Ajayi Adebayo Ebenezer... Research Project

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CHAPTER ONE

INTRODUCTION

1.1 Research background

Shea butter is a versatile plant fat extracted from kernels of shea nuts, seeds of shea trees
(Vitellaria paradoxa). Shea butter has long been used in sub-Saharan Africa for medicinal,
culinary, and other applications and serves as a cocoa butter equivalent in the manufacture of
chocolate as well as an ingredient in cosmetics[1].Shea butter is a slightly yellowish or ivory-
colored fat. It is widely used in cosmetics as a moisturizer, salve or lotion. Shea butter is
edible and is used in food preparation in Africa Occasionally the chocolate industry uses
Shea butter mixed with other oils, as a substitute for cocoa butter, although the taste is
different.Shea butter extract is a complex fat that contains, besides many nonsaponifiable
components (substances that cannot be fully converted into soap by treatment with alkali),
the following fatty acids:oleic acid (40-60%), stearic acid (20-50%), linoleic acid (3-11%),
palmitic acid (2-9%), linolenic acid(<1%) and arachidic acid(<1%).[2]
However, the main importance of the shea tree (Vitellaria paradoxa) is due to the
vegetablefat that can be extracted from the dried kernels which is traditionally utilised in
largequantities for cooking, as a moisturising cream, for illumination, for soap-making, as a
herbalmedicine, for fire-lighting and for waterproofing house. This vegetable fat is called
shean butter [3]. The raw or unrefined is the purest and most effective, as it is the most natural
andleast processed. The two most natural ways to extract the unrefined shea butter is by hand
oran expeller. This keeps all the vitamins, minerals and other natural properties of the
sheabutter intact, making it very beneficial.
Shea butter like most vegetable oils and fats consist of mixtures of triacylglycerols
whichconstitutes about 95% of its constituents and a non-triacylglygerol which contains
variableamounts of phospatides, free fatty acids, unsaponifiable matter, oxidation products
and otherimpurities. These impurities have an adverse effect on the quality of shea butter as
they havedifferent effects on the nutritional, functional and organoleptic properties of the
shea butter
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Consequently, traditional shea butter has to be purified (or refined) in order to mitigate these
components and its overall quality with the least damage to the triacylglygerol [4].
Considering countries like Malaysia who have attained an economic upliftment through
theplantation and processing of palm oil. Nigeria has a chance to boost her economy
bymaximally exploiting other of her resources apart from petroleum. One of these resources
is shea butter.For industrial processors, Shea has been relegated to a low cost substitute
product, but as withtrue Cinderella commodities, there is a glimmering interest from the high
value niche markets forgreater use of Shea. Currently, Shea is undergoing renewed demand
from the high valuecosmetics companies and for this market sector, the very fact that Shea
remains a wildernesscrop that it is produced naturally, that it has cultural and medicinal
qualities and is collected andprocessed by womens groups in remote rural areas, all combine
to create a fashionablemarketing scenario for high profile cosmetics products.

1.2 Problem statement
Traditionally, in West Africa, processi6f shea butter were practiced by the collectors of the
69shea nuts by persons using their own approach and methods. Local production of shea
butter revealed problems which include the inconsistent product and the difficulty to control
or procure consistent product due to the lack of quality control and the varied and degraded
quality shea butter. Shea butter, especially, undergoes hydrolytic and oxidative degradations
during the post-harvest processing and storage, which results in the shea butter characterized
by high values of free fatty acids and peroxide values. All these factors lead to inconsistency
of quality and limited shelf-life of shea butter. Hence this research work is necessary so as to
provide a mechanical way of extracting shea butter and to assess an increase in the quality of
shea butter produced.

1.3 Aims and objectives of the study
Consequently, the aim of this work is to develop a mechanical process to extract shea butter.
It is anticipated that the mechanized extraction process will lead to:
1. Improving the appearance and acceptability of shea butter by its users.
2. Reduced impurities which are usually formed during the traditional production.
3. The development an effective mechanized extraction process for shea butter that is
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efficient and can easily be implemented on a small or large scale.
The objective of this work includes;
1. Effect of Temperature of water added to paste
2. Effect of kneading Speed on shea butter yield
3. Effect of kneading time on shea butter yield.
4. Determination of the kneading speed in revolution per minutes.
5. Determination of some physio-chemical properties on the shea butter such as acid
value, saponification value and refractive index.
6. Determination of the composition of fatty acid in the shea butter

1.4 Method and Scope
The method that will be employed in this work is the use of food processor to knead the
shea paste for the extraction of shea butter. This method involves crushing and grinding of
shea nuts, the paste is mixed with water and then kneaded at specific speed and time. Water
is added subsequently, and fat is scooped from the surface of the kneaded paste, the fat is
then boiled, weighed and then analysed. The procedure is repeated at different speed,
temperature and time.
This work is limited to the extraction of shea butter found in Saki, Oyo State Nigeria. Also
other methods of extraction will not be considered due to the time and economic constraints
for this research.
1.5 Relevance of research to the society
The following will be the relevance of this research to the Nigerian society:
To generate employment opportunities for the Nigerian populace.
To increase foreign exchange generation of Nigeria through the exportation of shea butter
to foreign nations.
To serve as a catalyst for the development of a shea butter processing industry in Nigeria.
To serve as a reference material for other studies and advancements in the area of shea
butter extraction in Nigeria.

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CHAPTER TWO

LITERATURE REVIEW

2.1 The shea butter tree

The history of the Shea tree, Butyrospermum parkii, is well known and documented in the
Western world since the days of Mungo Park, the British explorer who first described the tree
from his journeys in West Africa in the 18th century. In the semi-arid sub-Saharan region the
Shea tree is a valuable asset, yielding edible oil for domestic use and products for cosmetic and
pharmaceutical uses. It is because of these unique healing properties that the Shea tree got its
name, the karite tree, which means the TREE OF LIFE [5, 6].
Vitellara paradoxa, the Shea butter tree, grows across a wide swathe of Sahelian Africa, from
Senegal to Ethiopia. Throughout, the Shea belt, the trees are highly valued by the local
communities not only for the economic and dietary value of the cooking oil, but also for the fruit
pulp, bark, roots and leaves, which are used in traditional medicines and for the wood and
charcoal, used for building and cooking. European explorers recorded the Shea tree as early as
1728 and first samples were collected by Mungo Park in 1796. It was some 30 years after Parks
expedition to West Africa, that the tree was classified as Vitellaria paradoxa by von Gaertner in
1807. In 1865, the West African tree was re-classified as Butyrospermum parkii, by Theodore
Kotschy, and the East African subspecies was classified as Butyrospermum nilotica[6].
In his journals, Park described the local trade in Shea products as a vibrant inland commercial
activity and since that time agricultural officers posted to Africa have made detailed notes of the
local trade in Shea nuts, butter, oil, cake and latex and also speculated on its export trade
potential. Along with many other oil crops, samples were tested for fuel and food products. By
the 1920s, a flourishing trade was developing between West Africa and Europe where the butter
was used in making vegetable margarine and candles. However, changing agricultural policies in
Europe and new product formulations led to a decline in demand for Shea and in many respects
Shea now falls into the Cinderella crop category.
Shea nut (SN) is known as Kandayi, Osisi and Emi among the Hausa, Igbo and Yoruba people of
Nigeria, respectively.Butyrospermum Paradoxum (shea butter tree) is locally abundant in the
middle belt areas (Benue, Kwara,Niger states and Abuja) where it is found growing wild [7]. Shea
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butter continues to be used and traded in the Sahel as a source of cooking oil but shea butter is no
longer a mainstream industrial product. Despite interest by Governments and FAO expert panels
to develop local industries on shea butter, no attempts have been made to domesticate the crop
and essentially shea butter remains a wild fruit that is seasonally gathered by the local
community. For industrial processors, shea butter has been relegated to a low cost substitute
product, but as with true Cinderella commodities, there is a glimmering interest from the high
value niche markets for greater use of Shea.
Currently, shea butter is undergoing renewed demand from the high value cosmetics companies
and for this market sector, the very fact that Shea remains a wilderness crop that it is produced
naturally, that it has cultural and medicinal qualities and is collected and processed by womens
groups in remote rural areas, all combine to create a fashionable marketing scenario for high
profile cosmetics products.
The shea tree is such a valuable tree and its various areas of utilization can be shown in the table
below.

Table 2.1: Utilization of the Shea tree [6]

Part of tree
(Vernacular)
Recorded use

Fruit

Eaten fresh or dried and stores for later use.
Also described as a famine food.

Seeds

Dried seeds used for oil production or sold
for immediate income

Oil

The oil is mainly used as edible oil, for
frying, as an addition to sauces or sold in
local markets as an important source of
income. Other uses include utilization in
many cultural ceremonies (wedding, birth,
naming of new babies, funeral,
rain, crop/soil fertility, divining the future
and ordination of local chiefs or priests) and
as a preparation for battle. The oil has also
been described as a traditional; moisturizer,
as an ointment for newborn babies, as a
lubricant of machinery and as an important
component of medicines for sprains, scabies
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or as an open wound dressing. The oil/fat can
also be used to produce traditional soap and
to protect wood or metal from corrosion.
Wood

The wood is used as charcoal or firewood
and the pools are frequently employed as the
roof or Y shaped poles in house
construction. The timber is also used for
local handicrafts (stools, pestles and mortars)
and as beehives. In addition, large tree boles
are used to build local canoes.

Whole tree

The whole tree is said to improve soil
fertility, provide shade and protect against
wind or soil erosion.

Leaves

Although rarely utilized, the leaves from this
tree species are used in funeral
ceremonies
Flowers

The flowers are used to flavour tobacco, as
a medicine to reduce chest pains and to cure
eye problems. They are also know to be
important in honey
production
Bark

Frequently used as a medicine for stomach
problems, specifically against
diarrhoea
Residue

The bi-product or residue from oil production
is commonly used as a termicide
for houses (to protect walls and poles) or
crops, burnt to repel mosquitoes and
the ashes from this product can be used to
produce local salt
Latex

The latex is used as a medicine to dress open
wounds, as a glue to seal pots or calabashes
and as an adhesive to trap animals or birds

Roots

The roots are utilized in the production of
traditional medicines.

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2.2 Overview of shea butter

2.2.1 Shea butter

Shea butter is the fat extracted from the kernels of Vitellaria paradoxa Gaertner
(Sapotaceae), which is also known as Butyrospermum parkii. The species is found across 19
countries across the African savanna zone from Senegal to Ethiopia. Shea butter contains
high levels of UV-B absorbing triterpene esters, including cinnamic acid, tocopherols
(vitamin A), and phytosterols. Shea butter does contain a high percentage of unsaponifiables,
such as phytosterols (campesterol, stigmasterol, beta-sitosterol , and alpha-spinosterol) and
triterpenes (cinnamic acid esters, alpha- and beta-amyrin, parkeol, buytospermol, and lupeol),
and hydrocarbons such as karitene [8,9] .Shea butter is not a recent discovery or
accomplishment. This all-natural product has been around for centuries. In fact, it is believed
that some of the early users of shea butter were such noted women as Cleopatra and the
Queen of Sheba. About 200 years ago, Europeans rediscovered shea butter. Now, shea butter
is made in 19 African countries.
Shea Butter is only found in the tropics of Africa. It is extracted from the nuts of the Shea-
Karite tree which begins to bear fruit after about 15 years; and can take up to 30 years to bear
a quality crop of nuts with a high content of irremovable fatty acid. It is this irremovable fatty
acid that gives Shea Butter its unique healing properties and makes it far superior to cocoa
butter and other vegetable butters. Traditionally, Shea Butter was extracted by people who
picked the nuts, cracked them, grilled them and pounded them. They were boiled in water for
hours until the Shea Butter rose to the surface. It was then scooped into gourds and left to
cool and set. Shea Butter is solid at room temperature although it quickly liquefies right
around body temperature. This Shea Butter is called unrefined Shea Butter or raw Shea
Butter. Since Shea Butter is an all natural product, it can vary widely in quality, appearance
and smell depending on where it is produced from and how it is refined or extracted.
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Figure 2.1 - Agricultural parkland, with shea trees

Figure 2.2 - Shea fruit

Figure 2.3 - Shea Nut
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Figure 2.4 - Shea Butter

2.2.2 Composition of shea butter
Native shea butter consists mainly of triglycerides and a large fraction of unsaponifiable
materials.The fatty acid composition of the triglycerides is dominated by oleic, stearic and
linoleic acids. The unsaponifiable fraction contains high amounts of cinnamic acid esters of
triterpene alcohols but also a smaller fraction of sterols. The most characteristic triterpene
alcohol of shea butter is butyrospermol but other important constituents are lupeol as well as
alpha- and beta-amyrin. Shea butter also contains tocopherols (Vitamin E) functioning as
antioxidants.

2.2.2.1 Free fatty acids
Shea butter is composed of five principal fatty acids: palmitic, stearic, oleic, linoleic, and
arachidic (Table 2.2) [8]. The fatty acid composition is dominated by stearic and oleic acids,
which together account for 85-90% of the fatty acids] .The relative proportions of these two fatty
acids produces differences in shea butter consistency. The high stearic acid content gives the
shea butter its solid consistency, while the percentage of oleic acid influences how soft or hard
the shea butter is.
The proportions of stearic and oleic acids in the shea kernels and butter differ across the
distribution range of the species. Ugandan shea butter has consistently high oleic acid content,
and is liquid at warm ambient temperatures. Ugandan shea butter fractionizes into liquid and
solid phases, and is the source of liquid shea oil. The fatty acid proportion of West African shea
butter is much more variable than Ugandan shea butter; the oleic content ranges from 37 to 55%.
Variability can even be high in relatively small local populations; a tree that produces hard butter
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can be located right next to one that produces soft butter. Nuts are gathered from a wide area for
local production, so shea butter consistency is determined by the average fatty acid profile of the
population.

Table 2.2: Fatty acid variation in shea butter [8]

Fatty Acid Percentage of Total fatty acid(%)
Mean Minimum Maximum
Palmitic 4.0 2.6 8.4
Stearic 41.5 25.6 50.2
Oleic 46.4 37.1 62.1
Linoleic 6.6 0.6 10.8
Arachidic 1.3 0.0 3.5
Fatty acid carbon chain length:number of double bonds
N.B. Data are from 432 trees samples in 42 populations in 10 countries [8]

2.2.2.1 Phenolics
Phenolic compounds are known to have antioxidant properties. A recent study characterized
and quantified the most important phenolic compounds in shea butter [9]. This study identified 10
phenolic compounds in shea butter, eight of which are catechins, a family of compounds being
studied for their antioxidant properties. The phenolic profile is similar to that of green tea, and
the total phenolic content of shea butter is comparable to virgin olive oil. Phenolics of shea butter
extracted by traditional methods are usually more than those extracted by hexane. Furthermore,
they note that the catechin content alone of shea kernels is higher than the total phenolic content
of ripe olives. [10].
2.2.2Properties of shea butter

Smell: Shea Butter like all other natural products has a natural scent. These scents do not
stink. The natural scent is usually stronger if the shea butter is fresh. As the Shea Butter
gets older, the natural scent diminishes. Shea Butter with no scent is not unrefined shea
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butter. Traditionally extracted or cold pressed shea butter will usually have a nutty and a
slight smoky scent to it because it is prepared under open fire. Once applied to skin or
hair, there is no scent. Unrefined shea butter will not be fragranced.

