices of the two PPO samples. Quality
geographical locations of tomato significantly affect its characteristics of two pili pulp oil samples significantly
carotenoid content and bioaccessibility. Meanwhile, vary from commercially available oil samples. There is
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