UPGRADE OF THE INDIGENOUS PRODUCTION OF SHEA BUTTER

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DEPARTMENT OF CHEMICAL ENGINEERING

COVENANT UNIVERSITY, OTA, OGUN STATE,

NIGERIA

UPGRADE OF THE INDIGENOUS METHOD OF

PRODUCTION OF SHEA BUTTER

A FINAL YEAR RESEARCH PROJECT

BY

AJAYI ADEBAYO EBENEZER

08CF07626

JUNE 2013

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UPGRADE OF THE INDIGENOUS METHOD OF

PRODUCTION OF SHEA BUTTER

A FINAL YEAR RESEARCH PROJECT

Presented to

College of Science and Technology

School of Engineering

The Department of Chemical Engineering

By

AJAYI ADEBAYO EBENEZER

MATRIC. NO: 08CF07626

In Partial Fulfillment of the requirements for the Degree Bachelor of Engineering in Chemical

Engineering

COVENANT UNIVERSITY, OTA

JUNE, 2013.

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CERTIFICATION

I hereby declare that the contained report on “Upgrade of the indigenous method production of

shea butter” was researched, and the results thoroughly analyzed, under the supervision of the

project supervisor and approved having satisfied the partial requirements for the award of

Bachelor of Engineering in Chemical Engineering (B.Eng.), Covenant University, Ota.

AJAYI ADEBAYO EBENEZER Date

PROF.F.K. HYMORE Date

Supervisor

PROF.F.K. HYMORE Date

Head of Department

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DEDICATION

I dedicate this work to The Almighty God, who is greater than the greatest, and also to my caring

and wonderful parents Mr. & Mrs. Ajayi who always want the best for me. Glory!

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ACKNOWLEDGEMENT

Firstly, I would like to acknowledge my project supervisor, Professor F.K. Hymore for his

support and guidance in the course of this project.

I would also want to sincerely appreciate the teaching staff and the laboratory technologists of

the Department of Chemical Engineering for taking interest in my project. I also want to

appreciate some of my friends: Olopade Kate, Ofure Egbele, Amoo Kehinde and Adetayo

Adeniji. for their support throughout the course of the project work.

AJAYI ADEBAYO EBENEZER.

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ABSTRACT

In this study, the upgrade of the indigenous method of production of shea butter was

investigated. This was achieved by the use of Electric Food processor for the kneading process.

The effects of Time, Temperature and Speed on the extract of the shea butter were investigated

by using a 23

factorial plan. The effect of roasting of the shea butter seeds before extraction was

also investigated. The extracted shea butter was analyzed for its fatty acid distribution using a

Gas Chromatography-Mass Spectrometer and some physic-chemical properties.

Higher extraction temperature and shorter time increased the yield of shea butter. The effect

however depended on the level of other factors. Kneading time had the most significant effect on

the yield. Roasting the shea butter seeds before extraction gave higher yield (33.4%) compared

with 2.8% for non roasting. Although the physico-chemical properties of the shea butter from

both roasted and unroasted seeds were similar, there was still some significant difference

between their acid values- 12.3 for roasted and 5.3 for non roasted, and in their ester values-

155.99 for roasted and 205.07 for non roasted. The chromatographic analysis indicated lower

fractions of the oleic acid (7.92% and 0 % in roasted and unroasted seed respectively) and stearic

acid (24.9% and 23.01% in roasted and unroasted seed respectively). This contrasts with

literature values (Oleic acid 46.4% and Stearic acid 41.5%). Further studies are needed to

confirm if these differences may be attributed to regional varieties of the shea nuts.

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TABLE OF CONTENTS

CONTENTS PAGE

TITLE PAGE i

DECLARATION iii

DEDICATION iv

ACKNOWLEGDEMENT v

ABSTRACT vi

TABLE OF CONTENTS vii

LIST OF TABLES xi

LIST OF FIGURES xii

CHAPTER ONE

INTRODUCTION 1

1.1 Research background 1

1.2 Problem statement 2

1.3 Aims and objectives of the study 2

1.4 Method and scope 3

1.5 Relevance of research to the society 3

CHAPTER TWO

LITERATURE REVIEW 4

2.1 The shea butter tree 4

2.2 Overview of shea butter 7

2.2.1 Shea butter 7

2.2.2 Composition of shea butter 9

2.2.2.1 Free fatty acids 9

2.2.2.2 Phenolics 10

2.2.3 Properties of shea butter 10

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2.2.4 Importance and uses of shea butter 11