Shelf-life: This is another area of misunderstanding for some people. Unrefined Shea
Butter does not spoil. Its healing properties are very powerful within the first year and a
half. After that, it is still usable but not as beneficial. There is no need to store it in a
freezer or refrigerator. Treat it like you treat your moisturizers and lotions. Keep it in a
cool dry place. There is no special way to handle it. It just is. If you have ever
encountered spoiled unrefined shea butter, then it was not unrefined shea butter to begin
with.
Texture: The native shea butter is a semi-solid, waxy material which melts at
approximately 30-35C.The texture of shea butter is smooth. Fresh shea butter is usually
very soft. As the shea butter ages, it becomes stiffer but still smooth. Shea Butter is
naturally thick and fatty (in a good way). A little goes a long way. Shea Butter is easily
melted by the hot sun or any form of heat. This will make it liquefy. It will get back to its
solid state once it is in a cool area. When shea butter is melted under direct heat or very
high temperatures, the texture changes. It becomes grainy and never returns to its
original texture. Some processed Shea Butter may have a gummy texture to it.

2.2.4 Importance and uses of shea butter
2.2.4.1 Traditional use of shea butter in Africa
Shea butter has long been used in the West African countries, dating back to ancient Egypt based
on the record that during the Cleopatras Egypt, caravans carried clay jars of valuable shea butter
for cosmetic uses (Goreja, 2004). Many records on traditional uses of shea butter have focused
on its ethno pharmacological uses. Shea butter was used by local healers as a treatment for
rheumatism, inflammation of the nostrils, nasal congestion, leprosy, cough, and minor bone
dislocation [11]. Shea butter has also been used for soothing and accelerating healing after
circumcision, and for preventing stretch marks in African pregnant women (Goreja, 2004),
which is frequently mentioned on the advertisement of shea butter products. Shea butter has also
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been used to massage newly born babies. In addition, shea butter has been used as an insect
repellent, providing protection against Simulium infection (Goreja, 2004).
In addition to the ethnopharmacological uses, shea butter has been used in West African cuisine
as edible oil due to its high nutritional value and affordable price[12].Shea butter is used as the
base of many soups and condiments (Goreja, 2004). For example, when shea butter is mixed
with onion and pepper, it becomes a popular condiment. Beverages made with shea butter
combined with millet flour, water, and savory spices have been served during weddings,
funerals, and work parties.
African local communities have also found uses and applications of shea butter for lamp and
heating oils, lubricants, weather-proofing roofs and soap manufacturing. Shea butter, in
addition, has been beneficial for domestic animals as moisturizer which is applied to dogs to
protect their skin and paws against harsh sand and salt.
2.2.4.2 Benefit of using shea butter
Skin, scalp, and hair emollient and moisturizing activity: Due to the semi-solid
characteristics and buttery consistency, shea butter itself can be used as great emollient
and moisturizer without further processing
Anti-aging of skin due to protease-inhibiting activity: Collagen and elastin are the
major structural proteins providing skin with toughness and plumpness and -amyrin and
lupeol, the triterpenes also found in the unsaponifiable fraction of shea butter, were found
to contribute to the inactivation of proteases such as metalloprotease (e.g., collagenase) as
well as serine protease (e.g., elastase)
Sun-screening function: Cinnamate esters oftriterpene alcohol which are the main
constituent of shea butters unsaponifiable fraction are known to have strong absorbance
of UV radiation in the wavelength range at 250-300 nm, which make the addition of shea
butters unsaponifiables into sunscreens provide synergistic sun-protection by increasing
absorption of UVB radiation.
Anti-inflammatory effect: Traditional uses of shea butter in African folk medicine have
been greatly attributed to the anti-inflammatory properties of shea butter, which may be
related to the unsaponifiable fraction, especially triterpene alcohols and phytosterols.
Although, there is a lack of studies using unsaponifiable components (lupeol, -amyrin,
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and -amyrin) specifically isolated from shea butter, several studies have focused on the
same components found in other species.

2.3 Shea nut processing
2.3.1 Drying of kernels
After the shea nuts are collected the nuts go through five processing steps before they are
place in storage, put out for sale or before butter can be extracted from them. The process of
obtaining dried kernels is depicted schematically in figure 2.5.

FIGURE 2.5 Steps of processing freshly picked nuts into dried kernels[13]
2.3.1.1 Removal of pulp
After the nuts have been collected, the pulp of the shea fruit is removed. The pulp contains
highamounts of sugar that encourages the growth of fungi which decreases oil content of the
kernel. So the purpose of the removal of pulp is to prevent further growth of fungi.
2.3.1.2 Boiling

After depulping the nuts are boiled to terminate the germination process of the nuts. The
germination process starts within a few days after the nuts have fallen to the ground and leads to
the formation of free fatty acids, which will result in poorer shea butter quality and can cause a
bad taste. After the nuts have been cooked for about 45 minutes ash is added to the nuts.
According to the locals this step stops the formation of starch and is needed to successfully
obtain she abutter later on. The prolonged boiling of the fruits tends to destroy desirable natural
compounds that keep the kernel in good condition. The processors state that boiling for a
prolonged period makes extraction of butter during more difficult or even impossible later on.

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2.3.1.3 Drying nuts
When boiling is finished the nuts are left on the ground or on the roof for a couple of days to
dryin the sun. At the end of this drying step, the moisture content of the nuts will be
approximately8% of their weight. Shea can nuts will turn black if the nuts cannot dry well,
forexample if they are wetted by rain or when direct sunlight is not available. Poorly dried or
blacknuts fetch lower prices on the market than well-dried kernels.

2.3.1.4 Removal of shell
The nuts are well-dried when they produce a rattling noise when shaken. At this point, the
shellhas detached from the kernel and the shell can be easily removed by hand after the nut
iscracked. Cracking of the shell is done by gently pounding the nuts with a mortar or stone.

2.3.1.5 Drying kernels
The kernels are then dried for another 3 to 5 days. After this the moisture contents in
kernelsshould be about 1% of their weight. This is done to prevent fungi to grow in the nut.In
table below the results of time of labour and resource costs are shown per processing step.
Thiswas measured during shea nut processing by women in the Kpare community. In table 2.3
anoverview is given on the resources cost, labour time, aim of the step, and tools used
perprocessing step.
1. Time necessary to collect water and firewood is not included
2 .Weather dependent; more sun, less time needed to dry
Once the kernels are dried they are either stored, or they are sold or processed right away.
Generally, shea kernels stored in large plastic sacks inside a storage room. In Ghana there were
two types of standard sized bags which are the one that can contain 120 kg of shea kernels
(40coco bowls1 of kernels), and the smaller bag can contain 90 kg of kernels (30 coco bowls).
During storage the kernels sometimes get infested with fungi. This is the case when the nuts are
not well dried, or when the nuts are stored in humid conditions. To get rid of the fungi the
kernels are washed with fresh water and re-dried for a couple of days. Other problems that occur
during storage are maggots that eat the nuts.

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TABLE 2.3 - Schematic overview: processing steps of getting the nuts ready for storage

2.3.2 Shea butter extraction

FIGURE 2.6 - Steps of processing shea kernels into shea butter
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2.3.2.1 Traditional manual extraction[13]
When the women extract shea butter, a maximum of six to twelve kg of kernels is processed
at a time. This is because some processing steps need to be done on the same day with limited
time intervals, and with too much quantity being processed at the same time, this is not possible.
The processing steps needed for traditional shea butter extraction and that will described in this
section are: 1. breaking 2. roasting, 3. pounding 4. grinding 5. beating and 6. boiling.
A. Breaking
The first step is to is to break the kernels into small pieces so that they are prepared for roasting.
Breaking is done with a mortar and pestle.

FIGURE 2.7Nut crushing
B. Roasting
Then these nut pieces are roasted. After this step it is vital that all the process that follow:
pounding, grinding, beating and boiling are done with limited time intervals. Roasting is stopped
when the kernels attain a deep brown colour and when they can be easily broken by hand.
According to Schreckenberg, roasting at a temperature close to 120C will lead to maximum
butter extraction without the kernel getting burnt. Butter extracted from burned kernel bits will
become black and cant be sold on the market.

FIGURE 2.8Roasting of shea nuts
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C. Pounding
Once roasted, pieces are again pounded with a mortar and pestle to obtain a brown-black paste.
The paste is then removed and put in a cooking pot is heated to facilitate the grinding step which
is next.
D. Grinding
The heated black paste is grinded with a grinding stone on a flat stone surface. This step is
indicated by the respondents to be the hardest. This step is a vital part for the butter extraction
process, for the thoroughness at which the grinding is done will be a determinant factor for the
quantity of butter that is eventually obtained.
E. Beating
Before the paste is beaten, warm water is mixed into the paste. Warm water is added several
times during the beating to keep the paste at a relative high temperature because if the paste
becomes too cold the mass becomes though and beating becomes difficult. During the beating
process the butter should appear as a creamy mass floating on top of the mixture, see figure 2.7.

FIGURE 2.9 - Creamy mass separating from brown water

F. Boiling
This mass is then washed once or twice before boiling. Washing will remove unwanted shea nut
and contaminant compounds from the butter, however it also removes vitamins and taste; so too
much washing is undesirable. To obtain the butter the creamy mass is boiled in a cooking pot.
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FIGURE 2.10Boiling/dehydration

Due the lower boiling point of water compared to the butter, the water will evaporate leaving the
butter behind. Women remove pot from the fire and wait a few minutes for the oil to cool down
and decant to remove any remaining impurities, leaving a clear yellow oil. After this the oil is
left to cool down, it will turn into a solid white butter. The labour and resource costs for each of
the described steps are shown in table 2.4.

TABLE 2.4: Schematic overview of processing steps butter extraction

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2.3.2.2 Chemical (solvent) extraction
Shea butter has been extracted from the seeds of the shea tree, B, Parkii, with various organic
solvents. Petroleum ether (40C-60C), n-hexane, chloroform and benzene. These solvents,
particularly petroleum ether and n-hexane, can be used for the production of shea butter that is
free oxidized fat and coloring impurities. It was, therefore, thought desirable to employ the
solvent extraction, method, which can be used to extract the oil at a lower temperature and thus
avoid oxidation of the fat. Petroleum ether and n-hexane extraction will in a lower recovery than
chloroform, but the products were acceptable in comparison with the product obtained by
chloroform extraction [14].
To remove the natural aroma and color, most companies use a chemical called hexane. This
depletes the natural healing properties not to mention that a harmful chemical has been added. It
is not necessary to take off the shea butter aroma and color as Shea butter is non greasy and will
not clog your pores. It is quickly absorbed into your skin within minutes, leaving it non greasy
and the earthy aroma disappears soon as it is absorbed by the skin. Most of the fatty contents are
obtained by chemical extraction using hexane as the solvent; it has an advantage of higher
percentage of fatty acid.

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2.3.2.3 Soxhlet extractor
In this method, seeds of shea butter were packed in soxhlet extraction and extracted with a
solvent until extraction was complete. The solvent was evaporated under reduced pressure to a
constant weight and the extracted fat was weighed. In the case of aqueous extraction, the
powdered seeds are boiled with a suitable quantity of distilled water and the supernatant oil layer
was weighed. Currently, hexane, a solvent obtained from petrochemical sources, is the solvent
used for oil extraction. This solvent can be emitted during extraction and recovery and has been
identified as an air pollutant since it can react with other pollutants to reduce ozone and
photochemical oxidants.
A lot of work has been carried out on analysis of shea butter oil by a number of workers,
primarily because of extensive demandsfor oils both for human consumption and for
industrialapplications; consequently there is an increasing needto search for oils from non-
conventional sources to augmentthe available ones and also to meet specific applications, hence
the soxhlet extractor was used. A typical operation mechanism is as follow; 300 ml of petroleum
ether was poured into a round bottom flask. 10 g of the sample was placed in the thimble and
was inserted in the centre of the extractor. The soxhlet was heated at 40C-60C. When the
solvent was boiling the vapour rose through the vertical tube into the condenser at the top. The
liquid condensate dripped into the filter paper thimble in the centre which contained the solid
sample to be extracted. The extract seeped through the pores of the thimble and filled the siphon
tube, where it flowed back down into the round bottom flask. This was allowed to continue for
30 min. It was then removed from tube, dried in the oven, cooled in the desiccators and weighed
again to determine the amount of oil extracted. Further extraction was carried out at 30 min
intervals until the sample weight at further extraction and previous weight became equal. The
experiment was repeated by placing 5 g of the sample into the thimble again. The weight of oil
extracted was determined for each 30 min internal. At the end of the extraction, the resulting
mixture containing the oil was heated to recover solvent from the oil.
2.3.2.4 Screw press
Presses have a number of different designs, which can be grouped into screw or hydraulic
operation. Both types can be manual or motor driven. In all types, a batch of raw material is
21

placed in a heavy duty perforated metal cage and pressed by the movement of a heavy metal
plunger. The amount of material in the cage varies from 5-30 kg with an average of 20 kg. Layer
plates can be used in larger cages to reduce the thickness of the layer of raw material and speed
up removal of oil. The pressure should be increased slowly to allow time for the oil to escape.
Screw types are more reliable than hydraulic types but are slower and produce less pressure. The
fat is squeezed out of the heated shea-powder under high pressure. For a high amountof fat, a
press capable of at 125bar pressure is required. The fat must then be cleared of allresidues by
bringing it to the boil together with okra, lemon juice and water. To increase the output, the
process can be repeated. The resulting press cake is excellent for use as fuel forovens and
reduces the fuel wood demand. The amount of fat derived is determined by thecondition of the
shea nut. The yield will be greater if the harvest carefully stored andpreserved. Complete
inactivation of enzymes will prevent the formation of free fat acids.
The heating of the powder to between 100 and 120 Centigrade is not difficult but theunassisted
use of the press needs longer to learn. In order to get a maximum pressure of
125 bar a lot of force is required by the user. [15].

