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Extraction of Essential Oil from Orange Peel using Different Methods and Effect
of Solvents, Time, Temperature to Maximize Yield

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ISSN 2321 3361 © 2019 IJESC

Research Article Volume 9 Issue No.12

Extraction of Essential Oil from Orange Peel using Different Methods

and Effect of Solvents, Time, Temperature to Maximize Yield
TsegayeFekadu1, Tesfaye Seifu2, Abambagade Abera3
Department of Chemistry
College of Natural Sciences, Arba Minch University, Ethiopia

Abstract:
Presently, in Ethiopia orange peels are discarded as wastes after consumption of edible parts of orange fruits. To get the highest
quality and quantity of orange peel oil, it is necessary to know the suitable methods for drying and the appropriate form of the peel,
whether in the form of pieces, grated or powder. Essential oils are highly concentrated substances, which are extracted from fruit
peels, flowers, leaves, stems, roots and seeds. These oils are often used for their flavor and their therapeutic or odiferous properties, in
wide selection products such as foods, pharmaceuticals, medicines, perfumery industry and cosmetics. The main objectives of this
research is to extract essential oil from orange (citrus sinensis) peels by two methods: hydro distillation and solvent extraction, to
study the effect of extraction conditions (solvent type, extraction time, and temperature) on oil yield and compare the results of the
two methods, the resulting essential oil was analyzed its physical and chemical properties. From the results obtained, it was observed
that the orange peels could give the maximum yields of essential oil to be 3 % and 2 % when hydro distillation and solvent extraction
were employed, respectively, and that was an indication that the highest yield of essential oil was given by hydro distillation among
the methods considered. The physical and chemical properties values obtained from the characterization of the oil revealed that it
could be used in different process industries for production of other valuable products.

Key word: Essential oil, hydro distillation, effect of temperature.

I. INTRODUCTION (Fortunella,Eremocitrus, Clymendia, Poncirus, Microcitrus, and

Citrus), which are native to the tropical and sub-tropicalregions
Essential oils are used in a wide variety of consumer goods such of Asia, but the major commercial fruits belong togenus Citrus.
as detergents, soaps, toilet products, cosmetics, pharmaceuticals, The genus citrus includes several importantfruits such as
perfumes, confectionery food products, soft drinks, distilled oranges, mandarins, lime, lemons and grape fruits [4, 5]. The
alcoholic beverages (hard drinks) and insecticides. The world essential oil is present in the fruit’s peelin great quantities. The
production and consumption of essential oils and perfumes are citrus essential oil is a mixture ofvolatile compounds and mainly
increasing very fast. Production technology is an essential consists of monoterpene hydrocarbon [6, 7]. Essential oils are
element to improve the overall yield and quality of essential oil. mixtures of over a hundredcompounds that can be approximated
The traditional technologies pertaining to essential oil processing into three fractions:terpene hydrocarbons, oxygenated comp
are of great significance and are still being used in many parts of ounds and nonvolatilecompounds. The terpene fraction can
the globe. Water distillation, water and steam distillation, steam constitutefrom 50 to more than 95% of the oil [4]. Essential oil
distillation, cohobation, maceration and enfleurage are the most fromcitrus is a large type of natural flavours and fragrances
traditional and commonly used methods. Maceration is adaptable which is popularly used in food industries, daily chemical
when oil yield from distillation is poor. Distillation methods are products and health care field. The citrus species arepotential
good for powdered almonds, Rose petals and rose blossoms, sources of variable oil which might be utilizedfor edible and
whereas solvent extraction is suitable for expensive, delicate and other industrial purposes. Essential oils arebroadly used as
thermally unstable materials like jasmine, tuberose, and pharmaceutical components, in nutritionsupplements and for
hyacinth. Water distillation is the most favored method of cosmetic industry and aromatherapy [8]. The exact function of
production of citronella oil from plant material [1, 2]. Essential essential oils in a plant isunknown, it may be to attract insects
oils are generally derived from one or more plant parts, such as for pollination, or to repel harmful insects or it may be simply a
flowers (e.g. rose, jasmine, carnation, clove, mimosa, rosemary, metabolic intermediate [5]. Orange juice is one of the most
lavander), leaves (e.g. mint, Ocimum spp., lemongrass, jamrosa), widely-consumed beverages today in world. Approximately 50-
leaves and stems (e.g. geranium, patchouli, petitgrain, verbena, 60% of the processed fruits are transformed into citrus peel,
cinnamon), bark (e.g. cinnamon, cassia, canella), wood (e.g. which is composed of peels, seeds and membrane residues. With
cedar, sandal, pine), roots (e.g. angelica, sassafras, vetiver, the increase in production of processed fruit wastes generated is
saussurea, valerian), seeds (e.g fennel, coriander, caraway, dill, increasing enormously.Large amounts of these wastes pose the
nutmeg), fruits (bergamot, orange, lemon, juniper), rhizomes problem of disposal without causing environmental pollution.
(e.g. ginger, calamus, curcuma, orris) and gums or oleoresin These wastes can be effectively disposed by manufacturing
exudations (e.g. balsam of Peru, Myroxylon balsamum, storax, useful by products from them [9, 10]. Orange peel oil has been
myrrh, benzoin) [3]. Citrus fruits belong to six genera chosen for extraction because it provides a great potential for