2.2.4.1 Traditional use of shea butter in africa 11

2.2.4.2 Benefit of using shea butter 12

2.3 Shea nut processing 13

2.3.1 Drying of kernels 13

2.3.1.1 Removal of pulp 13

2.3.1.2 Boiling 13

2.3.1.3 Drying of nuts 14

2.3.1.4 Removal of shell 14

2.3.1.5 Drying kernels 14

2.3.2 Shea butter extraction 15

2.3.2.1 Traditional manual extraction 16

2.3.2.2 Chemical (solvent) extraction 19

2.3.2.3 Soxhlet extractor 20

2.3.2.4 Screw press 21

2.3.2.5 Centrifuge 21

2.3.2.6 Food processor/dough kneader as a substitute for mixing and kneading steps 23

2.4 Quality control 24

2.4.1 Unsaps 24

2.4.2 Impurities 25

2.4.3 Scent 25

2.4.4 Shelf-life 25

2.4.5 Variability 25

2.5 Factorial experimental design 26

2.5.1 Introduction 26

2.5.2 Experiments with factors each at two levels 26

2.6 Economic analysis for developing an improved shea butter industry. 27

2.6.1 Nigeria and shea butter 28

2.6.2 The state of shea nut in Nigeria 28

CHAPTER THREE

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MATERIALS AND METHODS 29

3.1 Raw materials and reagents 29

3.2 Instrumentation and equipment 29

3.3 Methods 30

3.3.1 Seed preparation 30

3.3.2 Traditional method upgrade 31

3.3.2.1 Experiment 1- determining the major factor affecting the production of shea butter 33

3.3.2.2 Experiment 2- determination of the effect of speed of kneading blade on yield. 39

3.3.2.3 Experiment 3-determination of the effect of time of kneading on yield. 39

3.3.2.4 Examining the effect of roasting on yield. 40

3.3.3 Determination of the physico-chemical properties 40

3.3.3.1 Acid value 40

3.3.3.2 Refractive index 41

3.3.3.3 Saponification value 42

3.3.3.4 Ester value 43

3.3.3.5 Specific gravity 43

3.3.4 GC analysis of fatty acid composition 43

3.3.4.1 Transesterification of fatty acids to fatty acid methyl esters (fames) 43

3.3.4.2 Identification of (fames) using gas chromatography with flame ionization detector

(gc-fid) 44

3.3.5 Determination of the speed in revolution per minute of the kneading blade. 44

3.4 Safety precautions 45

CHAPTER FOUR

RESULTS AND DICUSSION OF RESULTS 46

4.1 Results 46

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4.1.1 Calibration of the speed of the kneading blade in revolution per minute 46