2.3.2.5 Centrifuge
Typical experimental procedures for the centrifugal extraction of shea butter are as follows;
The system designed was a centrifuge machine. It extracted oil from shea nut paste by
centrifugation. Extraction involved separating oil from the water and from the paste cattle cake.
The moving part of the device was driven by a motor, or by an engine, depending on the
availability and convenience of either. A shaft driven by the motor or engine was equipped at its
other end with a rotating drum. The drum, with a capacity of 10 kg of shea paste, had a rotation
speed of 1,000 rpm. That speed was high enough to separate the three components of the paste,
i.e. the oil, which had the lowest specific mass and floated to the surface, the water which had an
intermediate specific mass, and the cattle cake which was heaviest and moved down to the
bottom of the drum. Two bailing devices fitted inside the drum were used to take off the oil and
then the water from the drum, once separation was considered to be sufficient.
Figure-10 shows three different oil extraction processes. The central part of the diagram (Branch
B) presents the traditional butter extraction method, as already explained. The left-hand part
(Branch A) presents the pressing method, which is currently the most widespread or most
22

common mechanical extraction method. The centrifugation method (Branch C), which we tested,
is shown on the right-hand side of the diagram. The expected result in all three methods is the
same i.e. they all aim to squeeze the oil from the cells containing it.
The oil of the kernels or nuts is more or less strongly confined in oil cells, depending on the
capillary strength retaining them [16]. All the methods mentioned above are designed to overcome
forces and burst the cells in order to release the oil they contain [17]. That is done by heating,
pressing, or centrifuging i.e. thermal or mechanical processes. The final step, in all the methods,
i.e. once the oil has been released, is to separate the oil from the other components of the initial
paste. The process tested here set out to dilute the shea paste with water to facilitate diffusion of
the oil from the burst cells into the water. Several types of treatment were tested prior to
centrifugation, the goal being to expel oil from the cells into the water [18]. Each operation, such
as churning, heating or centrifuging, needed to keep the oil clean and clear, meaning that, after
treatment, the oil should display low oxidization and low acidity, a low moisture content, and a
low solid matter content.
23

FIGURE 2:11. Shea butter extraction diagram: (A) manual press, (B) traditional, (C)
Centrifugation.

2.3.2.6 Food processor/dough kneader as a substitute for mixing and kneading steps
In order to improve the quality of the shea butter extraction, new processing technologies has
been introduced. This includes triage (removing germinated, shrunken and insect damaged
kernels), a machine grinder and a hand power mixer. A food processor is a kitchen appliance
used to facilitate various repetitive tasks in the process of preparation of food. Today, the term
almost always refers to an electric-motor-driven appliance, although there are some manual
devices also referred to as "food processors. Food processors are similar to blenders in many
ways. The primary difference is that food processors use interchangeable blades and disks
(attachments) instead of a fixed blade. Also, their bowls are wider and shorter, a more
appropriate shape for the solid or semi-solid foods usually worked in a food processor. Usually,
24

little or no liquid is required in the operation of the food processor, unlike a blender, which
requires some amount of liquid to move the particles around its blade. The food processor can be
used as a substitute for the dough kneading process in the traditional method of extracting shea
butter.

FIGURE2:12. Electrical food processor

The nuts are ground in a machine grinder that has been washed and dried a day before to reduce
impurities and insoluble debris. The hot and cold water mixing and kneading steps are
respectively done in the processor bowl of the mixer as the processor bowl is larger and mere
manufactured than the blender. Water is going to be measured and then added through the feed
chute and the processor lid. The processor has four different speeds- low, medium, fast and
pulse. The speed of the processor should be at maximum during the kneading stage to break the
emulsion during the separation stage large amount of cold water is poured through the chute to
separate the oil from the cake.

2.4 Quality control[19]
2.4.1 Unsaps
Whole unrefined butter recommended for Natural Cosmetic Products since it includes
the complete unsaponifiable content.
Ultra-violet light protection, anti-inflammation, Moisturizing, regenerative & anti-
wrinkle.
25

Presence of significant fraction (3-12% of total butter) includes many bioactive chemicals
e.g. triterpene alcohols, phenols, sterols & karitene.

2.4.2 Impurities
Filtering ensures the removal of fine particles, resulting from extraction methods, but
leaves the chemical benefits intact
The texture of pure, or virgin shea butter can be changed by re-melting & stirring
frequently to prevent crystallization while the butter solidifies
Avoid contamination with iron & water

2.4.3 Scent
The strange but characteristic shea butter smell or scent (combinations of musty,
smoky, vaguely fishy-metallic fragrances) are due to traditional processing methods
&research is in progress to prevent or reduce their prevalence
Shea kernel quality is primary determinant of butter quality including scent.
Therefore those supplying the US need close links to the actual pickers, & first stage
processors, of shea nuts.

2.4.4 Shelf-life
With correct storage, high quality traditional shea butter has a shelf life of at least
one year at room temperature (220 C) recommended to keep bulk shea butter In
refrigerated conditions in sealed containers that exclude light (ultra-violet, air &
water that can damage butter & other chemicals)
Final stage of preparing traditional shea butter is to boil the molten-butter all
microorganisms are destroyed & water content is minimized.

2.4.5 Variability
There is a wide natural variation interns of fat profile, melting point, colour,
unsaponifiable composition, etc, for shea butter of different provenances(source
location). Mixing fats & oils from different shea varieties maybe useful for adjusting
melting-point. R&D is in progress is identify & quantify natural variability.
26

2.5 Factorial experimental design[20]
2.5.1 Introduction
Factorial experiments are experiments that investigate the effects of two or more factors or
input parameters on the output response of a process. Factorial experiment design or simply
factorial design is a systematic method for formulating steps needed successfully implement
a factorial experiment. Estimating the effects of various factors in the output of a process
with a minimal number of observations is crucial to being able to optimize the output of the
process.
In a factorial experiment, the effects of varying the levels of the various factors affecting
the process output are investigated. Each complete trial or replication of the experiment
takes into account all the possible combinations of the varying levels of these factors.
Effective factorial design ensures that the least number of experiment runs are conducted to
generate the maximum amount of information about how input variables affect the output of
a process.

2.5.2Experiments with factors each at two levels
The simplest of the symmetrical factorial experiments are the experiments with each of
thefactors at 2 levels. If there are n factors each at 2 levels, it is called as a 2
n
factorial where
the power stands for the number of factors and the base the level of each factor.
Consider the case of 3 factors A, B, C each at two levels (0 and 1) i.e. 23 factorial experiments.

TABLE 2.5 Two-level 3-factor full-factorial experiment patterns
RUN A B C AB AC BC ABC YIELD
1 - - - + + + - Y1
2 + - - - + + Y2
3 - + - - + - + Y3
4 + + - + - - - Y4
5 - - + + - - + Y5
6 + - + - + - - Y6
27

7 - + + - _ + - Y7
8 + + + + + + + Y8
EFFECT

CALCULATION
A= (Y
+
)/4
-
(Y
-
)/4
The result is then presented on an absolute value of table in order to determine the major
factor affecting the process.

2.6 Economic analysis for developing an improved shea butter industry.
Since labour is underutilized in the improved shea butter processing technology (ISBPT) and
bridge press (BP) methods, more of the effort of the existing labour should be tapped to
enable efficient allocation of labour input. Labour use in the case of the traditional method
should be reduced to allow for efficient resource use. In the case of capital, capital
expenditure should be reduced under the traditional and ISBPT methods for efficient
resource allocation. The BP method is allocatively efficient in the use of capital. To enhance
the adoption of the improvedmethod of processing, limiting factors such as high cost of
processing equipment and lack of access to credit, lack of access to improved equipment,
high maintenance cost, lack of awareness on the improved methods and the poor quality of
butter produced in the BP method must be addressed. These factors could be addressed
A, B and C all three at first level
A at second level and B and C at first level
A and C both at first level and B at second level
A and B both at second level and C is at first level.
A and B both at first level and C at second level.
A and C at second level, B at first level
A is at first level and B and C both at second level
A, B and C all the three at second level

28

through the provision of effective and efficient extension education on the operation of
processing machines, increased access to credit, and the development of more efficient
processing machines at affordable prices.

2.6.1 Nigeria and shea butter
Shea nut has been exported from West Africa to Europe since 18
th
century. Shea trees have
significant economic value and are assets to Nigerians today. According to FAO statistics,
Nigeria produced 372,000 metric tons of shea nuts in 2004 representing 57.1% of the world
total. However the countrys export of shea nuts for that year amounted to only 880 metric
tons, far below the graduation capacity. Majority of the products are wasted.

2.6.2 The state of shea nut in nigeria
Shea nut trees grow wild in the wet savanna area in the northern, southern guinea zones and
the dry savanna of the Sudan zone. In Nigeria today the trees grows in an extremely wide
area of Niger, Nasarawa, Kebbi, Kwara, Kogi, Oyo, Ondo, katsina, Kaduna, Adamawa,
Taraba, Borno and Sokoto State. 70% quantity of shea nut produced are not collected and
thus laid wasted inside bush/farmlands.

29

CHAPTER THREE

MATERIALS AND METHODS
In this chapter, the materials and methods used in the experiment are described in appropriate
sections.
3.1 Raw materials and reagents
1. Shea butter (crude): The crude shea butter was obtained from an open market in Saki, Oyo
state. Nigeria
2.0.1M Sodium Hydroxide (NaOH).
3. Distilled water.
4. 0.1M Potassium hydroxide(KOH)
5. Methanol
6. Phenolphthalein Indicator.
7. 0.5 M Hydrochloric acid (HCl).

3.2 Instrumenation and equipment

1. Royalty turbo Handmixer
2. Plastic bowls
3. 200ml and 500 ml-Beakers.
4. Mortar Pestle
5. Oven
6. Wet mill
7. Small transparent container for sample
8. Porous bits (broken glass).
9. Weighing Balance.
10. Thermometer
11. Water heater/electric kettle
12. Muslin cloth for sieving.
13. Flat bottom flask.
14. Heating Mantle.
30

15. Spatula.
16. Aluminum table spoon.
17. NYC-101 Electric Oven.
18. Scer Scientific 300037 Programmable refractometer.
19. Conical Flask.
20. Crystal display of tachometer.
21. Water bath.
22. Reflux Condenser
23. Burette
24. Pipette
25. Stopwatch

3.3 Methods
3.3.1 Seed preparation
Seed Cleaning: The Shea nuts were soaked for about 30mins in hot water and washed several
times with clean hot water to get rid of possible surface mould and possible oxidized oil emitted
from bad nuts.
Drying: The kernels were dried under the sun till they were totally dried, this took about 2days,
this dehydrates the wets nuts and exposes the bad ones from the lot. Bad and black nuts are then
separated from the good ones. The kernels were kept in an air-tight plastic container prior to use.

FIGURE 3.1 BLOCK FLOW DIAGRAM OF SEED PREPARATION

SOAKING WITH
HOT WATER
WASHING WITH
HOT WATER
DRYING
31

3.3.2 Traditional method upgrade

FIGURE 3.2 BLOCK FLOW DIAGRAM OF TRADITIONAL UPGRADE PROCESS

Nut crushing: The selected nuts are then broken into smaller portions by mortar and pestle
making them ideal for the oven.
Roasting of crushed nuts: The crushed nuts are sent to the oven immediately after crushing and
roasted at 105-115C for30mins.

FIGURE 3.3Electric Oven

NUTS CRUSHING ROASTING OF
CRUSHED NUTS
MILLING OF
ROASTED NUTS
HOT WATER
KNEADING

COLD WATER
KNEADING
COLD WATER
MIXING
COLD WATER
SEPARATION
SCOOPING OF
FAT
BOILING OF FAT
FILTRATION OF
OIL
SOLIDIFICATION
32

Nut Crushing: The roasted Shea nuts are allowed to cool down for at least 10 minutes and at
most 30 minutes, before being milled in a milling machine into a fine paste.
Cold water kneading: Mixing continues and small amount of coldwater added from time to
time to get a smoother texture. This vigorous mixing breaks the emulsion, causing the fat to
break away from the cake.

FIGURE 3.4 Hand mixer

Hot water kneading: When the fat begins to break away from the cake (this is indicated by the
colour of the mixture from chocolate to milk chocolate), hot water is added to the paste to melt
the fat and set it free from the cake. This important step facilitates the separation.

FIGURE 3.5 Electric Water bath

Cold water separation: Large amount of coldwater is then poured on the mixture and stirred
continuously causing a grey, oily scum to rise. As the stirring continues, more fat is washed and
forced to float on the cold water that separates it from the cake, which now begins to settle at the
bottom of the rubber bowl. Hence the fat was gathered from the surface.
33

Scooping of fat: The fat was collected from the surface of the cake with a flat metal spoon.
Boiling of fat: Boiling dehydrates the fat completely. It also clarifies the oil/butter as last cake
residues are fried and settle under the pot.

FIGURE 3.6Heating mantle

Filtration and solidification: The oil was filtered using a muslin cloth and then allowed to
solidify by putting it in the refrigerator.

3.3.2.1 Experiment 1
Determining the major factor affecting the production of shea butter
The factor was determined by using a factorial experimental design, hence the experiment was
ran 8 times (2
3
) at different conditionsand was repeated again.
Experimental Run 1
300g of Shea butter was weighed into the Hand Mixer.
Kneading was started at the lowest speed of kneading blade i.e (speed1 for
2minutes) with 2 minutes interval rest after kneading to avoid overheating in the
motor of the kneader.
After the first rest, 50ml of water at room temperature was added to the paste.
34

Subsequent kneading was done at speed 3 for 7minutes with 2 minutes interval
rest after kneading to avoid overheating in the motor of the kneader
Water at 35C was added at a volume of 100ml at two different times after the
second rest.
The last 2 cycles are done for 8 minutes instead of the initial 7 minutes.
The total time for the experimental run was 30minutes.
2000ml of water at room temperature was added and then the fat was scooped
from the surface of the kneaded mixture with a flat metal spoon.
The fat was then boiled until all the water present had evaporated and the residue
shea cake had been fixed in the oil.
The hot oil was allowed to cool and then sieved through a muslin cloth. The
filtered oil was then weighed and refrigerated till analysis was to be carried out.
The yield of the oil in percentage was evaluated.
Experimental Run 2
second rest.
35

Experimental Run 3
After the second and third rest, 50ml of water at room temperature was added to
the paste.
Water at 35C was added at a volume of 100ml after the fourth and fifthrest.
Experimental Run 4
the paste.
36

Water at 45C was added at a volume of 100ml after the fourth and fifth rest.
Experimental Run 5
second rest.
37

Experimental Run 6
second rest.
Experimental Run 7
the paste.
38

Experimental Run 8
the paste.

