Journal of Vocational Studies on Applied Research Vol.

5(1)2023:10-16, Salsabila and Broto

Optimization of Papaya Seed Oil Production Process

(Carica papaya L.) with Soxhlation Extraction Method using
Factorial Design
Salsabila* and R.TD. Wisnu Broto

Industrial Chemical Engineering Technology, Faculty of Vocational School, Diponegoro University

Jl. Prof. Soedharto, S.H., Tembalang, Semarang
*)
Corresponding author: [email protected]

Abstract – This study aims to optimize the extraction of papaya seed oil (Carica papaya L.) using a factorial design level 2. Papaya
seeds are a significant component of the fruit, comprising approximately 14.3% of the total fruit weight. These seeds contain about
25% vegetable oil, predominantly composed of unsaturated fatty acids, which have the potential to be processed into consumable
oil. The extraction method employed is Soxhlet extraction using a non-polar solvent, n-hexane. A factorial design level 23 was
utilized to determine the most influential process variables. The variables were considered to the ratio of papaya seed mass to
solvent volume (1:7 and 1:11), particle size (10 and 30 mesh), and extraction time (170 and 190 min). Optimization was conducted
using the quicker method calculation, where the determination of the largest effect and the largest main effect played a crucial
role. The analysis revealed that the ratio of papaya seed mass to solvent volume had the most significant main effect, with an effect
value of 0.1217. From the analysis, it was found that the 1:7 ratio produced the lowest level of Free Fatty Acids (FFA) in the oil,
at 0.5076%, which aligns with the Indonesian National Standard (SNI) requirement of 0.36-0.82% FFA content. Furthermore, an
analysis of density, viscosity, and moisture content was conducted on the 1:7 ratio. The test results showed that the 1:7 ratio
resulted in an oil density of 0.924 g/mL, moisture content of 0.07127%, and FFA content of 0.5076%. However, based on theoretical
knowledge, an increase in FFA content leads to a decrease in oil quality. Additionally, higher ratios corresponded to increased
moisture content and density. In conclusion, the papaya seed oil produced in this study complies with the Indonesian National
Standard (SNI, 01-3555-1998) regarding FFA content (0.36-0.82%), moisture content (maximum 0.15%), and density (0.924-0.929
g/mL).
Keywords: carica papaya L.; papaya seed oil; soxhlation extraction; factorial design
Received: January 30, 2023 Revised: June 06, 2023 Accepted: June 09, 2023

Doi: http://dx.doi.org/10.14710/jvsar.v5i1.17308
[How to cite this article: Salsabila and Broto, R.T.D.W. (2023). Optimization of Papaya Seed Oil Production Process (Carica papaya L.) with
Soxhletation Extraction Method using Factorial Design. Journal of Vocational Studies on Applied Research, 5(1), 10-16. doi:
http://dx.doi.org/10.14710/jvsar.v5i1.17308]