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further commercial form. Peel of citrus fruit has numerous Materials and methods
glands that contain oil that is typically recovered as major by Study Area
product. Each citrus fruit has its own characteristic set of Arba Minch town is one of the emerging towns of Ethiopia
compounds that comprise the oil and that are responsible for its which is located in SNNPR state of Ethiopia. The name Arba
flavor and aroma to products such as carbonated drinks, ice- Minch was derived from the “forty springs” which means a
creams, cakes, air-fresheners and perfumes. Recently developed collection of more than forty springs which are located in the
extraction methods like supercritical fluid extraction, microwave Arba Minch natural forest. It is found in Gamo zone and used as
assisted extraction and Sox let method has been used for oil a zonal capital town. It is located at about 454 km south of Addis
extraction, know a day they also use solvent extraction, water Ababa (capital city of Ethiopia). Astronomically Arba Minch is
distillation and steam distillation methods. The basic parameters located at 6°04′ North Latitude and 36°40′ East Longitude.
influencing the quality of an extract are the solvent used for Experimental Site
extraction, the manufacturing process (extraction technology) Extraction and Characterization of essential oil from orange peel
used with the type of equipment employed. The use of was carried out at Chemistry Research Laboratory, Arba Minch
appropriate extraction technology, plant material, manufacturing University.
equipment, extraction method and solvent and the adherence to Chemicals
good manufacturing practices certainly help to produce a good Analytical grade chemicals that were used in the study include
quality extract. In this research, solvent extraction, steam N-hexane, petroleum, methanol, acetone, hydrochloric acid,
distillation, and water distillation methods use to extract oil potassium hydroxide, nitric acid, sodium hydroxide, distilled
from orange peel and compare those terms of costing, yielding water, and phenolphthalein indicator.
and time and reproducing better natural aroma of orange Plant material:Orange peels were collected from Sikela market.
essential oil [11, 12]. Material/Instruments
All glassware’s used in the extraction of essential oil were
II. RESEARCH OBJECTIVES washed with dilute nitric acid and rinsed in distilled water, dried
in hot oven prior to use, to avoid any unwanted reaction during
General Objectives the extraction process. The materials/instruments used for this
To extracted essential oil from orange peel using different work were round bottom flask, Basket heater, thermometer,
methods and effect of solvents, time, temperature to maximize measuring cylinder, separating funnel, electronics balance,
yield grinder, Knife.
Specific Objectives Collection and identification of orange peel
 To extract essential oil from orange peel samples. Orange peel was collected from Sikela marketin Arba Minch,
 To determine the optimum time and temperature to Ethiopia. Orange peel was botanically identified using the
extract orange peel essential oil for the highest yield. standard morphological characteristic features.Orange peels
 To conduct the physicochemical characterization of were collected in plastic bags and transported to the laboratory
essential oil produced. of chemistry for extraction and characterization of oil.A sample
 To compare the best extraction methods depend on yield. of orange peel is shown in Figure 1

Figure.1. Orange Peels Sample

Preparation of orange peel powder sac present in them. After the orange peels were obtained, they
The collect sample of orange peels is cleaned and pith is were washed, cleaned with water and chopped, placed on
manually separated from the outer coloured part of the peels. blotting paper, spread out and dried under shade at room
That is because of the reason that the majority of the oil in oil temperature for 5 days. The shade dried orange peelswas grinded

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to give consistent and fine powder (Figure 2) using electrical labeled airtight container at ambient temperature and protected
grinder. The powdered orange peels was then stored in well from sunlight for further use.