39

Determination of the effect of speed of kneading blade on yield.
The shea paste is prepared as shown in the block diagram of traditional upgrade process.
Experimental Run
second rest.
This procedure was repeated using kneading speed 3, 4, 5.

Determination of the effect of time of kneading on yield.
The shea paste is prepared as shown in the block diagram of traditional upgrade process.
40

Experimental Run
The experiment was carried out as experiment 3.3.2.2 using speed 5 and
temperature of water added at 45C for total kneading periods of 45minutes and
30minutes and 20minutes each.

Examining the effect of roasting on yield.
A sample of the cleaned dried kernels was wet-milled without roasting.
Experimental Run
The experiment was carried out as experiment 3.3.2.2 for a total kneading period
30minutes.

3.3.3 Determination of the physio-chemical properties
Shea butter samples from traditional upgrade was analyzed and the following analyses was
carried out
3.3.3.1 Acid value
Acid value (or "neutralization number" or "acid number" or "acidity") is the mass of potassium
hydroxide (KOH) in milligrams that is required to neutralize one gram of chemical substance.
The acid number is a measure of the amount of carboxylic acid groups in a chemical compound,
such as a fatty acid, or in a mixture of compounds. In a typical procedure, a known amount of
sample dissolved in organic solvent is titrated with a solution of potassium hydroxide with
known concentration and with phenolphthalein as a color indicator.

41

Procedure:
I. 10.0g of the oil sample was weighed into 250ml conical flask.95% alcohol (neutral
alcohol) was prepared by diluting methanol with sodium hydroxide (5ml NaOH + 95ml
ethanol= 100ml neutral alcohol).
II. 50ml of neutral alcohol and 50ml benzene were added to the oil in the flask. The contents
of the flask were shaken well to dissolve.
III. The contents of the flask were shaken well to dissolve. The contents were then titrated
against 0.1Npotassium hydroxide solution using phenolphthalein as indicator.
IV. The end point was the appearance of a pale permanent pink colour and the titre value
were recorded.
The acid value is calculated mathematically as:
Acid Value =

(3.1)
Where,
X = volume of KOH required to neutralize the solution (ml)
M
1
= strength of KOH

W
1
= weight of oil used (g)
The number 56.1 is the atomic weight of potassium hydroxide (KOH)
3.3.3.2 Refractive index
The refractive index of a substance measures how the substance affects light traveling through it.
It is equal to the speed of light in a vacuum divided by the speed of light in that substance. When
light travels between two materials with different refractive indexes, it bends at the boundary
between them.
The refractive index test was carried out using a programmable refractometer.
Procedure:
I. The apparatus is firstly standardized using pure distilled water whose refractive index at
20
0
C is 1.3330.
42

II. A drop of the sample was inserted into the machine. After about 1-2 minute(s) the
machine read off the refractive index in Brix scale and the temperature at which the
refractive index was taken.
III. The actual refractive index was gotten by converting from Brix scale to normal refractive
index using conversion tables.
FIGURE 3.3 REFRACTOMETER

3.3.3.3 Saponification value
Saponification value is the number of mg of potassium hydroxide (KOH) required to saponify
the esters in 1g of a sample; and to neutralize the free acids. It also indicates the amount of
average molecular weight of triglycerides contained in the oil.

Procedure:
I. 1 gram of oil was weighed into 250ml dry round bottom flask.
II. 50ml of 0.5ml alcoholic potassium hydroxide was added to the oil. Porous bits were
added to ensure uniform heating.
III. The reflux condenser was setup and the contents of the round bottom flask was refluxed
for about 1 hr. after refluxing the mixture is allowed to cool and is then titrated against
standard hydrochloric acid and the titre values are recorded. Similarly,
IV. 50ml of the same alcoholic KOH, blank (no oil added) was refluxed in a round bottom
flask for 1hr, cooled and titrated against standard 0.5N HCL.
V. The titre value was recorded and the titre value gotten was then used to determine the
saponification value.
The saponification value is calculated mathematically as:
Saponification Value =

(3.2)
43

Where,
Z = volume of HCL required to neutralize excess alkali (ml)
Z = (X Y) ml
X = titer value of HCL against oil and KOH after reflux (ml)
Y = titer value of HCL against KOH alone after reflux (ml)
M
1
= strength of HCL
W
1
3.3.3.4 Ester value
Ester value was obtained by subtracting the acid value from the saponification value. Ester value
represents the number of milligrams of potassium hydroxide required tosaponify the esters
present in 1g of the oil.

3.3.3.5 Specific gravity
The Specific Gravity - SG - is a dimensionless unit defined as the ratio of density of the shea
butter oil to the density of water at a specified temperature. This was done by measuring the
density of shea butter oil in reference to the density of distilled water at 20C

3.3.4 GC Analysis of fatty acid composition
3.3.4.1 Transesterification of fatty acids to fatty acid methyl esters (fames)
0.5 g of homogenized shea butter was refluxed with 5 mL of 0.5 N potassium hydroxide
methanolic solution for 5 minutes. After the reflux, 15 mL of ammonium chloride and sulfuric
acid in methanol solution was added and heated for 3 minutes and after the mixture cooled down,
10mL of hexane was added and a solvent fraction was recovered using separating funnel. Then
1.5 mL of the solvent fraction containing fatty acid methyl esters (FAMEs) was dried over
sodium sulfate, and centrifuged at 13000 rpm for 5 minutes. After the centrifugation, the
resultant solution was subjected to GC analysis.
44

3.3.4.2 Identification of (FAMES) using gas chromatography with flame ionization
detector (GC-FID)
FAMEs were analyzed on an Econo-Cap EC-WAX Capillary Column (length 30m,
internal diameter 0.25mm, phase Polyethyleneglycol, film 0.25m, Alltech, Deerfield, IL) in an
HP 6890 series gas chromatograph equipped with a flame ionization detector and an automated
injector (Agilent, Wilmington, DE). Samples were injected at an initial oven temperature of 60
C held for 1 minute. Then the column temperature was increased at a rate of 10C / min to 200
C. The injector and the flame ionization detector (FID) temperatures were set to 220 C. Helium
was used as the carrier gas.
Peak identification was performed by comparison of retention times of standard solutions to that
of individual fatty acid standards. Fatty acids were expressed as % of total fatty acids.

3.3.5 Determination of the speed in revolution per minute of the kneading blade.
This was done to know the actual rotational speed of the kneading blade; the different rotational
speeds of the processor are indicated as 1,2,3,4 and 5 on the food processor.
The speed of the kneading blade was measured by using photo/contact tachometer. The speed
had to be determined by measuring the speed levels from 1-5. This was done by contacting the
tachometer at the point of attachment of the kneading blade at a particular sped level and
recording the measured value (the measured value is given on the liquid crystal display of
tachometer). This was done for all speed level.
3.4 Safety precautions
All nuts were washed and rinsed several times with clean hot water to get
ridofpossible surface moldand possible oxidized oilemitted from bad nuts.
Zero error of the measuring balance was avoided when measurement was carried out.
The shea nut paste was milled in batches in order to avoid the surface area of the
paste from been exposed.
The kneading time operation was properly monitored using a digital stopwatch in
order to ensure accuracy.
45

Special care was taken with heat source (oven and heating mantle) to avoid all unsafe
conditions.
During the experiment, all fans were switched off to avoid inaccuracy in
measurements.
Clockwise direction was maintained during the kneading process in order to ensure
uniform mixing.

46

CHAPTER FOUR

RESULTS AND DISCUSSION OF RESULTS
In this chapter the result of the experiments carried out in the laboratory are outlined and
described in various sections.
4.1 Results
4.1.1 Calibration of the speed of the kneading blade in revolution per minute

TABLE 4.1 Kneading speed in revolutions per minute
SELECTOR SPEED ACTION SPEED (RPM)

1 874.9
2 912.3
3 996.9
4 1018
5 1123

4.1.2 Determination of yield of oil
4.1.2.1 Factorial experimental design using manual method
Where A= Temperature (- =35C, + = 45C)
B=Time (- =30mins, + = 45mins)
C= Speed (- =996.9rpm, + = 1123rpm

47

TABLE 4.2 Manual Factorial experimental results (Detailed calculation is shown in the
appendix C)
MAIN
EFFECTS
INTERACTION
EFFECTS
YIELDIN%
RUN ORDER OF
RUN
A B C AB AC BC ABC Y
1

Y
2

1 7 - - - + + + - 28.7 24.1 26.4
2 3 + - - - - + + 28.8 30 29.4
3 5 - + - - + - + 25.6 23.8 24.7
4 1 + + - + - - - 29.7 30.1 29.9
5 8 - - + + - - + 31.3 28.7 30
6 4 + - + - + - - 33.1 33.7 33.4
7 6 - + + - _ + - 27.3 25.3 26.3
8 2 + + + + + + + 20.1 22.1 21.1
ABSOLUTE VALUE
OF EFFECT
1.6 4.3 0.1 1.6 2.5 3.7 2.7 27.65

From the above result it is shown that factor B which is time produces the greatest effect in the
yield of shea butter. B=4.3.

FIGURE 4.1 Main Effects for shea butter yield (fitted means)
45 35
30
29
28
27
26
45 30
5 3
30
29
28
27
26
TEMPERATURE
M
e
a
n
TIME
SPEED
Main Effects Plot for YIELD
Fitted Means
48

FIGURE 4.2 Interaction plot for shea butter yield (fitted means)

4.1.2.2 Factorial experimental design using minitab

TABLE 4.3 Minitab Factorial experimental results

RunOrder PtType Blocks
TEMPERATURE
(C)
TIME
(mins)
SPEED
(rpm) YIELD
1 1 1 35 45 996.9 24.7
2 1 1 45 30 1123 33.4
3 1 1 45 45 1123 21.1
4 1 1 45 30 996.9 29.4
5 1 1 35 45 1123 26.3

6 1 1 45 45 996.9 29.9
7 1 1 35 30 996.9 26.4
8 1 1 35 30 1123 30
45 30 5 3
30.0
27.5
25.0
30.0
27.5
25.0
TEMPERA TURE
TIME
SPEED
35
45
TEMPERATURE
30
45
TIME
Interaction Plot for YIELD
Fitted Means
49

FIGURE 4.3 Pareto Chart of the Effects of shea butter

The uncoded correlation equation from the design software is as follows
Y=583.351-17.5324A-19.4948-0.550357C+0.583872AB+0.0174465AC+0.0189268BC-
0.000570975ABC

0
0.5
1
1.5
2
2.5
3
3.5
4
4.5
5
B BC ABC AC AB A C
E
F
F
E
C
T

TERM
FACTOR NAME
A TEMPERATURE
B TIME
C SPEED
Lenth's PSE= 3.75
50

4.1.3 Effects of the speed of kneading blade on shea butter yield

TABLE 4.4 Effects of kneading speed on yield (Detailed calculation of yield is shown in the
appendix C)
Temperature = 45C and Time = 30minutes
Speed (RPM) Weight of Oil (grammes) Yield (%) Yield % using
Minitab Equation
ERROR
912.3 60.9 20.3 27.4 7.1
996.9 88.2 29.4 29.4 0
1018 90.3 30.1 31.4 1.3
1123 100.2 33.4 33.4 0

FIGURE 4.4Effects of kneading speed on yield

y = -0.0003x
2
+ 0.7193x - 367.0121
R = 0.9970
20
22
24
26
28
30
32
34
36
900 950 1000 1050 1100 1150
Y
I
E
L
D

(
%
)

SPEED OF KNEADING BLADE (RPM)
TEMP= 45C
TIME=30mins
51

4.1.4 Effects of kneading time on shea butter yield

TABLE 4.5 Effect of kneading time on yield (Detailed calculation of yield is shown in the
appendix C)
Temperature = 45C and Speed =1123rpm
Time (minutes) Weight of oil (grammes) Yield (%)
45 63.3 21.1
30 100.1 33.4
20 39.6 13.2

FIGURE 4.5Effects of kneading time on yield
y = -0.1136x
2
+ 7.7x - 95.36
R = 1
10
15
20
25
30
35
40
20 25 30 35 40 45 50
Y
I
E
L
D

(
%
)

KNEADING TIME (minutes)
TEMP= 45C
SPEED = 1123rpm
52

4.1.5 Effects of roasting before kneading on shea butter yield

TABLE 4.6 Effects of roasting on yield (Detailed calculation of yield is shown in the appendixC)
Shea paste Weight of Oil (grammes) Yield (%)
Roasted 100.1 33.4
Unroasted 8.4 2.8

FIGURE 4.6Effects of roasting of shea paste before kneading

4.1.6 Physicochemical properties
0
5
10
15
20
25
30
35
40
ROASTED UNROASTED
Y
I
E
L
D

(
%
)

SHEA PASTE
TEMP= 45C
TIME=30mins
53

TABLE 4.7 Physicochemical properties of Shea butter yield
Oil Sample Acid value Saponification
Value
Ester
Value
Refractive
index
Specific
Gravity
@20C
Roasted 12.31 168.3 155.99 1.4666 0.912
Unroasted 5.31 210.38 205.07 1.4660 0.923

4.1.7 Chromatographic analysis of free-fatty acid composition of shea butter
The common names of the some of the components of the shea butter are listed below [22].
n-Hexadecanoic acid = Palmitic acid
Octadec-9-enoic acid = Oleic acid
Trans-13-Octadecanoic acid = Elaidic acid
Octadecanoic acid = Stearic acid
Cis-13- Octadecanoic acid = Linoleic acid

a. Roasted Shea butter sample.
TABLE 4.8Fatty acid variation in Roasted shea butter
Retention time Component Percentage in oil (%)
25.609 Palmitic acid 6.75
29.419 Oleic acid 7.92
29.557 Elaidic acid 16.99
29.974 Stearic acid 13.31
TOTAL 74.08
b. Unroasted shea butter sample
TABLE 4.9Fatty acid variation in unroasted shea butter
54

Retention time Component Percentage in oil (%)
11.464 5-Tetradecene 2.73
25.448 Palmitic acid 5.94
29.276 Linoleic acid 8.29
29.374 Cis-Vaccenic acid 20.42
40.451 Squalene 1.24
TOTAL 92.62

4.2 Discussion of result
4.2.1 Calibration of the speed of the kneading blade in revolution per minute
The various speed of the electric food mixer (i.e 1, 2, 3, 4, 5) was calibrated in
revolutions per minute using a device used for measuring the speed of rotation which is a crystal
display tachometer. And the speeds in revolution per minutes are 874.9, 912.3, 996.9, 1018 and
1123 according to Speed 1, 2, 3, 4, and 5 respectively.