INTRODUCTION that it has the opportunity to be developed into raw

Papaya (Carica papaya L.) is a type of plant materials for both vegetable oil and alternative fuels
that is cultivated in the garden or yard (horticulture), (Azhari et al., 2020). On the other hand, papaya seeds
currently papaya is a plant that is quite widely contain fatty acids, most of which are unsaturated fatty
cultivated in Indonesia. The seed content in papaya acids that can produce vegetable oil for public
fruit is about 14.3% of the whole papaya fruit. Simply consumption.
put, papaya seeds can be utilized as a digestive Papaya seed oil is known to be yellow in color
medicine, skin, and as a source to obtain vegetable oil and contains 71.60% oleic acid. 15.13% palmitic acid;
with a certain fatty acid content (Wulandari, 2017). 7.68% linoleic acid; 3.81% citric acid and other fatty
In papaya seeds, when calculated by dry acids in relatively small or limited amounts. Besides
weight, papaya seeds contain ±25% oil. When containing fatty acids, papaya seeds also contain other
compared to sunflower seeds at 22.23% and soybeans chemical compounds such as phenols, alkaloids, and
at 19.63%, the oil content of papaya seeds is more so saponins (Andaka & Fajrah, 2020). Papaya seed oil is
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a type of vegetable oil. Vegetable oil is oil obtained Multikimia Raya. The equipment used included a
from the extraction process of extracts from various Soxhlet extraction apparatus, a distillation apparatus,
parts of plants. Based on its use, vegetable oil is a chopper, an oven, sieves (10 and 30 mesh),
divided into two groups, namely, vegetable oil used in Erlenmeyer flasks, an analytical balance, measuring
the food industry (edible oil) and in the non-food cylinders, volumetric pipettes, an electric heater,
industry (non-edible) (Andaka & Fajrah, 2020). clamps and stands, a magnetic stirrer, measuring
Currently, the utilization of papaya seeds is flasks, glass funnels, porcelain crucibles, a desiccator,
usually only discarded after the fruit is consumed. burettes, and filter paper.
Some researchers have previously conducted research Preparation Materials
on the utilization of papaya seeds as a source of The research procedure for the material
vegetable oil. Papaya seeds, which have a clear preparation phase in this study referred to a previous
membrane, if processed for oil will be very profitable. study conducted by Zamrodah (2018), following a
With the increasing demand for oil production, series of steps. The process started with washing the
especially in food oil as a substitute for petroleum papaya seeds thoroughly and drying them under
whose price is getting higher and higher, this is an sunlight for approximately 1 day. Subsequently, the
opportunity to increase papaya seed oil production. dried papaya seeds were further dried in an oven at a
Papaya seed oil has a great opportunity to be increased temperature of 100°C for 1 hour. Once the papaya
in volume, among others, by improving the production seeds were dried, they were crushed using a chopper
process system. Extraction processes that are usually and sieved through 10 and 30 mesh size screens. If
carried out conventionally have difficulties in there were still papaya seeds that did not meet the
determining operating conditions. As a result, oil yield 10/30 mesh size requirement, they were crushed again
and oil quality are low and it is difficult to produce using a chopper and sieved once more.
good quality oil in large quantities (Nofrin et al., Extract Papaya Seeds
2012). Therefore, an appropriate extraction method is The procedure for the Soxhlet extraction of
needed to produce good quantity and quality of papaya papaya seeds in this study referred to Zamrodah's
seed oil. research (2018). It began with the preparation of 35 gr
In this study, the method used was liquid of 10-mesh-sized papaya seeds. The dried papaya
extraction, which is considered one of the most seeds were then wrapped in filter paper and placed into
effective and commonly used methods. It involves the assembled Soxhlet apparatus. Next, 400 mL of n-
using a solvent that can directly contact the material hexane solvent was added to a three-necked flask. The
and operate continuously, ensuring the solvent used material was extracted for 170 min at a temperature of
for extraction is always pure. Additionally, the oil 70℃, corresponding to the specified variable. The
within the material can be reused. In the extraction extracted results were collected in an Erlenmeyer flask
process, commonly used solvents include n-hexane and further experiments were conducted for
and ethanol. However, previous research has subsequent variables.
demonstrated that n-hexane solvent can produce oil Table 1. Research Variables
with better quality and quantity. Generally, the Variable
Lowe Upper
selection of solvents is influenced by factors such as Limit (-) Limit (+)
high selectivity, boiling point, polarity, low toxicity, Ratio of papaya seed mass
1:7 1:11
insolubility in air, and inertness, preventing reactions to solvent volume
Particle Size 10 mesh 30 mesh
with other substances (Guenther, 1987).
Extraction Time 170 min 190 min
Therefore, it can be concluded that
qualitatively, papaya seed oil is better produced using
n-hexane solvent as it can yield good oil quality and a
large quantity. In this study, innovation was carried
out by optimizing the Soxhlet extraction of papaya
seed oil using a factorial design experiment with a
level 23 to determine the most influential process
variables, understand the interactions between
variables, and determine the optimal results in the
extraction process to obtain papaya seed oil.

RESEARCH METHOD
Materials and Tools
The materials used in this study were 280 gr of
Figure 1. Soxhlation Apparatus Tools
dried papaya seeds obtained from Banyumanik Market
and 4 liters of n-hexane solvent obtained from PT.