4.1.2 Determination of yield of oil 46

4.1.2.1 Factorial experimental design using manual method 46

4.1.2.2 Factorial experimental design using minitab 48

4.1.3 Effects of the speed of kneading blade on shea butter yield 50

4.1.4 Effects of kneading time on shea butter yield 51

4.1.5 Effects of roasting before kneading on shea butter yield 52

4.1.6 Physicochemical properties 53

4.1.7 Chromatographic analysis of free-fatty acid composition of shea butter 53

4.2 Discussion of results 54

4.2.1 Calibration of the speed of the kneading blade in revolution per minute 54

4.2.2 The factorial experimental design for the effects of various factors on the oil yield 54

4.2.3 The effects of the speed of kneading blade on shea butter yield. 56

4.2.4 The effect of kneading time on shea butter yield 56

4.2.5 The effect of roasting before kneading on shea butter yield 56

4.2.6 Physicochemical properties of shea butter oil 57

4.2.7 Chromatographic analysis of shea butter oil 58

CHAPTER FIVE 61

5.1 CONCLUSION 61

CHAPTER SIX 62

6.1 RECOMMENDATION 62

REFERENCES 65

APPENDIX A: EXPERIMENTAL RUNS 65

APPENDIX B: FORMULAE 77

APPENDIX C: CALCULATIONS 78

APPENDIX D: GAS CHROMATOGRAPHY & MASS SPECTROMETRY ANALYSIS 83

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LIST OF TABLES

TABLE TITLE PAGE

2.1 Utilization of the Shea tree 5

2.2 Fatty acid variation in shea butter 10

2.3 Schematic overview of processing steps of getting nuts ready for storage 15

2.4 Schematic overview of processing steps butter extraction

2.5 Two-level 3-factor full-factorial experiment patterns 26

4.1 Kneading speed in revolutions per minute 46

4.2 Manual Factorial experimental results 47

4.3 Minitab Factorial experimental results 48

4.4 Effects of kneading speed on yield

4.5 Effects of kneading time on yield 51

4.6 Effects of roasting on yield 52

4.7 Physicochemical properties of shea butter yield 53

4.8 Fatty acid variation in roasted shea butter 53

4.9 Fatty acid variation in roasted shea butter 54

4.10 Comparison of Physiochemical properties of shea butter extracted with literature

values extracted 57

4.11 Comparison of the five principal fatty acids composition of shea butter 59

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LIST OF FIGURES

FIGURE TITLE PAGE

2.1 Agricultural parkland, with shea trees 8

2.2 Shea fruit 8

2.3 Shea Nut 8

2.4 Shea Butter 9

2.5 Steps of processing freshly picked nuts into dried kernels 13

2.6 Steps of processing shea kernels into shea butter 15

2.7 Nut Crushing 16

2.8 Roasting of shea nuts 16

2.9 Creamy mass separating from brown water 17

2.10 Boiling/Dehydration 18

2.11 Shea butter extraction diagram 23

2.12 Electric Food processor 24

3.1 Block Flow diagram of seed preparation 30

3.2 Block Flow diagram of traditional upgrade process 31

3.3 Electric Oven 31

3.4 Hand Mixer 32

3.5 Electric water bath 32

3.6 Heating Mantle 33

4.1 Main Effects for shea butter yield (fitted means) 47

4.2 Interaction plot for shea butter yield (fitted means) 48

4.3 Pareto Chart of the Effects of shea butter 49

4.4 Effects of kneading speed on yield 50

4.5 Effects of kneading time on yield 51

4.6 Effects of roasting of shea paste before kneading 52

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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 women‟s 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 women‟s

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 30-35°C.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 Cleopatra‟s 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 oil‟s, 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 α-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 butter‟s 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

butter‟s 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, α-amyrin,

25

and β-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.

26

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.

27

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

28

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 2.7–Nut 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 120°C will lead to maximum

butter extraction without the kernel getting burnt. Butter extracted from burned kernel bits will

become black and can‟t be sold on the market.

FIGURE 2.8–Roasting of shea nuts

29

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.

30

FIGURE 2.10–Boiling/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

31

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 (40°C-60°C), 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.

32

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 40°C-60°C. 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

33

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

34

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.

35

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,

36

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.

37

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.

38

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 2n 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

39

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

40

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 18th

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 country‟s 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.

41

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.

42

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

43

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 105-115°C 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

44

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.

45

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 (23) 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.

46

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 35°C 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.







47




Experimental Run 3





After the second and third rest, 50ml of water at room temperature was added to

the paste.



Water at 35°C was added at a volume of 100ml after the fourth and fifthrest.










Experimental Run 4






the paste.

48



Water at 45°C was added at a volume of 100ml after the fourth and fifth rest.










Experimental Run 5









second rest.









49


Experimental Run 6









second rest.










Experimental Run 7






the paste.



50











Experimental Run 8






the paste.













51


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.

52

Experimental Run

The experiment was carried out as experiment 3.3.2.2 using speed 5 and

temperature of water added at 45°C 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.

53

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)

M1 = strength of KOH

W1 = 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.

54

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)

55

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)

M1 = strength of HCL



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 20°C

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.

56

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 0.25μm, 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 10°C / 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.

57

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.

58

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 (- =35°C, + = 45°C)

B=Time (- =30mins, + = 45mins)

C= Speed (- =996.9rpm, + = 1123rpm

59

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 Y1

Y2 ̅

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)

4535

30

29

28

27

26

4530

53

30

29

28

27

26

TEMPERATURE

Mea

n

TIME

SPEED

Main Effects Plot for YIELDFitted Means

60

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

4530 53

30.0

27.5

25.0

30.0

27.5

25.0

T EMPERA T URE

T IME

SPEED

35

45

TEMPERATURE

30

45

TIME

Interaction Plot for YIELDFitted Means

61

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

EFFE

CT

TERM

FACTOR NAME A TEMPERATURE B TIME C SPEED

Lenth's PSE= 3.75

62

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 = 45°C 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 = -0.0003x2 + 0.7193x - 367.0121 R² = 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= 45°C TIME=30mins

63

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 = 45°C 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 = -0.1136x2 + 7.7x - 95.36 R² = 1

10

15

20

25

30

35

40

20 25 30 35 40 45 50

Y

I

E

L

D

(

%)

KNEADING TIME (minutes)

TEMP= 45°C SPEED = 1123rpm

64

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= 45°C TIME=30mins

65

TABLE 4.7 Physicochemical properties of Shea butter yield

Oil Sample Acid value Saponification

Value

Ester

Value

Refractive

index

Specific

Gravity

@20°C

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

66

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 23) 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.