4.2.2 The factorial experimental design for the effects of various factors on the oil yield
In determining the oil yield, a factorial experiment was designed using 8 runs (i.e 2
3
) where the 3
main effects are: (A= temperature), (B= time) and (C=speed) was put into consideration at their
higher and lower values. (i.e temperature - =35 C and 45 C, time - = 30mins, + = 45mins,
speed - = 3, + = 5). The absolute value of effect of all main effects and interaction effects were
determined and the factor B, The time was determined as the major factor affecting the oil yield
with absolute value of 4.3. Thus increase in time produces a reduction in the yield of shea butter
and also the factors BC (Speed and Time) also had a great effect on the oil yield with absolute
effect of 3.7.
55

The manual calculation of the factorial experimental results were compared with the factorial
experimental design calculation using a software called minitab, is shown in Table 4.2 and
4.3respectively. Figure 4.1 shows the main effect s plot for the shea butter yield (using a fitted
means). The temperature plot shows that the yield of oil increases as the temperature increases,
while the oil yield decreases as the time increases. Also the yield of oil is virtually independent
of kneading speed.
The interaction plot for the shea butter yield shown in Figure 4.2 which basically compares the
relative strength of the effects across the factors. The first plot which describes the temperature
and time interactions indicates that both extraction time and extraction temperature have similar
effects on the yield of oil .For both factors, the yield decreases with temperature and kneading
time. However the interaction plot shows that the decrease in yield is greater when the time is
high (45mins) than when reaction time is low (30mins). The second plot which describes the
speed and temperature interactions indicates that the reaction speed and temperature have
different effects on the yield of oil. At the lower temperature the oil yield increases as the speed
increases while the higher temperature yield of oil decreases as the speed increases. The third
plot describes the speed and the time interaction. At lower kneading time, the yield of oil
increased with speed of kneading while at higher kneading time, the yield decreased with
increased kneading speed. However the increases in the yield is far greater when the kneading
time is (30mins) than when the kneading time is (45mins).
The pareto chart in figure 4.3 shows the magnitude of the effects of the three factors on the
yield and their respective absolute value. The pareto chart confirms the observation that kneading
time is by far the most important parameter affecting the yield of oil. The effect of other factors;
temperature and speed are much lower. The chart also shows effect of interaction, that is, the
effect of time depends on the level of the kneading rate.

4.2.3 The effects of the speed of kneading blade on shea butter yield.
The effect of the kneading speed on the yield was studied for 30mins, since the yield was
higher at lower kneading period. The results have been illustrated in figure 4.4 and tabulated data
56

in Table 4.4. The rate of increase in yield is much faster at the lower kneading rate than at higher
kneading speed. Increase in speed of kneading blade leads to increase in oil yield simply because
more vigorous kneading and mixing process helps to break the emulsion quickly, causing the fat
to break away from the shea cake completely
[19]
.

4.2.4 The effect of kneading time on shea butter yield
The results have been illustrated in figure 4.5 and tabulated in table 4.5. It was observed that
the yield of oil increased as the kneading time increases from 20 minutes to 30 minutes. This was
so because enough time is required for the fat to break away from the shea cake (which is
indicated by the change in colour of the mixture from chocolate to milky chocolate). It was also
noticed that the yield of oil at kneading time of 45 minutes was lower than that of kneading time
of 30minutes. Longer kneading time resulted in the separated fat remixing with the shea butter
cake. Less fat could be scooped from the surface of shea butter cake as a result of this.
It was observed that the oil yield increases as the kneading time increases from 20
minutes to 30 minutes; this was so because enough time is required for the fat to break away
from the shea cake (which is indicated by the change in colour of the mixture from chocolate to
milky chocolate). It was also noticed that the oil yield at kneading time 45 minutes was lower
than that of kneading time of 30minutes and 20 minutes, this occurred because after the time in
which the fat had melted (i.e separated from the cake, the fat then begins to mix with the shea
cake, which resulted in the lower amount of fat scooped at time 45 minutes.
4.2.5 The effect of roasting before kneading on shea butter yield
The effect of the roasting of the shea butter variation is clearly shown in Table 4.5. Roasted and
unroasted shea butter has an oil yield of 33.4% and 2.8% respectively. The roasted shea butter
resulted into higher oil yield simply because roasting of shea nut tends to make the fat crystalline
structure loosen for extraction.
[24].

4.2.6 Physicochemical properties of shea butter oil
The table below shows the comparison of the physicochemical properties of the roasted
and unroasted shea butter to literature values.
57

TABLE 4.10 Comparison of Physicochemical properties of shea butter extracted with literature
values extracted
Properties Roasted shea butter Unroasted shea butter Literature value[1]
Acid value 12.31 5.31 0.463-12.59
Refractive index 1.4666 1.4660 1.453-1.6
Saponification Value 168.3 210.38 160-223
Ester value 155.99 205.07 159.537-210.41
Specific gravity 0.912 0.923 0.916-0.917

The acid value of shea butter oil is the mass of KOH in milligrams that is required to
neutralize 1g of the shea butter oil. Basically the acid value is used to quantify the amount of
acid present. Roasting raises the Temperature of the shea butter mix. This decreases the viscosity
of the oil which tends to move towards the surface. Higher temperature tends to break and
destroy the cell during size reduction which tends to increase the acid formation. Hence the rate
of acid formation was higher when the shea butter was roasted. The acid value of roasted and not
roasted shea butter falls within the literature range of acid values as shown in Table 4.10. Hence,
roasting of shea nut before milling tends to increase the acid content.
Refractive index is the ratio of the speed of light in a vacuum to that in the oil under
examination which is related to the degree of saturation and the ratio of cis/trans double bonds,
and can also provide hints on the oxidative damage. The refractive index decreased from 1.4666
to 1.4660 for roasted and unroasted shea butter respectively. Basically the refractive index is
used for rapid sorting of fats and oils of suspected adulteration. Hence the refractive index of
roasted shea butter was higher than the unroasted shea butter because the shea butter continues to
be adulterated as the heating temperature increases
[24]
. This is due to excessive heating of the
shea nut in the oven. Both refractive index values of the shea butter oil falls within the literature
range of values as shown in Table 4.10.
58

The saponification value of shea oil is the number of milligrams of KOH or NaOH
required to saponify 1g of shea butter oil. It is a measure of the chain lengths of the fatty acid
presents. The saponification value decreased from 210.38 to 168.3 for unroasted and roasted shea
butter respectively. High saponification value may suggest use of the oil in the soap industry
[24]
.
Therefore, the unroasted shea butter oil has a higher chance of being used for the manufacturing
of soap. Both saponification values of the shea butter oil falls within the literature range of
values as shown in Table 4.10.
The Ester values decreased from 205.07 to 155.99 for unroasted and roasted shea butter
respectively. The higher the ester value, the more the palatability of the oil. Hence the unroasted
shea butter oil is more palatable and will therefore have better taste
[24]
. The ester value of roasted
she butter falls within the literature range of acid values as shown in Table 4.10.
Specific gravity of the shea butter is the density of the shea butter oil relative to the
density of water. Specific gravity decreased from 0.912 to 0.923 for roasted and unroasted oil
respectively. The unroasted oil has a higher specific gravity because it contains some amount of
moisture in it which was not removed completely since it was not heated in the oven
[24]
.. The
specific gravity value of roasted shea butter falls within the literature value as shown in Table
4.10

4.2.7 Chromatographic analysis of shea butter oil
The table below shows the comparison of the five principal fatty acids composition of
shea butter from the Chromatographic Analysis of roasted and unroasted shea butter with
literature values.

59

TABLE 4.11 Comparison of the five principal fatty acids composition of shea butter
Fatty Acid Roasted Shea
butter
Unroasted
Shea butter
Literature values [8]
Percentage of Total Fatty Acids
Mean Min Max
Palmitic Acid 6.75 5.94 4 2.6 8.4
Stearic Acid 24.9 23.01 41.5 25.6 50.2
Oleic Acid 7.92 - 46.4 37.1 62.1
Linoleic Acid - 8.29 6.6 0.6 10.8
Arachidic Acid - - 1.3 0.0 3.5

Shea butter is composed of five principal fatty acids: palmitic, stearic, oleic, linoleic, and
arachidic [23]. The fatty acid composition is dominated by stearic and oleic acids, which together
account for 85-90%of the fatty acids [23]. The relative proportions of these two fatty acids
produces differences in shea butter consistency. The high stearic acid content gives the shea
butter its solid consistency, while the percentageof oleic acid influences how soft or hard the
shea butter is. Palmitic Acid, Stearic Acid and Oleic acid were present in the roasted shea butter
sample while Palmitic Acid, Stearic Acid and Linoleic Acid were present in the unroasted shea
butter sample. The relative amount of stearic acid was only slightly higher than that of oleic acid
in the roasted shea butter sample. The percentages of stearic acid in the two samples (i.e roasted
and unroasted shea butter) were quite similar but still lower than the minimum values reported in
literature. [8]
Hence the difference in the compositions of the values of fatty acid in table 4.11 may be
due to the following reasons;
Variations in species location (i.e Geographical location)
Improper handling of oil samples when transferring to the location where the
analysis was carried out.
What is surprising is the relatively low content of oleic acid in the samples. The 7.92% content in
the roasted sample contrast sharply with the 37.1 to 62.1% reported in literature [8]. In the case of
60

the unroasted sample, no oleic acid was detected. Further analysis is needed to confirm if the
difference is due to regional varieties of the shea nuts.

61

CHAPTER FIVE
CONCLUSION
An upgrade of the indigenous technology for the production of shea butter using a food
processor (Electric hand mixer) was developed in this research work.
The findings in this work can be summarized in the following statements.
1. The yield of shea butter depended on the three main factors (Kneading Time, Speed of the
kneading blade and Temperature of the shea paste).
2. The time factor was the major determinant of the shea butter yield.
3. The oil yield increased as the kneading time increased from 20 minute to 30 minutes but
decreased after.
4. Roasting of shea butter increased the yield of the shea butter.
5. The saponification value, Ester value and specific gravity from unroasted shea nuts were
higher than those from roasted shea nuts.
6. The acid value and refractive index of the shea butter from roasted shea nuts were higher
than those from the unroasted shea nut.
7. The fatty acids composition of the roasted and unroasted shea butter extracted are palmitic
acid, stearic acid, linoleic acid and oleic acid but linoleic acid was not present in the roasted
shea butter. The oleic and stearic acid fractions are much lower than those reported in the
literature.

62

CHAPTER SIX

RECOMMENDATION
In the course of this study, various challenges were encountered. Thus for the future
improvements on the production of shea butter developed in this study, the following
recommendations have been made:
1. The mortar and pestle used for breaking the shea nuts should be replaced with advanced
equipment like a nut cracker so as to increase the efficiency.
2. The food processor should be replaced with a more efficient processor that has paddles so
that the production can be scaled up.
3. The milling machine should be available within the experimental environment so as to
reduce impurities and contamination of the paste.
4. Improvement can be done on the mixer by adding more dough hooks to allow a uniform
kneading and to also allow the mixer work effectively through each section without
having to move the mixer around the kneading.
5. Gas chromatography for free fatty acid analysis should be available within the
experimental environment so that analysis can be easily monitored and errors can be
checked.

63

REFERENCES
1. Hee Seung Nahm, Quality Characteristics of West African Shea Butter (Vitellaria
paradoxa) and Approaches to Extend Shelf-life, May 2011
2. Davrieux, F., Allal, F., Piombo, G., Kelly, B., Okulo, J.B., Thiam, M., Diallo, O.B. &
Bouvet, J.-M. (2010) Near Infrared Spectroscopy for High-Throughput Characterization
of Shea Tree (Vitellaria paradoxa) Nut Fat Profiles. Journal of Agricultural and Food
Chemistry, 58, 7811-7819.
3. Dr. Peter Lovett, The Shea butter Value Chain: Production, Transformation,and
4. Hamm W. and Hamilton R.J., Edible Oil Processing, CRC Press, 2000.
5. Jari Alander & Ann-Charlotte, Andersson, The shea butter family the complete
emollient range for skin care formulations, Karlshamns AB, Lipids for Care, 37482
Karlshamn, Sweden.
6. 21 Reasons to use shea butter, American Shea Butter Institute (ABSI), 2009.
7. Gabriel I.O. Badifu,Food potentials of some unconventional oilseeds grown in Nigeria
A brief review.
8. Maranz, S, Z. Wiesman, J. Bisgaard and G. Bianchi. 2004. Germplasm resources of
Vitellaria paradoxa based on variations in fat composition across the species distribution
range. Agroforestry Systems 60:71-76).
9. Carol Kelling, The Numerous Topical Benefits of Unrefined Shea Butter (2008)
10. (Maranz, S., Z. Wiesman and N. Garti. 2003. Phenolic constituents of shea (Vitellaria
paradoxa) kernels, J Agric Food Chem 51: 6268-6273).
11. Tella A. 1979. Preliminary Studies on Nasal Decongestant Activity from the Seed of Shea
Butter Tree, Butyrospermum parkii. Br. J. clin. Pharmac. 7:495-497.
12. Nielsen S.S. 2010. Food Analysis. Springer, New York, NY. Ch 14.
13. Shea nut and butter in Ghana Opportunities and constraints for local processing, Caroline
Mayumi Malotaux,Mirjam van Leeuwen,Mirjam Tolkamp2009.
14. A. Kar and H.C. Mital, The study of shea butter VI. The extraction of shea butter, Faculty
of pharmaceutical sciences. University of Nigeria, Nsukka, Nigeria, Received 21
November 1980, in revised from 14 July 1981,pp 86-87
64

15. Shea Butter Extraction in Mali, Appropriate Technology Bulletin No 6
Appropriate Technology International, 1985
16. ADEME AGRICE. 2001. Tensioactifs et olagineux, Etude sur les matires premires
olagineuses disponibles sur le march europen, URL :
http://www.ademe.fr/htdocs/publications/publipdf/etude.pdf
17. Anon. 2008. FIRSIT: Impact de la recherche scientifique, des inventions ET des
innovations sur les socit africaines. IRD, Ouagadougou, Burkina Faso.
18. Kapseu C., Tchiegang C., Parmentier M., Fomethe, A. and Kamga, R. 2001. Evolution du
Choix technologique par les femmes, Universit de Ngaoundr, URL : http://www.uni-
bayreuth.de/afrikanistik/mega-tchad/Table/Colloque2002/Kapseu.pdf
19. P. Lovett, The shea butter; A unique African product WATH, USAID.
20. P.K. BATRA AND SEEMA JAGGIIndian Agricultural Statistics Research Institute,
Library Avenue, New Delhi - 110 012. Factorial Experimental design.
21. Chemistry And Technology Of Oils And FatsChemistry And Technology Of Oils And
Fats By Dr. M.M. Chakrabarty
22. Lipomics fatty acid library
23. Maranz, S, Z. Wiesman, J. Bisgaard and G. Bianchi. 2004. Germplasm resources of
Vitellaria paradoxa based on variations in fat composition across the species distribution
range. Agroforestry Systems 60:71-76.
24. Quality characteristics of shea butter recovered from shea kernel through dry extraction
process. Olaniyan AM, Oje K. J Food Sci Technol, 2007, 44(4), 404-407

65

APPENDIX A
EXPERIMENTAL RUNS
1. EXPERIMENT 1- Determining the major factor affecting the production of shea
butter
a. RUN 1
Temperature= 35C
Time= 30minutes
Speed= 3 (996.9rpm)

WEIGHT
OF
PASTE
KNEADING
TIME
SPEED VOLUME
OF
WATER
ADDED
TEMPERATURE
OF WATER
ADDED
OBSERVATION
300g 2 1 -
2 - -
7 3 50ml 25C Paste becomes
soft
2 - - The paste
becomes smooth
and uniform
7 3 100ml 35C
2 - - The fat breaks
away from the
cake
8 3 100ml 35C
2 - - The colour
changes from
chocolate to milk
chocolate
8 3 - The fat melts and
its set free from
the cake.

