Extraction of Essential Oil from Neem Seed by Using Soxhlet Extraction Methods

International Journal of Advanced Engineering, Management and Science (IJAEMS) [Vol-3, Issue-6, Jun- 2017]
https://dx.doi.org/10.24001/ijaems.3.6.5 ISSN: 2454-1311
www.ijaems.com Page | 646
Extraction of Essential Oil from Neem Seed by
Using Soxhlet Extraction Methods
Bereket Tesfaye1
, Tilahu Tefera1,2*
Department of Chemical Engineering, Dire Dawa Institute of Technology, Dire Dawa, Ethiopia
Abstract— Extraction of essential neem oil from neem seed
was carried by soxhelt extraction method using different
organic solvents and parameters. Physico-chemical
property of the extracted oil was also determined by using
classical wet chemical method. Result revealed that, soxhlet
extraction using hexane has 40.35%; using ethanol-hexane
mixture of 60:40% volume proportion has 43.71%, using
ethanol 42.65% and using methanol 42.89%. For all
solvent type particle size has 355μm, extraction time 1hr up
to 3hrs and applied constant and varies temperatures .At
smaller extraction time, hexane produced oil yield greater
than from ethanol and methanol. Actually, ethanol not
produced oil at one hour extraction time. Thus, by effective
determination of factors like particle sizes, solvent type,
temperature, and time it is possible to investigate the result
on the quality and quantity of neem oil. Surprisingly,
mixtures of Ethanol and Hexane gave admirable results.
Predominantly, ethanol-hexane mixtures of 60:40, and
40:60% (volume proportions) gave better oil yields of 44%,
and 41.2% respectively than that of hexane (40.35%) at 3
hours of process time.
Keywords— Neem oil, Particle size, Soxhlet extraction,
Solvent type.
I. INTRODUCTION
Neem (Azadirachta indica A. Juss) is one of the very few
trees known in the Indian sub-continent. This tree is
belonged to Meliceae family and grows rapidly in the tropic
and semi-tropic climate. It is also observed that this tree
could survive in very dry and arid conditions. Neem seed is
a part of neem tree which has high concentration of oil.
Neem oil is widely used as insecticides, lubricant, drugs for
variety of diseases such as diabetes and tuberculosis. This
oil could also prolong leather goods when it is applied on
them. There are several methods to obtain neem oil from the
seeds like mechanical pressing, supercritical fluid
extraction, and solvent extraction (Puri, 1999).
Neem Oil is a vegetable oil gotten from the fruits, leaves
and seeds of neem tree. The tree is a member of the
Mahogany family, with generic name Azadirachta Indica A.
Juss, it is an evergreen tree which is endemic to the Indian
subcontinent and has been introduced to many other areas in
the tropics. It has also been found to thrive in the semi
tropics, arid and semi-arid climates in some countries
including Nigeria where it is known as Dongoyaro, meaning
―tall boy. The main reason behind the popularity of the
neem oil is that it is used to treat few of the most common
problems that the people face. The neem tree (Azadrichta
indica) is among the fastest-growing trees, it attains a height
of about 12-13 feet or 3.7- 3.96 meter and is a drought
resistant tree (Bankole, 1997, Lalea et al. 1999).
Neem oil is generally light to dark brown in color. It has a
bitter taste and an offensive odor similar to the combined
odors of garlic and peanut. It comprises mainly of
triglycerides (esters formed from a molecule of glycerol and
three molecules of fatty acids), and is very rich in
azadirachtin- the key component acting as insect repellent,
anti-feedant, anti-fungal and anti-viral, among others, it is
perhaps the most important commercial product of neem for
organic farming and medicines (Adeeko &Ajibola,1990,
Mongkhol et al. 2004). Also, it is being increasingly used in
manufacturing a large number of skin products: body soaps,
body lotions, and beauty care facial packs in combination
with other natural ingredients (Liaum et al., 2008).
The use of solvents and sohxlet extraction process for the
extraction of neem oil is generally preferred choice. This is
due to very high oil yield and less turbid oil obtained than
from mechanical pressing. Due to the relatively low
operating cost compared to supercritical extraction. The
solvent hexane is the most commonly used, as well as
preferred choice in extraction of oils from seed, even in
neem oil solvent extraction. This is largely due to its
availability at a reasonable cost and its suitable functional
characteristics for oil extraction. Amongst such
characteristics is its high solvent power for triglycerides at
fairly low temperatures, non-reactivity with oil and oil
miscella, as well as with equipment (Liaum et al., 2008).
The objective of present study was used soxhlet extraction
method and some selected organic solvent to extract
essential oil from neem seed. The effects of parameter such

