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

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

www.ijaems.com Page | 646

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
as temperature, time and particle size were studied. As the to remove dirt and other impurities material, and
solvents, we used ethanol, hexane, methanol and ethanol- subsequently dried in oven at 50C until it attained constant
hexane mixtures. moisture content. Then, neem seeds were pulverized to get
the particle sizes of 355m and prepared for extraction
II. MATERIALS AND METHODS process (Maria et al. 2008).
2.1. Materials
Neem seed used for the study was obtained from Dire Dawa 2.5. Method for extraction of neem oil
city. Dry oven was used for drying neem seed. Analytical 100 g of neem powder was placed into the thimble and
balance was used for weighed neem powder. Sieve was placed in the soxhlet chamber .500 ml of selected solvents
used for separate fine particles from neem powder. Filter were placed in a round bottom flask and assembled for
paper was used for filtration process. Heater Mantle was soxhlet extractor then the distillation process was begun.
used for heating the solution during soxhlet extraction time. After completed the extraction process, the solvent and
Soxhlet chamber was used for extraction process. Conical extractor were placed on water bath to evaporate the
flasks and 100 mL volumetric flasks were used for solvent. Then extracted neem oil was weighed by using the
measuring and solution preparation. Burette, beakers and following equation:
pipette were used for carry titration process. % oil yield
12
= 100....(1)
1
2.2. Chemicals (Reagent)
Where: W1=Sample weight initially placed in the thimble
N-hexane, Methanol, Toluene, Ethanol and mixtures of
and W2= sample weight after dried in the oven (Natarajan et
ethanol and hexane were used for extraction of oil from
al. 2003).
need powdered. Alcoholic potassium hydroxide (KOH),
Acid value and saponification value were determined
hydrochloric acid (HCl) and phenolphthalein indicator were
according to the methods prescribed by AOAC (1984).
used for determination of saponification value.
Specific gravity and pH were determined according to the
method of AOAC (1990).
2.3. Size reduction and sieve analysis of neem seeds
Neem kernel was crushed in KIKA-WERKE GMBH mill
III. RESULT AND DISCUSSION
with sieve size 2mm. The sample was sieved using vibrated
Extraction of essential neem oil from neem seed was carried
shaker with set of sieves sizes arranged in descending order
by soxhlet extraction method using some selected organic
1mm, 710m and 355m .This is because to investigate the
solvents and parameters. The effects of parameter such as
effect of particles size on yield and quantity of the oil.
temperature, time and particle size were studied. As the
Therefore, using 355m sieve is more effective and gives
solvents, we used ethanol, hexane, methanol and ethanol-
greater amount of oil than the else.
hexane mixtures. Results were tabulated in the following
tables. Three replicate measurements were carried for each
2.4. Preparation of neem seed powder
parameters (N=3).
Neem seed used for the study was obtained from Dire Dawa
city. Prior to use, the neem seeds were repeatedly washed

Table.1: show result of Soxhlet extraction using hexane with particle size 355m and at constant temperature.
Trial Temperature(0c ) 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 (355m) and varies temperature.
Trials Temperature (0c) Oil yield (%)
1 70 41.08
2 78 41.89
3 86 42.41

www.ijaems.com Page | 647

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
Table.3: show results of Soxhlet extraction using Ethanol-Hexane mixtures of 60:40% of volume proportion at constant
temperature
Trials Temperature(0C) 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 355m 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 355m 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 m
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 Sap.Value (mg Specific gravity PH
KOH/g) KOH/g)
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 that ethanol -hexane mixture of 60:40 % volume

Results obtained from the analysis showed that an increase proportions were better extraction liquid for higher yields of
in temperature generally favors an increase in oil yield. This oil attained.
phenomenon is due to the fact that oils are generally more
soluble at elevated temperatures (Sen et al. 1992). At higher 3.3. Effect of Time
temperatures, the viscosity of the solvent is reduced while Oil yield obtained (expressed in percent) was extraction
the diffusivity, as well as evaporation rate is increased. This time reliant. In general, the oil yield increased with increase
increases the contact time between the solvent and the oil in extraction time and there was no considerable increase
bearing material (Ayoola et al., 2014). From the above after 3hour (Ayoola et al., 2014). Results shown from table-
result, soxhlet extraction using hexane at constant 1, soxhlet extraction using hexane the time changed from
temperature (700C) which has 40.35% and temperatures at 1hr to 3hrs the oil yield rose 37.02% to 40.35%. In case of
860C has 42.41%. At same temperature, the results showed ethanol- hexane mixture of 60:40% and 40:60% volume

www.ijaems.com Page | 648

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

www.ijaems.com Page | 649

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
[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.

www.ijaems.com Page | 650