Figure.2. prepared powder sample

Extraction of essential Oil by hydro Distillation added to cover the peels. The flask was connected to the still
Water or hydro distillation is one of the oldest and easiest column which was connected to the condenser. Heat is supplied
methods. The Distillation set up is arranged as shown in Figure 3 to the distillation unit by temperature controlled basket heater.
.It consists of distillation flask, Basket heater, horizontal The experiment is carried out at different Temperature and. time
condenser and a conical flask.About 150 g of the orange peel period. The distillate is collected in a conical flask. This distillate
powder was weighed using digital weighing balance and then has two layers, one dense layer and other less dense layer. This
transferred into a round bottom flask with large amount of water is then separated using a separating funnel [.13]

Figure.3. Hydro distillation set-up

Solvent Extraction: recorded. The weighed sample was dropped in the Soxhlet
extractorapparatus as shown inFigure-4. The extraction was
Essential oil extraction from orange peels was done using the carried out using normal hexane, methanol, and petroleum as the
Soxhlet method. The orange peels were pureed using a blender. extraction solvent. In the Soxhlet apparatus, the solvent in the
A round bottom flask was washed, oven dried, and cooled in a round bottom flask was heated from the heating mantle to
desiccator. To carry out this procedure, the ground peels were become evaporated and got condensed down through the sample
sieved using a standard 0.6 mm particle size sieve. A dried mass where it was able to extract the oil along, thereby, giving a
of 10 g of the orange peel powder was weighed, and the weight mixture of oil and solvent, which was later separated [13].

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 Figure.4. Soxhlet apparatus set- up
Separation of essential oil Since water is denser than oil, it is collected at the bottom of the
When the mixture is poured into a Separatory funnel, the oil and funnel.After this the funnel tap is opened and the liquid at the
water separate into two distinct layers as shown in Figure 5. bottom of the funnel is transferred into a container.

Figure.5. Schematic representation of the separating funnel

The oil and solvent (n- hexane, methanol….) mixture was separated using rotary evaporator as shown in figure 6 and the separation
was carried out by principle of rotary evaporator.

Figure.6. Rotary evaporator

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Calculation of oil yield Chemical characteristics of extracted essential oil
The yield of the oil extracted using each of the two methods of Determination of saponification value of the essential oil
extraction was calculated using equation 1. Saponification value, being the weight of potassium hydroxide
Weight of oil extracted expressed in milligrams that is required to saponify 1 g of oil
% yield = x100Equation 1
Weight of sample used was also determined in this work. To carry out this, 2 g of the oil
was weighed into a 200-ml conical flask into to which 50 ml of
Characterization of the Essential Oil 0.5 M of KOH was added. Then followed by addition of 3 drops
The essential oil extracted from orange peels at the optimum of phenolphthalein indicator and it was titrated against 0.5 M
processing conditions (the highest yield) was characterized by HCl until pink color disappeared that observed during
determining the physicochemical properties. Outlined below are phenolphthalein indicator added to the mixture of oil sample and
the tests carried out on the oil. [13, 14]. KOH. This procedure was repeated without the oil and the titre
Physical characteristics of extracted essential oil value was determined from the blank value [13]. The
Sensory analysis of the essential oil saponification value was calculated using Equation 4.
Sensory analysis was carried out on the oil to determine its V2−V1
physical properties. This involved sense of sight, smell and Saponification value = x28.1Equation 4
w
touch. Where, V1 is the blank titrate value, V2 is the sample titrate value
Determination of solubility of the essential oil in water and W is the weight of the sample.
A few drops of the oil was added to a test tube containing little Determination of acid value of orange peel essential oil
amount of water. The test tube was stirred thoroughly with a To determine the acid value of the extracted oil, 2 g of the oil
stirring rod. Two separate phases were observed. The sample was weighed into a conical flask containing 50 ml of
insolubility of the oil in water was inferred from that operation. ethanol. Three drops of phenolphthalein indicator were added to
Determination of density of the oil the mixture. The resulting mixture was titrated against 0.1 M
The density of the oil extracted was determined by weighing an NaOH [13] and consistently shaken until a dark pink color was
empty beaker and recording its value. Thereafter, essential oil observed. The acid value was calculated using Equation 5. The
was poured into the beaker and the weight was taken. The volume of the 0.1 M NaOH was noted.
56.1x V x N
density of the oil was thus calculated using equation 2. Acidic value = Equation 5
Weight of oil sample weight of sample
Density = x100 Equation Determination of ester value of the oil
Volume of oil sample
2 Ester value, which is defined as the number of milligrams of
Determination of specific gravity of orange peel essential oil potassium hydroxide required to saponify the fatty acid esters in
All experiments were carried out in triplicates, and average one gram of the oil, was also determined for the oil extracted in
values taken. A clean and dry bottle was weighed using a this work. It was obtained as the difference between the
weighing balance. Distilled water was poured into the bottle and saponification value and the acid value of the oil [13] as given in
weighed. In the same manner, the same volume of oil was Equation 6.
poured into the same bottle and weighed. The specific gravity Ester value= saponification value- acid valueEquation 6
was calculated as the ratio of weight of oil to that of water [13]
as given in equation 3. III. RESULT AND DISCUSSION
Oil specific gravity =
Weight of particular volume of oil extract The effects of extraction temperature and extraction time on
x100Equation 3
Weight of equal volume of water essential oil yield from orange peels were investigated.