as temperature, time and particle size were studied. As the
solvents, we used ethanol, hexane, methanol and ethanol-
hexane mixtures.
II. MATERIALS AND METHODS
2.1. Materials
Neem seed used for the study was obtained from Dire Dawa
city. Dry oven was used for drying neem seed. Analytical
balance was used for weighed neem powder. Sieve was
used for separate fine particles from neem powder. Filter
paper was used for filtration process. Heater Mantle was
used for heating the solution during soxhlet extraction time.
Soxhlet chamber was used for extraction process. Conical
flasks and 100 mL volumetric flasks were used for
measuring and solution preparation. Burette, beakers and
pipette were used for carry titration process.
2.2. Chemicals (Reagent)
N-hexane, Methanol, Toluene, Ethanol and mixtures of
ethanol and hexane were used for extraction of oil from
need powdered. Alcoholic potassium hydroxide (KOH),
hydrochloric acid (HCl) and phenolphthalein indicator were
used for determination of saponification value.
2.3. Size reduction and sieve analysis of neem seeds
Neem kernel was crushed in KIKA-WERKE GMBH mill
with sieve size 2mm. The sample was sieved using vibrated
shaker with set of sieves sizes arranged in descending order
1mm, 710μm and 355μm .This is because to investigate the
effect of particles size on yield and quantity of the oil.
Therefore, using 355μm sieve is more effective and gives
greater amount of oil than the else.
2.4. Preparation of neem seed powder
Neem seed used for the study was obtained from Dire Dawa
city. Prior to use, the neem seeds were repeatedly washed
to remove dirt and other impurities material, and
subsequently dried in oven at 50°C until it attained constant
moisture content. Then, neem seeds were pulverized to get
the particle sizes of 355μm and prepared for extraction
process (Maria et al. 2008).
2.5. Method for extraction of neem oil
100 g of neem powder was placed into the thimble and
placed in the soxhlet chamber .500 ml of selected solvents
were placed in a round bottom flask and assembled for
soxhlet extractor then the distillation process was begun.
After completed the extraction process, the solvent and
extractor were placed on water bath to evaporate the
solvent. Then extracted neem oil was weighed by using the
following equation:
% oil yield
=
𝑊1−𝑊2
𝑊1
𝑋100…………………………..…………..(1)
Where: W1=Sample weight initially placed in the thimble
and W2= sample weight after dried in the oven (Natarajan et
al. 2003).
Acid value and saponification value were determined
according to the methods prescribed by AOAC (1984).
Specific gravity and pH were determined according to the
method of AOAC (1990).
III. RESULT AND DISCUSSION
Extraction of essential neem oil from neem seed was carried
by soxhlet extraction method using some selected organic
solvents and parameters. The effects of parameter such as
temperature, time and particle size were studied. As the
solvents, we used ethanol, hexane, methanol and ethanol-
hexane mixtures. Results were tabulated in the following
tables. Three replicate measurements were carried for each
parameters (N=3).
Table.1: show result of Soxhlet extraction using hexane with particle size 355μm and at constant temperature.
Trial Temperature(0
c ) Time (min) Oil yield (%)
1 70 60 37.02
2 70 120 39.43
3 70 180 40.35
Table.2: Show results of Soxhlet extraction using hexane with constant particle size (355μm) and varies temperature.
Trials Temperature (0c) Oil yield (%)
1 70 41.08
2 78 41.89
3 86 42.41