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Distillation the pycnometer until it reaches the mark. Let stand for
Separation of the solution is by distillation 30 min then clean the neck of the pycnometer with
method. Separation is done to produce a solution that filter paper and leave at room temperature. Then
is free of solvents. The purpose of this separation remove and weigh. Do the procedure with blank water
process is to obtain a purer sample to produce as well. Then to calculate the density:
vegetable oil. This distillation process refers to W1 -W0
Density (ρ)= (2)
Volume of Pycnometer
previous research, namely Zamrodah (2018) with the
stages of the process starting with assembling the Information
distillation device, putting the papaya seed oil that has W1 = Weight of pycnometer with sample (gr)
been extracted into a three-neck flask, then inserting a W0 = Empty pycnometer weight (gr)
vacuum pressure source into the channel before the Water Content
Erlenmeyer, heating at 70℃ for 1 hour, then Analysis of water content in papaya seed oil
distillation is stopped when there is no dripping by washing the porcelain cup using distilled water,
solvent. Weigh and measure the volume of the then drying the porcelain cup in the oven at 105°C for
resulting oil yield. ± 1 hour. After that, cool in a desiccator for 30 min,
then weigh and record the weight. Do the treatment on
the porcelain cup until you gain a constant weight.
Then, weigh 5 gr of sample in a porcelain cup and heat
it in an oven at 105°C for ± 1 hour. After that, re-cool
in a desiccator for 30 min and measure the porcelain
cup containing the sample until a constant weight is
obtained. Then calculate the water content with the
following formula:
w -w
Water Content = 0 1 x 100% (3)
w0
Information:
w0 = Weight of the cup with oil before it is in the oven
w1 = Weight of the cup with oil after it's been in the
oven
The quality requirement for maximum water content
of papaya seed oil is 0.15% w/w.
Figure 2. Set of Distillation Equipment Free Fatty Acid
Crude analysis of free acids in papaya seed
Viscosity oil can be done by preparing 0.1 N NaOH solution and
The way to measure and calculate viscosity is standardizing it. After that, measure 2-5 gr of sample
by using an Ostwald Viscometer, suction ball, into an Erlenmeyer and add 50 mL of 95% ethanol.
stopwatch, glass funnel and measuring cup. First, put Then, add 3-5 drops of phenolphthalein (PP) indicator
clean water into a measuring cup then put it into the and titrate with 0.1 N NaOH standard solution until the
Ostwald Viscometer while turning on the stopwatch color changes to pink. Note the volume of NaOH
then when the water reaches the limit mark turn off the titration results and finally, calculating the free fatty
stopwatch. Then do this for the papaya seed oil acid content in the sample using the following
produced. Finally, calculate the viscosity value with formula:
the following formula: V NaOH x N NaOH x 282
ɳ=
txρ
x ɳ0 (1) FFA Content = x 100%
t 0 x ρ0 Weight of Papaya Seed Oils
Information: (4)
ɳ = Papaya Seed Oil Viscosity (cP) Quality requirements for free fatty acids (FFA) of
ɳ0 = Water Viscosity (cP) papaya seed oil, namely 0.36-0.82% w/w.
t = Flow Time of Papaya Seed Oil (s)
t0 = Water Flow Time (s) RESULTS AND DISCUSSION
ρ = Density of Papaya Seed Oil (gram/mL) Design Experiment is one form of
ρ0 = Density of Water (gram/mL) experiment that can control all external variables that
Density can affect the course of the experiment. In the design
Density is calculated to determine the density experiment, each tested variable is determined at
of the papaya seed oil produced. To know the density, several values, and all possible combinations of
the first step is to clean the pycnometer by rinsing it variables are tried. This research uses a factorial
with acetone and diethyl ether. Dry the empty design method 23, where each variable is taken at only
pycnometer and weigh its mass. Put the sample into 2 levels, and 3 variables are changed, namely the mass
ratio to the solvent (1:7 and 1:11), the particle size of