Weight of container = 10.2g
Weight of container + oil =89.4g
Weight of oil =79.2g
Yield = 26.4%

66

b. RUN 2
Temperature= 45C
Time= 30minutes
Speed= 3 (996.9rpm)

WEIGHT
OF
PASTE
KNEADING
TIME
SPEED VOLUME
OF
WATER
ADDED
TEMPERATURE
OF WATER
ADDED
OBSERVATION
300g 2 1 -
2 - -
soft
2 - - The paste
becomes smooth
and uniform
7 3 100ml 45C
away from the
cake
8 3 100ml 45C
2 - - The colour
changes from
chocolate to milk
chocolate
its set free from
the cake.

Yield = 29.4%

c. RUN 3
Temperature= 35C
Time= 45minutes
Speed= 3 (996.9rpm)

WEIGHT
OF
PASTE
KNEADING
TIME
SPEED VOLUME
OF
WATER
ADDED
TEMPERATURE
OF WATER
ADDED
OBSERVATION
300g 2 1 -
67

2 - -
7 3 - Paste becomes
soft
2 - - The paste
becomes smooth
and uniform
7 3 50ml 25C
away from the
cake
7 3 50ml 25C
2 - - The colour
changes from
chocolate to milk
chocolate
8 3 100ml 35C The fat melts and
its set free from
the cake.
2 - -
8 3 100ml 35C
2 -
8 3 The mixture
becomes soft and
light

Yield = 24.7%

d. RUN 4
Temperature= 45C
Time= 45minutes
Speed= 3 (996.9rpm)

WEIGHT
OF
PASTE
KNEADING
TIME
SPEED VOLUME
OF
WATER
ADDED
TEMPERATURE
OF WATER
ADDED
OBSERVATION
300g 2 1 -
2 - -
7 3 - Paste becomes
soft
68

2 - - The paste
becomes smooth
and uniform
7 3 50ml 25C
away from the
cake
7 3 50ml 25C
2 - - The colour
changes from
chocolate to milk
chocolate
its set free from
the cake.
2 - -
8 3 100ml 45C
2 -
8 3 The mixture
becomes soft and
light

Yield = 29.9%

e. RUN 5
Temperature= 35C
Time= 30minutes
Speed= 5 (1123rpm)

WEIGHT
OF
PASTE
KNEADING
TIME
SPEED VOLUME
OF
WATER
ADDED
TEMPERATURE
OF WATER
ADDED
OBSERVATION
300g 2 1 -
2 - -
soft
2 - - The paste
becomes smooth
and uniform
69

7 5 100ml 35C
away from the
cake
8 5 100ml 35C
2 - - The colour
changes from
chocolate to milk
chocolate
its set free from
the cake.

Weight of oil =90g
Yield = 30%

f. RUN 6
Temperature= 45C
Time= 30minutes
Speed= 5 (1123rpm)

WEIGHT
OF
PASTE
KNEADING
TIME
SPEED VOLUME
OF
WATER
ADDED
TEMPERATURE
OF WATER
ADDED
OBSERVATION
300g 2 1 -
2 - -
soft
2 - - The paste
becomes smooth
and uniform
7 5 100ml 45C
away from the
cake
8 5 100ml 45C
2 - - The colour
changes from
chocolate to milk
chocolate
70

its set free from
the cake.

Yield = 33.4%

g. RUN 7
Temperature= 35C
Time= 45minutes
Speed= 5 (1123rpm)

WEIGHT
OF
PASTE
KNEADING
TIME
SPEED VOLUME
OF
WATER
ADDED
TEMPERATURE
OF WATER
ADDED
OBSERVATION
300g 2 1 -
2 - -
7 5 - Paste becomes
soft
2 - - The paste
becomes smooth
and uniform
7 5 50ml 25C
away from the
cake
7 5 50ml 25C
2 - - The colour
changes from
chocolate to milk
chocolate
its set free from
the cake.
2 - -
8 5 100ml 35C
2 -
8 5 The mixture
becomes soft and
light

71

Yield = 26.3%

h. RUN 8

Temperature= 45C
Time= 45minutes
Speed= 5 (1123rpm)

WEIGHT
OF
PASTE
KNEADING
TIME
SPEED VOLUME
OF
WATER
ADDED
TEMPERATURE
OF WATER
ADDED
OBSERVATION
300g 2 1 -
2 - -
7 5 - Paste becomes
soft
2 - - The paste
becomes smooth
and uniform
7 5 50ml 25C
away from the
cake
7 5 50ml 25C
2 - - The colour
changes from
chocolate to milk
chocolate
its set free from
the cake.
2 - -
8 5 100ml 45C
2 -
8 5 The mixture
becomes soft and
light

72

Yield = 21.1%

2. EXPERIMENT 2- Determination of the effect of speed of kneading blade on yield.
i. RUN 9
Temperature= 45C
Time= 30minutes
Speed= 2 (912.3rpm)

WEIGHT
OF
PASTE
KNEADING
TIME
SPEED VOLUME
OF
WATER
ADDED
TEMPERATURE
OF WATER
ADDED
OBSERVATION
300g 2 1 -
2 - -
soft
2 - - The paste
becomes smooth
and uniform
7 2 100ml 45C
away from the
cake
8 2 100ml 45C
2 - - The colour
changes from
chocolate to milk
chocolate
its set free from
the cake.

Yield = 20.3%

j. RUN 10 (SAME AS RUN 2)
Temperature= 45C
Time= 30minutes
73

Speed= 3 (996.9rpm)

WEIGHT
OF
PASTE
KNEADING
TIME
SPEED VOLUME
OF
WATER
ADDED
TEMPERATURE
OF WATER
ADDED
OBSERVATION
300g 2 1 -
2 - -
soft
2 - - The paste
becomes smooth
and uniform
7 3 100ml 45C
away from the
cake
8 3 100ml 45C
2 - - The colour
changes from
chocolate to milk
chocolate
its set free from
the cake.

Yield = 29.4%

k. RUN 11
Temperature= 45C
Time= 30minutes
Speed= 4 (1018rpm)

WEIGHT
OF
PASTE
KNEADING
TIME
SPEED VOLUME
OF
WATER
ADDED
TEMPERATURE
OF WATER
ADDED
OBSERVATION
300g 2 1 -
2 - -
74

soft
2 - - The paste
becomes smooth
and uniform
7 4 100ml 45C
away from the
cake
8 4 100ml 45C
2 - - The colour
changes from
chocolate to milk
chocolate
its set free from
the cake.

Yield = 30.1%

l. RUN 12 (SAME AS RUN 6)
Temperature= 45C
Time= 30minutes
Speed= 5 (1123rpm)

WEIGHT
OF
PASTE
KNEADING
TIME
SPEED VOLUME
OF
WATER
ADDED
TEMPERATURE
OF WATER
ADDED
OBSERVATION
300g 2 1 -
2 - -
soft
2 - - The paste
becomes smooth
and uniform
7 5 100ml 45C
away from the
75

cake
8 5 100ml 45C
2 - - The colour
changes from
chocolate to milk
chocolate

Yield = 33.4%
3. EXPERIMENT 3- Determination of the effect of time of kneading on yield.
a. RUN 13 (SAME AS RUN 8)
Temperature= 45C
Time= 45minutes
Speed= 5 (1123rpm)
b. RUN 14 (SAME AS RUN 12)
Temperature= 45C
Time= 30 minutes
Speed= 5 (1123rpm)
c. RUN 15
Temperature= 45C
Time= 20 minutes
Speed= 5 (1123rpm)

WEIGHT
OF
PASTE
KNEADING
TIME
SPEED VOLUME
OF
WATER
ADDED
TEMPERATURE
OF WATER
ADDED
OBSERVATION
300g 2 1 -
2 - -
soft
2 - - The paste
becomes smooth
8 5 100ml 45C
76

2 - - The colour
changes from
chocolate to milk
chocolate
5 5 -

Yield = 13.2%

4. EXPERIMENT 4- Examining the effect of roasting on yield.
a. RUN 16(SAME AS RUN 12 and 14)
Temperature= 45C
Time= 30 minutes
Speed= 5 (1123rpm)

b. RUN 17 (Unroasted shea paste)
Temperature= 45C
Time= 30 minutes
Speed= 5 (1123rpm)
WEIGHT
OF
PASTE
KNEADING
TIME
SPEED VOLUME
OF
WATER
ADDED
TEMPERATURE
OF WATER
ADDED
OBSERVATION
300g 2 1 -
2 - -
7 5 50ml 25C
2 - -
7 5 100ml 45C
2 - - Paste becomes
soft
8 5 100ml 45C
2 - - The colour
changes from
chocolate to milk
chocolate
8 5 - The fat melts

Weight of container = 5.3
Weight of oil =8.4g
77

Yield = 2.8%

APPENDIX B
FORMULAE

1. Yield =
* 100%

2. Effect of factorial experiment =

3. The acid value is calculated mathematically as:
Acid Value =

Where,
X = volume of KOH required to neutralize the solution (ml)
M
1
= strength of KOH

W
1

4. The saponification value is calculated mathematically as:

Where,
Z = volume of HC
l
required to neutralize excess alkali (ml)
Z = (X Y) ml
X = titer value of HC
l
against oil and KOH after reflux (ml)
Y = titer value of HC
l
against KOH alone after reflux (ml)
M
1
= strength of HC
l

W
1
= weight of oil used (g).
78

5. Ester value = Saponification value Acid value

APPENDIX C
CALCULATIONS
1. FACTORIAL EXPERIMENTAL DESIGN
1.1. PERCENTAGE YIELD OF SHEA BUTTER
Yield =
* 100%
a. RUN 1
Temperature= 35C
Time= 30minutes
Speed= 3 (996.9rpm)
= 26.4%

b. RUN 2
Temperature= 45C
Time= 30minutes
Speed= 3 (996.9rpm)
= 29.4%

c. RUN 3
Temperature= 35C
Time= 45minutes
Speed= 3 (996.9rpm)
= 24.7%

d. RUN 4
Temperature= 45C
Time= 45minutes
Speed= 3 (996.9rpm)
= 29.9%

e. RUN 5
Temperature= 35C
Time= 30minutes
79

Speed= 5 (1123rpm)
= 30%

f. RUN 6
Temperature= 45C
Time= 30minutes
Speed= 5 (1123rpm)
= 33.4%

g. RUN 7
Temperature= 35C
Time= 45minutes
Speed= 5 (1123rpm)
= 26.3%

h. RUN 8
Temperature= 45C
Time= 45minutes
Speed= 5 (1123rpm)
= 21.1%

1.2. ABSOLUTE VALUE OF EFFECT OF FACTORS.
Effect of factorial experiment =

A=
( )
A (Temperature) = 1.6
B=
( )
B (Time) = 4.3
C=
( )
B (Speed) = 0.1
AB=
( )
AB (Temperature*Time) = 1.6
80

AC=
( )
AB (Temperature*Speed) = 2.5
BC=
( )
BC (Time*Speed) = 3.7

ABC=
( )
ABC (Temperature*Time*Speed) = 2.7
2. EFFECTS OF THE SPEED OF KNEADING BLADE ON SHEA BUTTER YIELD
2.1 YIELD (%)
i. RUN 9
Temperature= 45C
Time= 30minutes
Speed= 2 (912.3rpm)
= 20.3%

j. RUN 10 (SAME AS RUN 2)

k. RUN 11
Temperature= 45C
Time= 30minutes
Speed= 4 (1018rpm)
= 30.1%

l. RUN 12 (SAME AS RUN 6)

2.2 YIELD % USING MINITABS EQUATION
The correlation equation from the design software is as follows
Y=583.351-17.5324A-19.4948-0.550357C+0.583872AB+0.0174465AC+0.0189268BC-
0.000570975ABC
Hence using TEMPERATURE (A) = 45C, TIME (B) = 30MINUTES and C as follows
a. 912.3 rpm = 27.4
81

b. 996.9 rpm = 29.4
c. 1018 rpm = 31.4
d. 1123 rpm =33.4
3. EFFECTS OF KNEADING TIME ON SHEA BUTTER YIELD
a. RUN 13 (SAME AS RUN 8)

b. RUN 14 (SAME AS RUN 12)
c. RUN 15
Temperature= 45C
Time= 20 minutes
Speed= 5 (1123rpm)
= 13.2%

4. EXAMINING THE EFFECT OF ROASTING ON YIELD
a. RUN 16 (SAME AS RUN 12 and 14)

b. RUN 17 (Unroasted shea paste)
Temperature= 45C
Time= 30 minutes
Speed= 5 (1123rpm)
= 2.8%

5. ACID VALUE
Roasted
Acid Value =

Where, X = 21.94ml
M
1
= 0.1N
W
1
= 10g
Acid Value:

= 12.31

82

Unroasted
Acid Value =

Where, X = 9.47ml
M
1
= 0.1N
W
1
= 10g
Acid Value:

= 27.30

6. SAPONIFICATION VALUE
Unroasted

Where,
Z = (X Y) ml
X = 38ml
Y = 30.5ml
Z = 7.5ml
M
1
= 0.5N
W
1
= 1g

= 210.38
Roasted

Where,
Z = (X Y) ml
X = 38ml
Y = 32ml
Z = 6ml
83

M
1
= 0.5N
W
1
= 1g

= 168.3

7. ESTER VALUE
Roasted:Saponification value Ester value =(168.3-12.31) =155.99
Unroasted:Saponification value Ester value = (210.38-5.31) = 205.7
8. SPECIFIC GRAVITY
Roasted
Mass of oil=45.6g
Volume of gravity bottle=50cm
3
Density of oil= (45.6/50)g/cm
3
= 0.912g/cm
3
Density of water @20C=1g/cm
3
Specific gravity =0.912
Unroasted
Mass of oil=46.15g
Volume of gravity bottle=50cm
3
Density of oil= (46.15/50)g/cm
3
= 0.923g/cm
3
Density of water @20C=1g/cm
3
Specific gravity =0.923

84

APPENDIX D
GAS CHROMATOGRAPHY AND MASS SPECTROMETRY ANALYSIS
1. Roasted Shea butter sample.