67

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

68

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.

69

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.

70

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.

71

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

72

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.

73

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.

74

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.

75

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

76

15. Shea Butter Extraction in Mali, Appropriate Technology Bulletin No 6

Appropriate Technology International, 1985

16. ADEME AGRICE. 2001. Tensioactifs et oléagineux, Etude sur les matières premières

oléagineuses disponibles sur le marché européen, 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 société 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, Université de Ngaoundéré, 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

http://www.alliedpublishers.com/BookDetails.aspx?BookId=228

http://www.alliedpublishers.com/BookDetails.aspx?BookId=228

77

APPENDIX A

EXPERIMENTAL RUNS

1. EXPERIMENT 1- Determining the major factor affecting the production of shea

butter

a. RUN 1

Temperature= 35°C

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 25°C Paste becomes

soft

2 - - The paste

becomes smooth

and uniform

7 3 100ml 35°C

2 - - The fat breaks

away from the

cake

8 3 100ml 35°C

2 - - The colour

changes from

chocolate to milk

chocolate

8 3 - The fat melts and

it‟s set free from

the cake.

Weight of container = 10.2g

Weight of container + oil =89.4g

Weight of oil =79.2g

Yield = 26.4%

78

b. RUN 2

Temperature= 45°C

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 45°C


away from the

cake

8 3 100ml 45°C

2 - - The colour

changes from

chocolate to milk

chocolate



the cake.




Yield = 29.4%

c. RUN 3

Temperature= 35°C

Time= 45minutes

Speed= 3 (996.9rpm)

WEIGHT

OF

PASTE

KNEADING

TIME

SPEED VOLUME

OF

WATER

ADDED

TEMPERATURE

OF WATER

ADDED

OBSERVATION

300g 2 1 -

79

2 - -

7 3 - Paste becomes

soft

2 - - The paste

becomes smooth

and uniform

7 3 50ml 25°C


away from the

cake

7 3 50ml 25°C

2 - - The colour

changes from

chocolate to milk

chocolate

8 3 100ml 35°C The fat melts and


the cake.

2 - -

8 3 100ml 35°C

2 -

8 3 The mixture

becomes soft and

light




Yield = 24.7%

d. RUN 4

Temperature= 45°C

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

80

2 - - The paste

becomes smooth

and uniform

7 3 50ml 25°C


away from the

cake

7 3 50ml 25°C

2 - - The colour

changes from

chocolate to milk

chocolate



the cake.

2 - -

8 3 100ml 45°C

2 -

8 3 The mixture

becomes soft and

light




Yield = 29.9%

e. RUN 5

Temperature= 35°C

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

81

7 5 100ml 35°C


away from the

cake

8 5 100ml 35°C

2 - - The colour

changes from

chocolate to milk

chocolate



the cake.



Weight of oil =90g

Yield = 30%

f. RUN 6

Temperature= 45°C

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 45°C


away from the

cake

8 5 100ml 45°C

2 - - The colour

changes from

chocolate to milk

chocolate


82


the cake.




Yield = 33.4%

g. RUN 7

Temperature= 35°C

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 25°C


away from the

cake

7 5 50ml 25°C

2 - - The colour

changes from

chocolate to milk

chocolate



the cake.

2 - -

8 5 100ml 35°C

2 -

8 5 The mixture

becomes soft and

light

83




Yield = 26.3%

h. RUN 8

Temperature= 45°C

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 25°C


away from the

cake

7 5 50ml 25°C

2 - - The colour

changes from

chocolate to milk

chocolate



the cake.

2 - -

8 5 100ml 45°C

2 -

8 5 The mixture

becomes soft and

light



84


Yield = 21.1%

2. EXPERIMENT 2- Determination of the effect of speed of kneading blade on yield.

i. RUN 9

Temperature= 45°C

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 45°C


away from the

cake

8 2 100ml 45°C

2 - - The colour

changes from

chocolate to milk

chocolate



the cake.