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the material (10 and 30 mesh), and the extraction time quality of papaya seed oil produced will be compared
(170 and 190 min). Therefore, 8 treatments are with the Indonesian National Standard (SNI) 01-3555-
obtained, and their effects will be analyzed. The use of 1998 and previous research conducted by
symbols (+) and (-) is used to indicate the upper and Cahyaningtyas et al. (2017).
lower limits of each variable in each experiment. The

Table 2. Data on Papaya Seed Oil Extraction Results (Factorial Design Level 23)

Variables
Interaction FFA Water
Run Changed Yields Density Viscosity
Content Content
Q S R TS TR SR TSR
1 - - - + + + - 39.57 0.927 2.58 0.564 0.056
2 + - - - - + + 57.40 0.924 3.75 0.6768 0.045
3 - + - - + - + 49.51 0.929 1.81 0.564 0.069
4 + + - + - - - 48.26 0.924 5.10 0.6768 0.044
5 - - + + - - + 41.63 0.928 4.24 0.7332 0.046
6 + - + - + - - 59.11 0.925 2.90 0.7332 0.053
7 - + + - - + - 67.34 0.928 1.68 0.7896 0.059
8 + + + + + + + 43.17 0.928 2.18 0.7332 0.053

This experiment was conducted with 8 running, P (%) Effect

with each run having a different treatment. Table 2 7.14 -0.0703
shows that the FFA content of the oil produced has a
21.43 -0.0143
value that corresponds to the sign of the level of
process variables, namely the ratio of materials and 35.71 -0.0139
solvents where the large ratio or marked (+) has a high 50.00 0.0139
FFA content while the small ratio or marked (-) has a 64,29 0.0143
smaller FFA content than the large ratio. To optimize 78.57 0.0421
this research, it is necessary to know the most
92.86 0.1271
influential process variables in the research by means
of the quicker method, namely by taking into account
the main effect and interaction on the resulting FFA Table 4 shows the determination of the
content. The calculation results for the most influential influential variable at 0.1271 which indicates the most
variables are shown in tables 3 and 4 and figure 3. influential variable is the ratio of ingredients and
solvents.
Table 3. Main Effect and Interaction Calculation
Results for FFA Levels
Effect Amount
I1, T 0.0421
12, S 0.0143
I3, R 0.1217
I12, TS -0.0139
I13, TR -0.0703
I23, SR 0.0139 Figure 3. Normal Probability Plot for 23
I123, TSR -0.0143
In Figure 3 shows that X7 is the result of the
Table 3 shows that from the result of the three calculation of the effect of extraction time with a
variables studied, the ratio is the most influential percent probability of moving away from density.
variable in the process of oil extraction from dried From the results of this analysis, process optimization
papaya seeds. When viewed from the calculation of a was carried out by varying the ratio of materials and
faster method that produces the greatest amount of solvents (R) to determine the FFA content of papaya
influence. seed oil and tested for the best results and then
Table 4. Determination of Influential Variables compared with previous research by Cahyaningtyas et

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al. (2017), Wulandari (2017) and the Indonesian this study is the ratio of materials and solvents, so the
National Standard (SNI). optimization process uses the time variable (T) and
particle size (S) as fixed variables and the variable
Optimization of Papaya Seed Oil Extraction ratio of materials and solvents (R) as a change’s
From the analysis of the table above, it can be variable. The results of the optimization carried out
concluded that the most influential process variable in can be seen in table 5.

Table 5. Optimization Results of Papaya Seed Oil Extraction

Ratio of Material to Seed Size
Extraction Time (Minute) FFA content (%)
Solvent (g/g) ( mesh )
1:7 0.5076
1:8 0.564
1:9 20 180 0.6204
1:10 0.6768
1:11 0.6204