Table.3: show results of Soxhlet extraction using Ethanol-Hexane mixtures of 60:40% of volume proportion at constant
temperature
Trials Temperature(0
C) Time (min) Oil yield (%)
1 70 60 25.06
2 70 120 37.87
3 70 180 43.71
Table.4: Show results of Soxhlet extraction using Methanol with particle size 355μm and at constant temperature
Trials Temperature(0c) Time(min) Oil yield (%)
1 70 60 25.38
2 70 120 39.05
3 70 180 42.89
Table.5: Show results of Soxhlet extraction using Ethanol with particle size 355μm and at constant temperature
Trials Temperature (0c) Time (min) Oil yield (%)
1 70 60 -
2 70 120 40.54
3 70 180 42.65
Table.6: Show result of Soxhlet extraction using ethanol- hexane mixture 40:60% of volume proportion with particle size 355 μm
and constant temperature
Trials Temperature (0c) Time(min) Oil yield (%)
1 70 60 26.23
2 70 120 36.42
3 70 180 40.21
3.1. Physico-chemical properties of extracted neem oil
In the present study the physico-chemical properties of the extracted essential neem oil was investigated by using classical wet
chemical method. Results were presented in table-7.
solvents Acid value (mg
KOH/g)
Sap.Value (mg
KOH/g)
Specific gravity PH
Ethanol 17.35 195.56 0.85 5.38
Hexane 18.05 202.04 0.90 6.04
60:40% hex/eth 14.46 194.48 0.90 4.86
40:60% hex/eth 17.11 198.36 0.89 4.98
3.2. Effect of Temperature
Results obtained from the analysis showed that an increase
in temperature generally favors an increase in oil yield. This
phenomenon is due to the fact that oils are generally more
soluble at elevated temperatures (Sen et al. 1992). At higher
temperatures, the viscosity of the solvent is reduced while
the diffusivity, as well as evaporation rate is increased. This
increases the contact time between the solvent and the oil
bearing material (Ayoola et al., 2014). From the above
result, soxhlet extraction using hexane at constant
temperature (700
C) which has 40.35% and temperatures at
860
C has 42.41%. At same temperature, the results showed
that ethanol -hexane mixture of 60:40 % volume
proportions were better extraction liquid for higher yields of
oil attained.
3.3. Effect of Time
Oil yield obtained (expressed in percent) was extraction
time reliant. In general, the oil yield increased with increase
in extraction time and there was no considerable increase
after 3hour (Ayoola et al., 2014). Results shown from table-
1, soxhlet extraction using hexane the time changed from
1hr to 3hrs the oil yield rose 37.02% to 40.35%. In case of
ethanol- hexane mixture of 60:40% and 40:60% volume