Yield = 20.3%

j. RUN 10 (SAME AS RUN 2)

Temperature= 45°C

Time= 30minutes

85

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 45°C


away from the

cake

8 3 100ml 45°C

2 - - The colour

changes from

chocolate to milk

chocolate



the cake.




Yield = 29.4%

k. RUN 11

Temperature= 45°C

Time= 30minutes

Speed= 4 (1018rpm)

WEIGHT

OF

PASTE

KNEADING

TIME

SPEED VOLUME

OF

WATER

ADDED

TEMPERATURE

OF WATER

ADDED

OBSERVATION

300g 2 1 -

2 - -

86


soft

2 - - The paste

becomes smooth

and uniform

7 4 100ml 45°C


away from the

cake

8 4 100ml 45°C

2 - - The colour

changes from

chocolate to milk

chocolate



the cake.




Yield = 30.1%

l. RUN 12 (SAME AS RUN 6)

Temperature= 45°C

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 45°C


away from the

87

cake

8 5 100ml 45°C

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= 45°C

Time= 45minutes

Speed= 5 (1123rpm)

b. RUN 14 (SAME AS RUN 12)

Temperature= 45°C

Time= 30 minutes

Speed= 5 (1123rpm)

c. RUN 15

Temperature= 45°C

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 45°C

88

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= 45°C

Time= 30 minutes

Speed= 5 (1123rpm)

b. RUN 17 (Unroasted shea paste)

Temperature= 45°C

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 25°C

2 - -

7 5 100ml 45°C

2 - - Paste becomes

soft

8 5 100ml 45°C

2 - - The colour

changes from

chocolate to milk

chocolate

8 5 - The fat melts

Weight of container = 5.3


Weight of oil =8.4g

89

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)

M1 = strength of KOH



4. The saponification value is calculated mathematically as:


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)

M1 = strength of HCl

W1 = weight of oil used (g).

90

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= 35°C

Time= 30minutes

Speed= 3 (996.9rpm)

= 26.4%

b. RUN 2

Temperature= 45°C

Time= 30minutes

Speed= 3 (996.9rpm)

= 29.4%

c. RUN 3

Temperature= 35°C

Time= 45minutes

Speed= 3 (996.9rpm)

= 24.7%

d. RUN 4

Temperature= 45°C

Time= 45minutes

Speed= 3 (996.9rpm)

= 29.9%

e. RUN 5

Temperature= 35°C

Time= 30minutes

91

Speed= 5 (1123rpm)

= 30%

f. RUN 6

Temperature= 45°C

Time= 30minutes

Speed= 5 (1123rpm)

= 33.4%

g. RUN 7

Temperature= 35°C

Time= 45minutes

Speed= 5 (1123rpm)

= 26.3%

h. RUN 8

Temperature= 45°C

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│

92

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= 45°C

Time= 30minutes

Speed= 2 (912.3rpm)

= 20.3%

j. RUN 10 (SAME AS RUN 2)

k. RUN 11

Temperature= 45°C

Time= 30minutes

Speed= 4 (1018rpm)

= 30.1%

l. RUN 12 (SAME AS RUN 6)

2.2 YIELD % USING MINITAB’S 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) = 45°C, TIME (B) = 30MINUTES and C as follows

a. 912.3 rpm = 27.4

93

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= 45°C

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= 45°C

Time= 30 minutes

Speed= 5 (1123rpm)

= 2.8%

5. ACID VALUE

Roasted

Acid Value =

Where, X = 21.94ml

M1 = 0.1N

W1 = 10g

Acid Value:

= 12.31

94

Unroasted

Acid Value =

Where, X = 9.47ml

M1 = 0.1N

W1 = 10g

Acid Value:

= 27.30

6. SAPONIFICATION VALUE

Unroasted


Where,

Z = (X – Y) ml

X = 38ml

Y = 30.5ml

Z = 7.5ml

M1 = 0.5N

W1 = 1g


= 210.38

Roasted


Where,

Z = (X – Y) ml

X = 38ml

Y = 32ml

Z = 6ml

95

M1 = 0.5N

W1 = 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=50cm3

Density of oil= (45.6/50)g/cm3= 0.912g/cm

3

Density of water @20°C=1g/cm3

Specific gravity =0.912

Unroasted

Mass of oil=46.15g

Volume of gravity bottle=50cm3

Density of oil= (46.15/50)g/cm3= 0.923g/cm

3

Density of water @20°C=1g/cm3

Specific gravity =0.923

96

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

5.00 10.00 15.00 20.00 25.00 30.00 35.00 40.00 45.00

500000

1000000

1500000

2000000

2500000

3000000

3500000

Time-->

Abundance

TIC: ROASTED aa.D\ data.ms

11.461

25.609

29.318

29.419

29.557

29.636

29.973

30.070

97

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 2 25.609 6.75 C:\Database\NIST08.L n-Hexadecanoic acid 102726 000057-10-3 99 Tetradecanoic acid 81211 000544-63-8 93 n-Hexadecanoic acid 102724 000057-10-3 91 3 29.316 24.50 C:\Database\NIST08.L 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 4 29.419 7.92 C:\Database\NIST08.L Octadec-9-enoic acid 122782 1000190-13-7 96 cis-13-Octadecenoic acid 122788 013126-39-1 96 trans-13-Octadecenoic acid 122798 000693-71-0 93 5 29.557 16.99 C:\Database\NIST08.L trans-13-Octadecenoic acid 122798 000693-71-0 99 cis-Vaccenic acid 122781 000506-17-2 98 cis-13-Octadecenoic acid 122788 013126-39-1 98 6 29.637 17.52 C:\Database\NIST08.L trans-13-Octadecenoic acid 122798 000693-71-0 99 cis-13-Octadecenoic acid 122788 013126-39-1 99 cis-Vaccenic acid 122781 000506-17-2 97 7 29.974 13.31 C:\Database\NIST08.L Octadecanoic acid 124558 000057-11-4 98 Octadecanoic acid 124556 000057-11-4 96 Pentadecanoic acid 91826 001002-84-2 76 8 30.072 11.59 C:\Database\NIST08.L Octadecanoic acid 124556 000057-11-4 98 Octadecanoic acid 124558 000057-11-4 96 Octadecanoic acid 124559 000057-11-4 93 New ESSENTIAL OIL .M Tue Apr 09 10:19:59 2013 Area Percent 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 :

98

ALS Vial : 1 Sample Multiplier: 1 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 New ESSENTIAL OIL .M Tue Apr 09 10:20:31 2013

99

20 40 60 80 100 120 140 160 180 200 220 240 260 280

0

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9000

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Abundanc e

Sc an 1464 (11 .464 min ): R OAST ED aa .D \ da ta .ms

55 .0

83 .0

111 .0

196 .0168 .1140 .0

20 40 60 80 100 120 140 160 180 200 220 240 260 280

0

1000

2000

3000

4000

5000

6000

7000

8000

9000

m/ z-->

Abundanc e

# 205111 : 4 -H ep ta fluo robu tyryloxyhexadec ane

55 .0

83 .0

29 .0

111 .0

135 .0 169 .0 224 .0200 .0 282 .0

100

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 00

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 3 9 3 6 (2 5 .6 0 9 m in ): R O A S T E D a a .D \ d a ta .ms7 3 .0

5 5 .0

1 2 9 .0

9 7 .0 2 1 3 .12 5 6 .11 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 00

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 xa d e c a n o ic a c id6 0 .0

4 3 .0

1 2 9 .0

8 3 .0

2 1 3 .0 2 5 6 .01 5 7 .01 8 5 .01 0 1 .0

2 3 9 .0

20 40 60 80 100 120 140 160 180 200 220 240 260 280 3000

2000

4000

6000

8000

m/ z-->

Abundanc e

Sc an 4584 (29.316 min): R OAST ED aa.D \ data.ms55.0

83.0

111.0264.1137.0 222.1165.0 193.1 309.9

20 40 60 80 100 120 140 160 180 200 220 240 260 280 3000

2000

4000

6000

8000

m/ z-->

Abundanc e

# 122798: trans-13-Oc tadec enoic ac id55.0

83.0

111.029.0 264.0137.0 165.0 222.0193.0

101

20 40 60 80 100 120 140 160 180 200 220 240 260 280

0

1000

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3000

4000

5000

6000

7000

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9000

m/ z-->

A bundanc e

S c an 4602 (29 .419 min ): R O A S T E D aa .D \ da ta .ms

55 .0

83 .0

111 .0264 .1

137 .0165 .0 222 .1193 .1 283 .2241 .0

20 40 60 80 100 120 140 160 180 200 220 240 260 280

0

1000

2000

3000

4000

5000

6000

7000

8000

9000

m/ z-->

Abundanc e

# 122782 : O c tadec -9 -eno ic ac id

55 .0

83 .0

264 .0111 .0

29 .0

222 .0138 .0 180 .0 283 .0161 .0 199 .0 241 .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