Table 5 shows that the bigger the ratio, the was fully extracted. Moving forward, the best research
higher the FFA content. However, based on theory, the result was obtained from the 1:7 material ratio, which
higher the FFA content, the lower the oil quality. We had the lowest FFA content of 0.5076%. This result
can see this in the optimization graph of papaya seed will be further analyzed for density, viscosity, and
oil extraction in figure 4. water content and then compared with previous
research by Cahyaningtyas et al. (2017), Wulandari
(2017) and the Indonesian National Standard (SNI).
Analysis of Papaya Seed Oil Extraction Results
Analysis of papaya seed oil extraction results
will be tested based on SNI standards for papaya seed
oil as vegetable oil which includes density, moisture
content and FFA content. This analysis is carried out
on the optimization results that have the lowest FFA
content, because the lower the FFA content, the higher
the quality of papaya seed oil.
Figure 4. Graph of Optimization of Papaya Seed
Oil Extraction Results

Based on the FFA (Free Fatty Acid) content

of the papaya seed oil produced, it can be observed that
the higher the ratio of material to solvent, the higher
the resulting FFA content. This can be seen in Table 5
and the graph in Figure 4, where the 1:10 material ratio
shows the highest FFA content, which is 0.6768, under
the optimum operating conditions of 20 mesh seed size
and 180 min of extraction time. This is because using
a larger amount of solvent on the dry papaya seeds will
yield a higher yield and can affect the FFA value, as Figure 5. Samples of Papaya Seed Oil
shown in the graph above, where a higher material-to- Density
solvent ratio corresponds to a higher FFA content. Density is a parameter used to determine the
Increasing the volume of solvent used enhances its components contained in oil. The more components
ability to extract the oil contained in the papaya seeds. contained in the oil, the higher the weight fraction.
Additionally, a larger volume of solvent also prolongs This means that the specific gravity of the oil will be
the extraction time between the material and solvent. greater. This specific gravity test is useful for
Thus, it can be concluded that an increasing material determining oil purity. From the observation of the
ratio leads to a higher FFA value, as evident in Table specific gravity of oil extracted from dried papaya
5 and Figure 4, except for the fifth experiment where seeds, it showed in table 6 with the research oil, oil
a decrease in FFA occurred as the oil in the sample

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from previous research and SNI papaya seed oil as a Table 8. Results of Oil-Free Fatty Acid Test from
comparison. Papaya Seed Extract as a comparison.
Table 6. Density Result of Papaya Seed Extract Oil Oil
Soxhlation SNI
Oil Results Results of
Testing Extracted Papaya
of Previous SNI Previous
Soxhletation Oil Seed Oil
Testing Research Papaya Research
Extracted Oil
Seed Oil Free
Fatty
Acids 0.36-
Density 0.924-0.929 0.5076 0.3762
0.924 0.910 (FFA) 0.82
(%
Based on table 6, it can be concluded that the w/w)
specific gravity value produced is 0.924 which meets Free fatty acid testing is an important
the requirements, namely in accordance with SNI, parameter for determining oil quality. The amount of
which is between 0.924-0.929 % and also based on the free fatty acids in the oil is indicated by the acid
research of Cahyaningtyas, et al. (2017) which is close number value. A high acid number indicates that the
to the specific gravity value of 0.910 gr/mL. free fatty acids contained in vegetable oil are also high
Water Content so that the quality of the oil will be lower, this is
The results of the observation of the moisture because the free fatty acids produced due to hydrolysis
content of the oil extracted from dried papaya seeds can reduce oil quality. Free fatty acids can increase
can be seen in table 7 with the research oil, the oil from due to repeated heating even at a constant temperature,
previous research and SNI papaya seed oil as a when viewed in table 8 the oil from the results of this
comparison. Moisture content in oil is one of the study is in accordance with SNI standards where the
parameters that determine the quality of oil. Where, resulting fatty acid content is 0.5076, in research
the higher the water content, the lower the quality of conducted by Wulandari (2017) produced FFA levels
the oil because water is one of the catalysts for of 0.3762 and from both studies the papaya seed oil
hydrolysis in oil. We can see in table 7 that the water produced is in accordance with SNI which is between
content of the research results is in accordance with 0.36 - 0.82.
the maximum limit of the SNI standard for papaya
seed oil and in previous research conducted by
Cahyaningtyas, et al. (2017) produced high water
content and exceeded the SNI value limit of 1.06%. In
this study, the water content can be influenced by the
amount of heating carried out starting from the
extraction process to the distillation process. However,
this can make the oil easily damaged and the water
content in the sample is carried away and can also
cause the water content to decrease. This is in
accordance with the theory of Swern (1982) that a Figure 6. Titration Results of Papaya Seed Oil
material with high water content will produce oil with for Determination of FFA Levels
high water content as well, so it will be easily The results of FFA content in this study were
hydrolyzed. This is also the same as that expressed by carried out under operating conditions with an
Winarno (1988), the higher the temperature and the extraction time of 180 min, a distillation time of 1 hour
longer the heating, the faster the evaporation will with a particle size of 20 mesh and a ratio of material
occur, so the water in the material will be lower. and solvent 1: 7, namely 400 ml of solvent and 35 gr
Table 7. Results of Water Content from Papaya Seed of dried papaya seed material.
Extract
CONCLUSION
Soxhlation
Oil Results SNI From the research results, data processing was
Testing of Previous Papaya carried out using a factorial design 23 and then
Extracted Oil
Research Seed Oil optimization was performed. The optimization was
Water done using the quicker method calculation, where the
max.
Content 0.07127 1.06
0.15 determination of the largest effect and the largest main
(%)
effect were determining factors. The analysis results
Free Fatty Acid
showed that the variable of papaya seed mass to
The results of the observation of free fatty acids
solvent volume ratio is an influential process variable
contained in papaya seed oil extracted are shown in
with the largest main effect, with an effect value of
table 8 with the research oil and SNI papaya seed oil
0.1217.