Library Search Report

Data Path : C:\msdchem\1\methods\New ESSENTIAL OIL .M\
Data File : ROASTED aa.D
Acq On : 8 Apr 2013 15:49
Operator : MEJIDA/ACHEM
Sample : ROASTED SHEA BUTTER
Misc :
ALS Vial : 1 Sample Multiplier: 1

Search Libraries: C:\Database\NIST08.L Minimum Quality: 90

Unknown Spectrum: Apex
5 . 0 0 1 0 . 0 0 1 5 . 0 0 2 0 . 0 0 2 5 . 0 0 3 0 . 0 0 3 5 . 0 0 4 0 . 0 0 4 5 . 0 0
5 0 0 0 0 0
1 0 0 0 0 0 0
1 5 0 0 0 0 0
2 0 0 0 0 0 0
2 5 0 0 0 0 0
3 0 0 0 0 0 0
3 5 0 0 0 0 0
T ime -->
A b u n d a n c e
T I C: R O A S T E D a a . D \ d a t a . ms
1 1 . 4 6 1
2 5 . 6 0 9
2 9 . 3 1 8
2 9 . 4 1 9
2 9 . 5 5 7
2 9 . 6 3 6
2 9 . 9 7 3
3 0 . 0 7 0
85

Integration Events: ChemStation Integrator - events.e

Pk# RT Area% Library/ID Ref# CAS# Qual
_____________________________________________________________________________
1 11.464 1.42 C:\Database\NIST08.L
4-Heptafluorobutyryloxyhexadecane 205111 1000282-97-2 87
Cyclotetradecane 56570 000295-17-0 86
5-Tetradecene, (E)- 56582 041446-66-6 86

n-Hexadecanoic acid 102726 000057-10-3 99
Tetradecanoic acid 81211 000544-63-8 93

trans-13-Octadecenoic acid 122798 000693-71-0 80
cis-9-Hexadecenoic acid 100949 1000333-19-5 74
cis-13-Octadecenoic acid 122788 013126-39-1 70

Octadec-9-enoic acid 122782 1000190-13-7 96

cis-Vaccenic acid 122781 000506-17-2 98


Octadecanoic acid 124558 000057-11-4 98
Pentadecanoic acid 91826 001002-84-2 76


New ESSENTIAL OIL .M Tue Apr 09 10:19:59 2013

Area Percent Report

Data File : ROASTED aa.D
Acq On : 8 Apr 2013 15:49
Sample : ROASTED SHEA BUTTER
Misc :
86


Integration Parameters: events.e
Integrator: ChemStation

Method : C:\msdchem\1\methods\New ESSENTIAL OIL .M
Title :

Signal : TIC: ROASTED aa.D\data.ms

peak R.T. first max last PK peak corr. corr. % of
# min scan scan scan TY height area % max. total
--- ----- ----- ---- ---- --- ------- ------- ------ -------
1 11.461 1447 1464 1485 BB 463297 18117152 5.81% 1.424%
2 25.609 3868 3936 3969 BV 3 743677 85879352 27.55% 6.749%
3 29.318 4472 4584 4589 BV 7 2006929 311691724 100.00% 24.497%
4 29.419 4589 4602 4603 VV 6 2181559 100810660 32.34% 7.923%
5 29.557 4603 4626 4629 VV 4 2674981 216180981 69.36% 16.990%

6 29.636 4629 4640 4660 VV 6 2999522 222860904 71.50% 17.515%
7 29.973 4660 4699 4700 VV 4 1946264 169342674 54.33% 13.309%
8 30.070 4700 4716 4742 VB 2 2531550 147502169 47.32% 11.593%

Sum of corrected areas: 1272385617


87

2 0 4 0 6 0 8 0 1 0 0 1 2 0 1 4 0 1 6 0 1 8 0 2 0 0 2 2 0 2 4 0 2 6 0 2 8 0
0
1 0 0 0
2 0 0 0
3 0 0 0
4 0 0 0
5 0 0 0
6 0 0 0
7 0 0 0
8 0 0 0
9 0 0 0
m / z - - >
A b u n d a n c e
S c a n 1 4 6 4 ( 1 1 . 4 6 4 m i n ) : R O A S T E D a a . D \ d a t a . m s
5 5 . 0
8 3 . 0
1 1 1 . 0
1 9 6 . 0 1 6 8 . 1 1 4 0 . 0
2 0 4 0 6 0 8 0 1 0 0 1 2 0 1 4 0 1 6 0 1 8 0 2 0 0 2 2 0 2 4 0 2 6 0 2 8 0
0
1 0 0 0
2 0 0 0
3 0 0 0
4 0 0 0
5 0 0 0
6 0 0 0
7 0 0 0
8 0 0 0
9 0 0 0
m / z - - >
A b u n d a n c e
# 2 0 5 1 1 1 : 4 - H e p t a f l u o r o b u t y r y l o x y h e x a d e c a n e
5 5 . 0
8 3 . 0
2 9 . 0
1 1 1 . 0
1 3 5 . 0 1 6 9 . 0 2 2 4 . 0
2 0 0 . 0
2 8 2 . 0
88

4 0 6 0 8 0 1 0 0 1 2 0 1 4 0 1 6 0 1 8 0 2 0 0 2 2 0 2 4 0 2 6 0
0
1 0 0 0
2 0 0 0
3 0 0 0
4 0 0 0
5 0 0 0
6 0 0 0
7 0 0 0
8 0 0 0
9 0 0 0
m / z - - >
A b u n d a n c e
7 3 . 0
5 5 . 0
1 2 9 . 0
9 7 . 0 2 1 3 . 1
2 5 6 . 1 1 5 6 . 9
1 8 5 . 0
1 1 2 . 9
2 3 9 . 0
4 0 6 0 8 0 1 0 0 1 2 0 1 4 0 1 6 0 1 8 0 2 0 0 2 2 0 2 4 0 2 6 0
0
1 0 0 0
2 0 0 0
3 0 0 0
4 0 0 0
5 0 0 0
6 0 0 0
7 0 0 0
8 0 0 0
9 0 0 0
m / z - - >
A b u n d a n c e
# 1 0 2 7 2 6 : n - H e x a d e c a n o i c a c i d
6 0 . 0
4 3 . 0
1 2 9 . 0
8 3 . 0
2 1 3 . 0 2 5 6 . 0
1 5 7 . 0
1 8 5 . 0
1 0 1 . 0
2 3 9 . 0
20 40 60 80 100 120 140 160 180 200 220 240 260 280 300
0
2000
4000
6000
8000
m/ z-->
Abundanc e
Sc an 4584 (29.316 min): ROASTED aa.D\ data.ms
55.0
83.0
111.0
264.1
137.0
222.1 165.0
193.1 309.9
20 40 60 80 100 120 140 160 180 200 220 240 260 280 300
0
2000
4000
6000
8000
m/ z-->
Abundanc e
# 122798: trans-13-Oc tadec enoic ac id
55.0
83.0
111.0
29.0
264.0
137.0
165.0 222.0 193.0
89

2 0 4 0 6 0 8 0 1 0 0 1 2 0 1 4 0 1 6 0 1 8 0 2 0 0 2 2 0 2 4 0 2 6 0 2 8 0
0
1 0 0 0
2 0 0 0
3 0 0 0
4 0 0 0
5 0 0 0
6 0 0 0
7 0 0 0
8 0 0 0
9 0 0 0
m / z - - >
A b u n d a n c e
5 5 . 0
8 3 . 0
1 1 1 . 0
2 6 4 . 1
1 3 7 . 0
1 6 5 . 0 2 2 2 . 1 1 9 3 . 1 2 8 3 . 2 2 4 1 . 0
2 0 4 0 6 0 8 0 1 0 0 1 2 0 1 4 0 1 6 0 1 8 0 2 0 0 2 2 0 2 4 0 2 6 0 2 8 0
0
1 0 0 0
2 0 0 0
3 0 0 0
4 0 0 0
5 0 0 0
6 0 0 0
7 0 0 0
8 0 0 0
9 0 0 0
m / z - - >
A b u n d a n c e
# 1 2 2 7 8 2 : O c t a d e c - 9 - e n o i c a c i d
5 5 . 0
8 3 . 0
2 6 4 . 0
1 1 1 . 0
2 9 . 0
2 2 2 . 0 1 3 8 . 0
1 8 0 . 0
2 8 3 . 0
1 6 1 . 0 1 9 9 . 0 2 4 1 . 0
2 0 4 0 6 0 8 0 1 0 0 1 2 0 1 4 0 1 6 0 1 8 0 2 0 0 2 2 0 2 4 0 2 6 0 2 8 0
0
2 0 0 0
4 0 0 0
6 0 0 0
8 0 0 0
m / z - - >
A b u n d a n c e
5 5 . 0
8 3 . 0
1 1 1 . 0
2 6 4 . 1
1 3 7 . 0
1 6 5 . 1 2 2 1 . 1
1 9 3 . 0
2 8 4 . 1 2 4 1 . 0
2 0 4 0 6 0 8 0 1 0 0 1 2 0 1 4 0 1 6 0 1 8 0 2 0 0 2 2 0 2 4 0 2 6 0 2 8 0
0
2 0 0 0
4 0 0 0
6 0 0 0
8 0 0 0
m / z - - >
A b u n d a n c e
# 1 2 2 7 9 8 : t r a n s - 1 3 - O c t a d e c e n o i c a c i d
5 5 . 0
8 3 . 0
1 1 1 . 0
2 9 . 0
2 6 4 . 0
1 3 7 . 0
1 6 5 . 0 2 2 2 . 0
1 9 3 . 0 2 8 4 . 0
90

2 0 4 0 6 0 8 0 1 0 0 1 2 0 1 4 0 1 6 0 1 8 0 2 0 0 2 2 0 2 4 0 2 6 0 2 8 0
0
2 0 0 0
4 0 0 0
6 0 0 0
8 0 0 0
m / z - - >
A b u n d a n c e
5 5 . 0
8 3 . 0
1 1 1 . 0
2 6 4 . 1
1 3 7 . 0
1 6 5 . 0 2 2 2 . 1
1 9 3 . 0
2 8 4 . 2 2 4 1 . 8
2 0 4 0 6 0 8 0 1 0 0 1 2 0 1 4 0 1 6 0 1 8 0 2 0 0 2 2 0 2 4 0 2 6 0 2 8 0
0
2 0 0 0
4 0 0 0
6 0 0 0
8 0 0 0
m / z - - >
A b u n d a n c e
5 5 . 0
8 3 . 0
1 1 1 . 0
2 9 . 0
2 6 4 . 0
1 3 7 . 0
1 6 5 . 0 2 2 2 . 0
1 9 3 . 0 2 8 4 . 0
2 0 4 0 6 0 8 0 1 0 0 1 2 0 1 4 0 1 6 0 1 8 0 2 0 0 2 2 0 2 4 0 2 6 0 2 8 0
0
2 0 0 0
4 0 0 0
6 0 0 0
8 0 0 0
m / z - - >
A b u n d a n c e
7 3 . 0
1 2 9 . 0
9 7 . 0
2 8 4 . 1
1 8 5 . 0 2 4 1 . 1
5 3 . 0
1 5 7 . 0 2 1 3 . 0
2 6 4 . 1
2 0 4 0 6 0 8 0 1 0 0 1 2 0 1 4 0 1 6 0 1 8 0 2 0 0 2 2 0 2 4 0 2 6 0 2 8 0
0
2 0 0 0
4 0 0 0
6 0 0 0
8 0 0 0
m / z - - >
A b u n d a n c e
# 1 2 4 5 5 8 : O c t a d e c a n o i c a c i d
4 3 . 0
7 3 . 0
1 2 9 . 0
2 8 4 . 0
9 7 . 0
1 8 5 . 0
2 4 1 . 0
1 5 7 . 0 2 1 3 . 0 1 8 . 0
91

2 0 4 0 6 0 8 0 1 0 0 1 2 0 1 4 0 1 6 0 1 8 0 2 0 0 2 2 0 2 4 0 2 6 0 2 8 0
0
2 0 0 0
4 0 0 0
6 0 0 0
8 0 0 0
m / z - - >
A b u n d a n c e
7 3 . 0
1 2 9 . 0
2 8 4 . 1 9 7 . 0
2 4 1 . 1 1 8 5 . 0
5 3 . 0
1 5 7 . 1 2 1 3 . 0
2 6 4 . 0
2 0 4 0 6 0 8 0 1 0 0 1 2 0 1 4 0 1 6 0 1 8 0 2 0 0 2 2 0 2 4 0 2 6 0 2 8 0
0
2 0 0 0
4 0 0 0
6 0 0 0
8 0 0 0
m / z - - >
A b u n d a n c e
4 3 . 0 7 3 . 0
1 2 9 . 0
9 7 . 0 2 8 4 . 0
1 8 5 . 0
2 4 1 . 0
1 5 7 . 0
2 1 3 . 0
1 5 . 0
92

2. Unroasted Shea butter sample.

Library Search Report

Data File : UNROASTED bb.D
Acq On : 8 Apr 2013 16:43
Sample : UNROASTED SHEA BUTTER
Misc :

Search Libraries: C:\Database\NIST08.L Minimum Quality: 90

Unknown Spectrum: Apex
Integration Events: ChemStation Integrator - events.e

Pk# RT Area% Library/ID Ref# CAS# Qual
_____________________________________________________________________________
5-Tetradecene, (E)- 56582 041446-66-6 91
Cyclotetradecane 56570 000295-17-0 90
7-Tetradecene, (Z)- 56580 041446-60-0 83