S c a n 4 6 2 6 (2 9 .5 5 7 min ): R O A S T E D a a .D \ d a ta .ms

5 5 .0

8 3 .0

1 1 1 .02 6 4 .1

1 3 7 .01 6 5 .1 2 2 1 .11 9 3 .0 2 8 4 .12 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 : tra n s-1 3 -O c ta d e c e n o ic a c id

5 5 .0

8 3 .0

1 1 1 .0

2 9 .0 2 6 4 .01 3 7 .0 1 6 5 .0 2 2 2 .01 9 3 .0 2 8 4 .0

102

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 .02 6 4 .1

1 3 7 .01 6 5 .0 2 2 2 .11 9 3 .0 2 8 4 .22 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 .01 3 7 .0 1 6 5 .0 2 2 2 .01 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 .11 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 ta d e c a n o ic a c id

4 3 .0

7 3 .0

1 2 9 .0

2 8 4 .09 7 .0 1 8 5 .0

2 4 1 .0

1 5 7 .0 2 1 3 .01 8 .0

103

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 .19 7 .0 2 4 1 .11 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 .01 8 5 .0

2 4 1 .0

1 5 7 .0 2 1 3 .01 5 .0

104

2. Unroasted Shea butter sample.

Library Search Report Data Path : C:\msdchem\1\methods\New ESSENTIAL OIL .M\ Data File : UNROASTED bb.D Acq On : 8 Apr 2013 16:43 Operator : MEJIDA/ACHEM Sample : UNROASTED SHEA BUTTER Misc : ALS Vial : 2 Sample Multiplier: 1 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 _____________________________________________________________________________ 1 11.464 2.73 C:\Database\NIST08.L 5-Tetradecene, (E)- 56582 041446-66-6 91 Cyclotetradecane 56570 000295-17-0 90 7-Tetradecene, (Z)- 56580 041446-60-0 83 2 25.448 5.94 C:\Database\NIST08.L n-Hexadecanoic acid 102726 000057-10-3 99 Tetradecanoic acid 81211 000544-63-8 93 Pentadecanoic acid 91826 001002-84-2 87 3 29.231 30.99 C:\Database\NIST08.L trans-13-Octadecenoic acid 122798 000693-71-0 99 cis-13-Octadecenoic acid 122788 013126-39-1 98 cis-Vaccenic acid 122781 000506-17-2 97

5.00 10.00 15.00 20.00 25.00 30.00 35.00 40.00 45.00

200000

400000

600000

800000

1000000

1200000

1400000

1600000

1800000

2000000

2200000

2400000

Time-->

Abundance

TIC: UNROASTED bb.D\ data.ms

11.466 25.446

29.229

29.278

29.376

29.772

34.82835.310

36.042

37.84740.450

105

4 29.276 8.29 C:\Database\NIST08.L cis-13-Octadecenoic acid 122788 013126-39-1 98 cis-Vaccenic acid 122781 000506-17-2 97 trans-13-Octadecenoic acid 122798 000693-71-0 96 5 29.374 20.42 C:\Database\NIST08.L cis-Vaccenic acid 122781 000506-17-2 91 6-Octadecenoic acid 122783 1000336-66-8 91 6-Octadecenoic acid, (Z)- 122790 000593-39-5 90 6 29.774 23.01 C:\Database\NIST08.L Octadecanoic acid 124556 000057-11-4 91 n-Hexadecanoic acid 102726 000057-10-3 90 Octadecanoic acid 124559 000057-11-4 90 7 34.827 1.43 C:\Database\NIST08.L 9-Octadecenal, (Z)- 110397 002423-10-1 78 9-Oxabicyclo[6.1.0]nonane, cis- 11317 004925-71-7 50 trans-13-Octadecenoic acid 122798 000693-71-0 45 8 35.307 0.85 C:\Database\NIST08.L 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)- 9 36.040 4.81 C:\Database\NIST08.L 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 10 37.848 0.31 C:\Database\NIST08.L 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 11 40.451 1.24 C:\Database\NIST08.L 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)- New ESSENTIAL OIL .M Tue Apr 09 10:26:12 2013 Area Percent Report Data Path : C:\msdchem\1\methods\New ESSENTIAL OIL .M\ Data File : UNROASTED bb.D