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Based on these results, additional optimization Cahyaningtyas, R., Soetjipto, H., & Riyanto, C. A.,
was conducted by varying the ratio to 1:7, 1:8, 1:9, (2017), The Effect of Purification on the Quality of
1:10, and 1:11. From this analysis, it was found that Papaya Seed Oil (Carica papaya L.) in Terms of
the 1:7 ratio variable resulted in oil with the lowest Physicochemical Properties, Proceedings of the 8th
Free Fatty Acid (FFA) content, which is 0.5076%, in SNST Year 2017, pp. 49–54.
accordance with the SNI (0.36-0.82) standard.
Furthermore, from the 1:7 ratio variable, density, Guenther., (1987), Essential Oils, In Volume 1,
viscosity, and water content analysis were conducted. Jakarta: UI Press.
The test results showed that the 1:7 ratio produced oil
with a density of 0.924 g/mL, water content of Nofrin Susilowati and Rosi Primaswari., (2012),
0.07127%, and FFA content of 0.5076%. Extraction of Candlenut Oil using Soxhlet Extraction
The research results indicated that as the ratio Method, Surakarta: Universitas Sebelas Maret.
of papaya seed mass to solvent volume increased, the
FFA content tended to increase. However, according SNI 01-3555-1998., (1998), Indonesian National
to theory, an increase in FFA content will decrease the Standard for Oil and Fat Testing.
oil quality. Additionally, higher ratios resulted in
higher water content and density. In conclusion, the Winarno, F.G., (1988), Food Chemistry and Nutrition,
papaya seed oil produced in this research meets the Third Edition, Publisher: PT. Gramedia, Jakarta.
SNI (01-3555-1998) standard with FFA content (0.36-
0.82), water content (maximum 0.15), and density Wulandari, R. H., (2017), Papaya Seed Oil Extraction
(0.924-0.929). with Variation of Solvent-to-Substrate Ratio and
Extraction Time.
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Zamrodah, Y., (2018), The Effect of Mass Ratio to
Andaka, G., & Fajrah, D. I., (2020), Extraction of Solvent and Temperature on the Yield of Oil from
Papaya Seed Oil using n-Hexane Solvent, Jurusan Papaya Seed Extraction (Carica papaya L.), 15(2), pp
Teknik Kimia, pp. 14–15. 1–23.

Azhari, Nilva Mutia, I., (2020), Oil Extraction Process

from Papaya Seeds (Carica Papaya) using n-Hexane
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