proportions the oil yield rapidly rose 25.06% to 43.71% and
26.23% to 40.21% respectively. The same condition was
appeared in methanol. Ethanol produced no oil at one hour
of extraction time. As the extraction time increased,
mixtures of 60% ethanol 40% hexane gave the maximum
oil yield. These show that the combination of solvents
favors higher oil yield compare to using these solvents
separately.
Results of physco-chemical properties of extracted neem oil
point out that, extraction using hexane solvent reported high
acid value (18mgKOH/g) and saponification value (202.04
mgKOH/g) than the other solvents. Acid value indicates
the amount of free fatty acids presents in an oil. Acid value
is good indicator of oil degradation caused by hydrolysis.
Also higher extraction temperature increased the acid value
because the extraction temperature influenced the
hydrolysis of neem oil (Adeeko & Ajibola , 1990).
Saponification value indicates the average molecular weight
of triglycerides in the oil (Fasina &Ajibola, 1989, Ayoola et
al., 2014). And also an increase in temperature increased the
saponification value because higher temperature caused
lipid to breakdown therefore reduced the average molecular
weight of the oil (Fasina &Ajibola, 1989, Adeeko &
Ajibola , 1990).
IV. CONCLUSION
This project work was intended to investigate the influence
of different factors such as Particle sizes, solvent type,
temperature, and time on the quantity of neem oil.
Variability of these operating conditions is the pre-dominant
factors for the quantity of the oil.
There are different methods for essential oil extraction from
neem seed. In the present study, soxhlet extraction method
was selected. In this extraction method the maximum oil
yield obtained was 43.71% by using ethanol-hexane
60:40% solvent with particle size of 355μm and for three
hours extraction time. The experimental quantitative
difference in the quantity of the oil was due to particle size
and extraction time variability.
Determination of the appropriate size of the particles and
optimal time for the recommended particle size needs to
have a consideration to get the maximum amount of the
required product. Volume proportions of ethanol-hexane
mixtures (60:40 and 40:60% respectively) served as
efficient solvent alternatives to the use of hexane in
essential neem oil extraction.
ACKNOWLEDGEMENTS
The authors grateful to Dire Dawa University Institute of
Technology Department of Chemical engineering, Ethiopia
for providing all kind of bear and encouragement to carry
out this thesis work.
CONFLICT OF INTEREST
The author(s) declare(s) that there is no conflict of interest
regarding the publication of this paper.”
REFERENCES
[1] Aalaa Elgasim Elshierh, Amina Bader Eldeen Edres,
Mohammed Elmokhtar Abd Elaziz (2014). Extraction
of Neem Oil from Neem Seeds.
[2] Adeeko K.A. and Ajibola O.O. (1990). Processing
Factors Affecting Yield and Quality of Mechanically
Expressed Groundnut Oil. Journal of Agricultural
Engineering. 45: 31-43.
[3] AOAC. Official methods of Analysis. 14th
edition,
Association of Official Analytical Chemists,
Washington, DC, (1984).
[4] AOAC. Official methods of Analysis. 15th
edition,
Association of Official Analytical chemists,
Washington, DC, (1990).
[5] Ayoola A.A., Efeovbokhan V.C., Bafuwa O.T. and
David O.T (2014). A Search for Alternative Solvent
To Hexane During Neem Oil Extraction International
Journal of Science and Technology Volume 4 No. 4,
ISSN 2224-3577
[6] Bankole, S.A. (1997). Effect of essential oils from two
Nigerian medicinal plants (Azadirachta indica and
Morinda lucida) on growth and aflatoxin B1
production in maize grain by a toxigenic Aspergillus
flavus, Letters in Applied Microbiology, Volume 24,
Issue 3, pages 190 –192
[7] Fasina O.O. and Ajibola O.O. (1989). Mechanical
Expression of Oil from Conophor Nut. Journal of
Agricultural Engineering. 44: 275-287.
[8] Khraisha Y.H. (2000). Retorting of Oil Shale
Followed By Solvent Extraction of Spent Shale:
Experiment and Kinetic Analysis. Journal of Energy
Sources. 22: 347-355.
[9] Lalea, N.E.S, Abdulrahmanb, H.T. (1999). Evaluation
of Neem (Azadirachta indica A. Juss) Seed Oil
Obtained by different Methods and Neem Powder for
the Management of Callosobruchus maculatus (F.)
(Coleoptera: Bruchidae) in Stored Cowpea, Journal of
Stored Products Research, Volume 35, Issue 2, Pages
135 –143.

[10]Liauw, M.Y., Natan, F.A., Widiyanti, P., Ikasari, D.,
Indraswati, N. and Soetaredj, F. (2008). Extraction of
Neem Oil (Azadirachta indica A. Juss) Using n-
Hexane and Ethanol: Studies of Oil Quality, Kinetic
and Thermodynamic. Journal of Engineering and
Applied Sciences.
[11]Maria Yuliana Liauw, F. A. Natan, P. Widiyanti, D.
Ikasari, N. Indraswati and F. E. Soetaredjo,
(2008). Extraction of neem oil (azadirachta indica a.
juss) using n-hexane and ethanol: ARPN Journal of
Engineering and Applied Science. 3, 2-4.
[12]Mongkhol khajornsilp D., Douglas S., Douglas P.L.,
Elkamel A., Teppaitoon W. and Pongamphai S.
(2004). Supercritical CO2 Extraction of Nimbin from
Neem Seeds-A Modeling Study. Journal of
Food Engineering. 71: 331-340.
[13]Natarajan, V., Venugopal, P.V., Menon, T. (2003).
Effect of Azadirachta Indica (neem) on the Growth
Pattern of Dermatophytes. Indian Journal of Medical
Microbiology. Volume : 21,Issue 2, page 98 -101.
[14]Puri H.S. (1999). Neem-The Divine Tree. Harwood
Academic Publishers, Amsterdam.

Extraction of Essential Oil from Neem Seed by Using Soxhlet Extraction Methods

More Related Content

What's hot (20)

Similar to Extraction of Essential Oil from Neem Seed by Using Soxhlet Extraction Methods (20)

Recently uploaded (20)

Extraction of Essential Oil from Neem Seed by Using Soxhlet Extraction Methods