Table.1. Effect of temperature

Temperature(oC) Time (min) Solvent Oil extracted (mL) Percentage yield
value (%)
90 180 Water 2 1.33
100 180 Water 4.5 3

Table.2. Effect of Time

Time (min) Temperature(oC) Quantity of oil Percentage yield value (%)
Extracted (ml)

30 100 0.7 0.47

60 100 2.1 1.4
90 100 2.5 1.6
120 100 3.3 2.2
150 100 3.8 2.53
180 100 4.5 3

Volume of Essential Oil obtained from orange peel was different extraction, in the range of 90-100 oC for extraction temperature
for different temperatures and at a particular temperature for the and 30–180 min, the observed maximum essential oil yield was
different time of heating. From table-1 and 2 for the essential oil 2 ml at extraction temperature of 90 oC and extraction time of

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180 min. Similarly the observed maximum essential oil yield shown in Figure-7. It can be seen from the figure that at no oil
was 4.5 ml at extraction temperature of 100 oC and extraction was obtained from the extraction from the initial timeup till
time of 180 min.Increase in extraction temperature and time about 60 min. From the graph it was observed that volume of
leads to a corresponding increase in essential oil yield, the oil Essential Oil obtained from orange peels is almost increasing
will eventually break out of the peel matrix and thus be linearly with time of heating at a particular temperature (90 0C).
extracted. Hydro distillation extraction method of obtaining It was also observed from the figure 7 that the yield of oil
essential from orange peels was carried out at a temperature of obtained when the extraction time was 180 min was 2 ml/150 g
90oC in this work, and the results obtained from this were as orange peel powder.

2.5

2
Quantity of Oil (ml)

1.5

0.5

0
30 60 90 120 150 180
Time (min)

Figure.7. Water distillation extraction process at 90 oC.

Carrying out the same water distillation procedure of the and, even, the amount of oil given was observed to keep on
essential oil extraction at a temperature of 100o C gave the increasing with increase in extraction time. For this process,
results that are shown in Figure-8. From the results given in which was carried out at 100o C, the yield of oil obtained when
Figure-8, it was noticed that oil was produced by the extraction the extraction time was 180 min was obtained to be 4.5 ml / 150
at the temperature of 100o C from the initial time of the process, g peel

4.5

3.5
Quantity of Oil (ml)

2.5

1.5

0.5

0
30 60 90 120 150 180
Time (min)

Figure.8. Water distillation extraction process at 100 oC.