Tetradecanoic acid 81211 000544-63-8 93
Pentadecanoic acid 91826 001002-84-2 87

5 . 0 0 1 0 . 0 0 1 5 . 0 0 2 0 . 0 0 2 5 . 0 0 3 0 . 0 0 3 5 . 0 0 4 0 . 0 0 4 5 . 0 0
2 0 0 0 0 0
4 0 0 0 0 0
6 0 0 0 0 0
8 0 0 0 0 0
1 0 0 0 0 0 0
1 2 0 0 0 0 0
1 4 0 0 0 0 0
1 6 0 0 0 0 0
1 8 0 0 0 0 0
2 0 0 0 0 0 0
2 2 0 0 0 0 0
2 4 0 0 0 0 0
T im e -->
A b u n d a n c e
T I C : U N R O A S T E D b b . D \ d a t a . m s
1 1 . 4 6 6
2 5 . 4 4 6
2 9 . 2 2 9
2 9 . 2 7 8
2 9 . 3 7 6
2 9 . 7 7 2
3 4 . 8 2 8
3 5 . 3 1 0
3 6 . 0 4 2
3 7 . 8 4 7
4 0 . 4 5 0
93


6-Octadecenoic acid 122783 1000336-66-8 91
6-Octadecenoic acid, (Z)- 122790 000593-39-5 90


9-Octadecenal, (Z)- 110397 002423-10-1 78
9-Oxabicyclo[6.1.0]nonane, cis- 11317 004925-71-7 50

3-Buten-1-ol, 3-methyl-2-methylene 3255 026431-13-0 35
(R)-(+)-3-Methylcyclopentanone 3233 006672-30-6 30
1,3-Dithiolane, 2-(28-norurs-12-en 213322 010153-89-6 27
-17-yl)-

Phthalic acid, decyl 2-ethylhexyl 200882 1000309-00-0 72
ester
Phthalic acid, 2-ethylhexyl tridec 208980 1000308-99-0 72
yl ester
Phthalic acid, 2-ethylhexyl hexyl 178604 1000309-02-5 64
ester

Urs-12-en-24-oic acid, 3-oxo-, met 210009 020475-86-9 95
hyl ester, (+)-
5(1H)-Azulenone, 2,4,6,7,8,8a-hexa 73264 006754-66-1 83
hydro-3,8-dimethyl-4-(1-methylethy
lidene)-, (8S-cis)-
Urs-12-en-3-ol, acetate, (3.beta.) 210017 000863-76-3 83

Squalene 198698 007683-64-9 99
Squalene 198700 007683-64-9 98
2,6,10,14,18,22-Tetracosahexaene, 198717 000111-02-4 98
2,6,10,15,19,23-hexamethyl-, (all-
E)-

Area Percent Report

Data File : UNROASTED bb.D
94

Acq On : 8 Apr 2013 16:43
Sample : UNROASTED SHEA BUTTER
Misc :

Integration Parameters: events.e
Integrator: ChemStation

Method : C:\msdchem\1\methods\New ESSENTIAL OIL .M
Title :

Signal : TIC: UNROASTED bb.D\data.ms

peak R.T. first max last PK peak corr. corr. % of
# min scan scan scan TY height area % max. total
--- ----- ----- ---- ---- --- ------- ------- ------ -------
1 11.466 1445 1464 1490 BB 2 412860 17115362 8.80% 2.728%
2 25.446 3866 3908 3967 BB 3 372878 37280496 19.18% 5.943%
3 29.229 4465 4569 4570 BV 3 1402998 194418026 100.00% 30.991%
4 29.278 4570 4577 4580 VV 4 1570880 51980889 26.74% 8.286%
5 29.376 4580 4594 4614 VV 7 1845024 128084479 65.88% 20.417%

6 29.772 4614 4664 4697 VV 4 1365834 144321756 74.23% 23.005%
7 34.828 5511 5547 5581 BB 5 133662 8944824 4.60% 1.426%
8 35.310 5605 5631 5649 BV 8 104797 5348171 2.75% 0.853%
9 36.042 5737 5759 5791 BV 2 628206 30143835 15.50% 4.805%
10 37.847 6072 6075 6092 VV 2 45750 1952070 1.00% 0.311%

11 40.450 6508 6530 6552 BV 3 163339 7752389 3.99% 1.236%

Sum of corrected areas: 627342297


95

2 0 3 0 4 0 5 0 6 0 7 0 8 0 9 01 0 01 1 01 2 01 3 01 4 01 5 01 6 01 7 01 8 01 9 02 0 0
0
1 0 0 0
2 0 0 0
3 0 0 0
4 0 0 0
5 0 0 0
6 0 0 0
7 0 0 0
8 0 0 0
9 0 0 0
m / z - - >
A b u n d a n c e
S c a n 1 4 6 4 ( 1 1 . 4 6 4 m i n ) : U N R O A S T E D b b . D \ d a t a . m s
5 5 . 0
6 9 . 0
8 3 . 0
9 7 . 0
1 1 1 . 0
1 2 5 . 0
1 3 9 . 9 1 5 4 . 0 1 9 6 . 0 1 6 7 . 8
2 0 3 0 4 0 5 0 6 0 7 0 8 0 9 01 0 01 1 01 2 01 3 01 4 01 5 01 6 01 7 01 8 01 9 02 0 0
0
1 0 0 0
2 0 0 0
3 0 0 0
4 0 0 0
5 0 0 0
6 0 0 0
7 0 0 0
8 0 0 0
9 0 0 0
m / z - - >
A b u n d a n c e
# 5 6 5 8 2 : 5 - T e t r a d e c e n e , ( E ) -
5 5 . 0
6 9 . 0
4 1 . 0
8 3 . 0
9 7 . 0
2 7 . 0
1 1 1 . 0
1 9 6 . 0
1 2 5 . 0
1 3 9 . 0 1 6 8 . 0 1 5 3 . 0
4 0 6 0 8 0 1 0 0 1 2 0 1 4 0 1 6 0 1 8 0 2 0 0 2 2 0 2 4 0 2 6 0
0
1 0 0 0
2 0 0 0
3 0 0 0
4 0 0 0
5 0 0 0
6 0 0 0
7 0 0 0
8 0 0 0
9 0 0 0
m / z - - >
A b u n d a n c e
7 3 . 0
5 5 . 0
1 2 9 . 0
2 1 3 . 0 9 7 . 0
2 5 6 . 1
1 8 4 . 9 1 5 6 . 9
1 1 3 . 0
2 3 8 . 8
4 0 6 0 8 0 1 0 0 1 2 0 1 4 0 1 6 0 1 8 0 2 0 0 2 2 0 2 4 0 2 6 0
0
1 0 0 0
2 0 0 0
3 0 0 0
4 0 0 0
5 0 0 0
6 0 0 0
7 0 0 0
8 0 0 0
9 0 0 0
m / z - - >
A b u n d a n c e
# 1 0 2 7 2 6 : n - H e x a d e c a n o i c a c i d
6 0 . 0
4 3 . 0
1 2 9 . 0
8 3 . 0
2 1 3 . 0 2 5 6 . 0
1 5 7 . 0
1 8 5 . 0
1 0 1 . 0
2 3 9 . 0
96

2 0 4 0 6 0 8 0 1 0 0 1 2 0 1 4 0 1 6 0 1 8 0 2 0 0 2 2 0 2 4 0 2 6 0 2 8 0
0
2 0 0 0
4 0 0 0
6 0 0 0
8 0 0 0
m / z - - >
A b u n d a n c e
5 5 . 0
8 3 . 0
1 1 1 . 0
2 6 4 . 1
1 3 6 . 9
1 6 5 . 0 2 2 0 . 1 1 9 3 . 0
2 8 4 . 2 2 4 0 . 8
2 0 4 0 6 0 8 0 1 0 0 1 2 0 1 4 0 1 6 0 1 8 0 2 0 0 2 2 0 2 4 0 2 6 0 2 8 0
0
2 0 0 0
4 0 0 0
6 0 0 0
8 0 0 0
m / z - - >
A b u n d a n c e
5 5 . 0
8 3 . 0
1 1 1 . 0
2 9 . 0
2 6 4 . 0
1 3 7 . 0
1 6 5 . 0 2 2 2 . 0
1 9 3 . 0
2 8 4 . 0
2 0 4 0 6 0 8 0 1 0 0 1 2 0 1 4 0 1 6 0 1 8 0 2 0 0 2 2 0 2 4 0 2 6 0 2 8 0
0
2 0 0 0
4 0 0 0
6 0 0 0
8 0 0 0
m / z - - >
A b u n d a n c e
5 5 . 0
8 3 . 0
1 1 1 . 0
2 6 4 . 1
1 3 7 . 0
2 2 2 . 0 1 6 5 . 0
1 9 3 . 1 2 8 4 . 1
2 0 4 0 6 0 8 0 1 0 0 1 2 0 1 4 0 1 6 0 1 8 0 2 0 0 2 2 0 2 4 0 2 6 0 2 8 0
0
2 0 0 0
4 0 0 0
6 0 0 0
8 0 0 0
m / z - - >
A b u n d a n c e
# 1 2 2 7 8 8 : c i s - 1 3 - O c t a d e c e n o i c a c i d
5 5 . 0
8 3 . 0
1 1 1 . 0
2 9 . 0 2 6 4 . 0
1 3 7 . 0
1 6 5 . 0 2 2 2 . 0
1 9 3 . 0
2 8 4 . 0
97

2 0 4 0 6 0 8 0 1 0 0 1 2 0 1 4 0 1 6 0 1 8 0 2 0 0 2 2 0 2 4 0 2 6 0 2 8 0
0
2 0 0 0
4 0 0 0
6 0 0 0
8 0 0 0
m / z - - >
A b u n d a n c e
5 5 . 0
8 3 . 0
1 1 1 . 0
2 6 4 . 1
1 3 7 . 0
2 2 2 . 1 1 6 5 . 0 1 9 3 . 1
2 8 3 . 9 2 4 2 . 2
2 0 4 0 6 0 8 0 1 0 0 1 2 0 1 4 0 1 6 0 1 8 0 2 0 0 2 2 0 2 4 0 2 6 0 2 8 0
0
2 0 0 0
4 0 0 0
6 0 0 0
8 0 0 0
m / z - - >
A b u n d a n c e
# 1 2 2 7 8 1 : c i s - V a c c e n i c a c i d
5 5 . 0
8 3 . 0
1 1 1 . 0
2 9 . 0
2 6 4 . 0
1 3 7 . 0
1 6 5 . 0 2 2 2 . 0
1 9 3 . 0
2 8 4 . 0
2 0 4 0 6 0 8 0 1 0 0 1 2 0 1 4 0 1 6 0 1 8 0 2 0 0 2 2 0 2 4 0 2 6 0 2 8 0
0
2 0 0 0
4 0 0 0
6 0 0 0
8 0 0 0
m / z - - >
A b u n d a n c e
7 3 . 0
1 2 9 . 0
9 7 . 0
2 8 4 . 1 1 8 5 . 0 2 4 1 . 1
5 3 . 0
1 5 7 . 0 2 1 3 . 0
2 6 4 . 0
2 0 4 0 6 0 8 0 1 0 0 1 2 0 1 4 0 1 6 0 1 8 0 2 0 0 2 2 0 2 4 0 2 6 0 2 8 0
0
2 0 0 0
4 0 0 0
6 0 0 0
8 0 0 0
m / z - - >
A b u n d a n c e
4 3 . 0 7 3 . 0
1 2 9 . 0
9 7 . 0 2 8 4 . 0
1 8 5 . 0
2 4 1 . 0
1 5 7 . 0 2 1 3 . 0
1 5 . 0
98

5 0 1 0 0 1 5 0 2 0 0 2 5 0 3 0 0 3 5 0 4 0 0 4 5 0
0
1 0 0 0
2 0 0 0
3 0 0 0
4 0 0 0
5 0 0 0
6 0 0 0
7 0 0 0
8 0 0 0
9 0 0 0
m / z - - >
A b u n d a n c e
5 5 . 0
1 2 9 . 0
9 5 . 0
1 8 5 . 0
4 5 3 . 2
3 9 3 . 1 2 4 1 . 0
2 9 5 . 3
3 5 5 . 2
5 0 1 0 0 1 5 0 2 0 0 2 5 0 3 0 0 3 5 0 4 0 0 4 5 0
0
1 0 0 0
2 0 0 0
3 0 0 0
4 0 0 0
5 0 0 0
6 0 0 0
7 0 0 0
8 0 0 0
9 0 0 0
m / z - - >
A b u n d a n c e
# 1 1 0 3 9 7 : 9 - O c t a d e c e n a l , ( Z ) -
5 5 . 0
9 8 . 0
1 3 5 . 0
2 4 8 . 0
1 8 2 . 0
5 0 1 0 0 1 5 0 2 0 0 2 5 0 3 0 0 3 5 0 4 0 0 4 5 0
0
1 0 0 0
2 0 0 0
3 0 0 0
4 0 0 0
5 0 0 0
6 0 0 0
7 0 0 0
8 0 0 0
9 0 0 0
m / z - - >
A b u n d a n c e
5 5 . 0
1 2 8 . 9
9 4 . 9
4 5 3 . 2
1 8 4 . 9 3 9 3 . 2
2 9 7 . 1 2 4 1 . 2
3 5 5 . 1
5 0 1 0 0 1 5 0 2 0 0 2 5 0 3 0 0 3 5 0 4 0 0 4 5 0
0
1 0 0 0
2 0 0 0
3 0 0 0
4 0 0 0
5 0 0 0
6 0 0 0
7 0 0 0
8 0 0 0
9 0 0 0
m / z - - >
A b u n d a n c e
# 3 7 8 0 7 : 1 - C y c l o p e n t e n - 3 - o n e , 1 - ( e t h o x y c a r b o n y l o x y ) -
2 9 . 0
6 9 . 0
1 7 0 . 0 1 2 6 . 0
99

5 0 1 0 0 1 5 0 2 0 0 2 5 0 3 0 0 3 5 0 4 0 0 4 5 0
0
1 0 0 0
2 0 0 0
3 0 0 0
4 0 0 0
5 0 0 0
6 0 0 0
7 0 0 0
8 0 0 0
9 0 0 0
m / z - - >
A b u n d a n c e
1 4 8 . 9
5 7 . 0
1 0 4 . 0
2 7 9 . 0
1 8 5 . 2 4 5 3 . 2 3 9 2 . 9 2 4 1 . 1
5 0 1 0 0 1 5 0 2 0 0 2 5 0 3 0 0 3 5 0 4 0 0 4 5 0
0
1 0 0 0
2 0 0 0
3 0 0 0
4 0 0 0
5 0 0 0
6 0 0 0
7 0 0 0
8 0 0 0
9 0 0 0
m / z - - >
A b u n d a n c e
# 2 0 0 8 8 2 : P h t h a l i c a c i d , d e c y l 2 - e t h y l h e x y l e s t e r
1 4 9 . 0
5 7 . 0
3 0 7 . 0
1 0 4 . 0
2 6 . 0

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