106

Acq On : 8 Apr 2013 16:43 Operator : MEJIDA/ACHEM Sample : UNROASTED SHEA BUTTER Misc : ALS Vial : 2 Sample Multiplier: 1 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 New ESSENTIAL OIL .M Tue Apr 09 10:26:35 2013

107

2 0 3 0 4 0 5 0 6 0 7 0 8 0 9 0 1 0 01 1 01 2 01 3 01 4 01 5 01 6 01 7 01 8 01 9 02 0 00

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 in ): U N R O A S T E D b b .D \ d a ta .m s5 5 .0

6 9 .0

8 3 .0

9 7 .0

1 1 1 .0

1 2 5 .01 3 9 .91 5 4 .0 1 9 6 .01 6 7 .8

2 0 3 0 4 0 5 0 6 0 7 0 8 0 9 0 1 0 01 1 01 2 01 3 01 4 01 5 01 6 01 7 01 8 01 9 02 0 00

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 tra d e c e n e , (E )-5 5 .0

6 9 .0

4 1 .0

8 3 .0

9 7 .0

2 7 .01 1 1 .0

1 9 6 .01 2 5 .0

1 3 9 .0 1 6 8 .01 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

S c a n 3 9 0 8 (2 5 .4 4 8 m in ): U N R O A S T E D b b .D \ d a ta .ms

7 3 .0

5 5 .0

1 2 9 .0

2 1 3 .09 7 .02 5 6 .11 8 4 .91 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 xa d e c a n o ic a c id

6 0 .0

4 3 .0

1 2 9 .0

8 3 .0

2 1 3 .0 2 5 6 .01 5 7 .01 8 5 .01 0 1 .0

2 3 9 .0

108

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

S c a n 4 5 6 9 (2 9 .2 3 1 min ): U N R O A S T E D b b .D \ d a ta .ms

5 5 .0

8 3 .0

1 1 1 .02 6 4 .11 3 6 .9

1 6 5 .0 2 2 0 .11 9 3 .0 2 8 4 .22 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 .01 3 7 .0 1 6 5 .0 2 2 2 .01 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 .11 3 7 .02 2 2 .01 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 is-1 3 -O c ta d e c e n o ic a c id

5 5 .0

8 3 .0

1 1 1 .0

2 9 .0 2 6 4 .01 3 7 .01 6 5 .0 2 2 2 .01 9 3 .0 2 8 4 .0

109

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 .02 6 4 .1

1 3 7 .02 2 2 .11 6 5 .0 1 9 3 .1 2 8 3 .92 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 is-V a c c e n ic a c id

5 5 .0

8 3 .0

1 1 1 .02 9 .0

2 6 4 .01 3 7 .0

1 6 5 .0 2 2 2 .01 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 .02 8 4 .11 8 5 .0 2 4 1 .1

5 3 .01 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 .01 8 5 .0

2 4 1 .0

1 5 7 .0 2 1 3 .01 5 .0

110

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 00

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 5 5 4 7 (3 4 .8 2 7 min ): U N R O A S T E D b b .D \ d a ta .ms5 5 .0

1 2 9 .0

9 5 .0

1 8 5 .0 4 5 3 .23 9 3 .12 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 00

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 ta d e c e n a l, (Z )-5 5 .0

9 8 .0

1 3 5 .02 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 00

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 5 6 3 2 (3 5 .3 1 3 m in ): U N R O A S T E D b b .D \ d a ta .ms5 5 .0

1 2 8 .9

9 4 .9

4 5 3 .21 8 4 .9 3 9 3 .2

2 9 7 .12 4 1 .23 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 00

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 -Cyc lo p e n te n -3 -o n e , 1 -(e th o xyc a rb o n ylo xy)-2 9 .0

6 9 .0

1 7 0 .01 2 6 .0

111

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 00

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 5 7 5 9 (3 6 .0 4 0 min ): U N R O A S T E D b b .D \ d a ta .ms1 4 8 .9

5 7 .0

1 0 4 .0 2 7 9 .01 8 5 .2 4 5 3 .23 9 2 .92 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 00

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 th a lic a c id , d e c yl 2 -e th ylh e xyl e ste r1 4 9 .0

5 7 .03 0 7 .01 0 4 .0

2 6 .0

UPGRADE OF THE INDIGENOUS PRODUCTION OF SHEA BUTTER

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