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Analyzing the results given in Figures 7 and 8, it can be seen that Solvent extraction
temperature is one of the factors affecting extraction process The effects of solvent type time on essential oil yield from
because the amount of oil obtained at the temperature of 90 o C orange peels were investigated.Solvent extraction method of
was found to be different from the amount given when the obtaining essential oil from orange peels was carried out using n-
extraction temperature was 100o C. It has also been observed that hexane, methanol, and petroleum ether solvent at temperature 60
the high temperature could favor extraction process because the and 80 degree Celsius for 3 hour in this work, and the results
oil given by the extraction process carried out at 100o C was obtained from this were as shown in table 3
found to be higher than that given when the temperature was set
to 90o C.
Table.3. Experimental data and response obtained from the solvent extraction process.
Solvent Weight of Volume of Temp Time Quantity of oil Percentage yield
peels (g) solvent (ml) (oc) (min) Extracted (ml) value (%)

N-Hexane 50 300 60 180 2.3 1.53

50 300 80 180 3 2
Methanol 50 300 60 180 1.5 1

50 300 80 180 2 1.33

Petroleum 50 300 60 180 1.2 0.8
Ether
50 300 60 180 1.8 1.2

As table 3 show high amount of essential oil from orange peel Characterization of the essential oil
was extracted using n-hexane, and methanol and petroleum ether
respectively. The results given in table 3 shows that the The extracted essential oil was analyzed to determine its
variations in the factors chosen as the independent variables of physical and chemical properties, and given in Tables 4, and 4
the process were having effects on the yield of oil obtained from are the results obtained from the analyses for the physical and
the extraction of orange peels. The change in solvent, time and the chemical properties respectively.
temperature was found to affect the quantity of oil extracted.
Physical characterization of extracted essential oil
As result show when the temperature of the experiment work
increase quantity of oil extracted also increase and also when the Moreover, the extracted essential oil was analyzed to determine
time of the experiment work increase quantity of oil extracted its physical properties, and given in Table 4 are the results
also increase. Therefore oil yield and time also oil yield and obtained from the analyses for the physical properties.
temperature are directly proportional to each other.

Table.4. Physical properties of essential oil from orange peel

As can be seen from the Table-4, the oil was obtained to have aromatic compounds. The extracted essential oil has a specific
virtually yellow colour with tangy smell, and it was observed to density less than 1 which implies that it is lighter than water and
be insoluble in water. As can be seen from the Table-4 the consequently will be insoluble in water. The density of the oil
specific gravity of the essential oil was 0.843. was estimated to be 0.86 g/cm3.This is in agreement with the
standard value of essential oil from orange peel waste.
The specific gravity determines the weight of the essential oil. It
is also important in determining the quality and purity of Chemical characterization of essential oil from orange peel
essential oil. Most of the essential oils have specific gravity
ranging from 0.696–1.88. Specific gravity values of oils are less The values obtained for the chemical properties of extracted
than 1 for most of the oils except few containing oxygenated essential oil are given in Table-5.

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 Table.5. Chemical properties of essential oil from orange peel

The acid value of the essential oil was 4.2 mg KOH/g. wastes increase. If the wastes are effectively managed to produce
Essential oils are concentrated and contain several volatile value-added products economic benefits along with reduced
aroma compounds which are majorly free fatty acids. Free fatty environmental problems can be achieved. Orange juice is one of
acids are considered as degrading in oils because they are the big juice sectors. From these sectors, large amount of wastes
responsible for oil rancidity. Oils with low acidity are especially orange peels are discarded. However, orange peel
considered as neutralized and safe for making skin care wastes can effectively be utilized for the economic production of
products as high acidity of oils may beharmful for skin [16]. value-added products such as pectin. Our results revealed that it
The low acid value of the extracted essential oil indicates that was possible to produce value-added products from the orange
the oil has excellent storage life. The saponification value of peel wastes such as essential oil.
the essential oil was 44.96 mg KOH/g. Saponification value is
an indicator of the average molecular weight and hence chain Acknowledgements
length. It is inversely proportional to the molecular weight of We would like to thank the Department of Chemistry, Arba
the oil [17]. High saponification values of oils are due to the Minch University, Ethiopia, for providing the laboratory
predominantly high proportion of shorter carbon chain lengths facilities and the necessary supports.
of fatty acids [18]. Low molecular weight (short to medium
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