ULTRASOUND ASSISTED EXTRACTION OF OIL FROM APRICOT KERNELS (Prunus armeniaca L.)

118 Pages·2017·24.2 MB·English

ULTRASOUND ASSISTED EXTRACTION OF OIL
FROM APRICOT KERNELS (Prunus armeniaca L.)

Dissertation

Submitted to the Punjab Agricultural University
in partial fulfillment of the requirements
for the degree of

DOCTOR OF PHILOSOPHY
in
PROCESSING AND FOOD ENGINEERING
(Minor Subject: Food Science and Technology)

By
Bazilla Gayas
(L-2013-AE-110-D)

Department of Processing and Food Engineering
College of Agricultural Engineering and Technology
 PUNJAB AGRICULTURAL UNIVERSITY
LUDHIANA - 141004

2017
1
CERTIFICATE I

This is to certify that the dissertation entitled “Ultrasound assisted extraction of oil
from apricot kernels (Prunus armeniaca L.)” submitted for the degree of Doctor of
Philosophy in the subject of Processing and Food Engineering (Minor subject: Food
Science and Technology) of the Punjab Agricultural University, Ludhiana, is a bonafide
research work carried out by Bazilla Gayas (L-2013-AE-110-D) under my supervision and
that no part of this thesis has been submitted for any other degree.
The assistance and help received during the course of investigation have been fully
acknowledged.

_____________________________
Major Advisor
(Dr. (Mrs.) Gagandeep Kaur Sidhu)
Sr. Research Engineering
Dept. of Processing and Food Engineering
Punjab Agricultural University,
Ludhiana-141004, Punjab, India

2
CERTIFICATE - II

This is to certify that the dissertation entitled, “Ultrasound assisted extraction of oil
from apricot kernels (Prunus armeniaca L.)” submitted by Bazilla Gayas (Admission No.
L-2013-AE-110-D) to the Punjab Agricultural University, Ludhiana, in partial fulfillment of
the requirements for the degree of Doctor of Philosophy in the subject of Processing and
Food Engineering (Minor subject: Food Science and Technology) has been approved by the
Student’s Advisory Committee after an oral examination on the same, in collaboration with
an external examiner.

______________________________ __________________________
(Dr. (Mrs.) Gagandeep Kaur Sidhu) (Dr. Devinder Dhingra)
Major Advisor External Examiner
Principal Scientist (AS & PE)
Agricultural Engineering Division
KAB-II (Krishi Anusandhan Bhawan),
PUSA, ICAR, New Delhi-110 012

_______________________
(Dr. A.K. Singh)
Head of the Department

_________________________
(Dr. (Mrs.) Neelam Grewal)
Dean Postgraduate Studies

3
ACKNOWLEDGEMENTS

First of all, I express my gratitude, appreciation and indebtness to Almighty Allah, who
out of his infinite love, bestowed and inspired the entire humanity towards knowledge, truth and
internal love and enabled me to complete this work.
I am grateful to my esteemed advisor, Dr. (Mrs.) Gagandeep Kaur Sidhu (Senior
Research Engineer), whose expertise, understanding, generous guidance and support made it
possible for me to work on a topic that was of great interest to me. It was pleasure working with
her.
I feel extremely priviledged to express my deep sense of reverene and indebtness to all
the members of my Advisory Committee Dr A.K.Singh (Senior Research Engineer cum Head),
Dr. (Mrs.) Amarjeet Kaur (Senior Milling Technologist) Department of Food Science and
Technology, Dr. (Mrs.) Amrit Mahal (Professor) Department of Mathematics, Statistics and
Physics for their sincere exhortation, meticulous guidance and constant encouragement
throughtout this research work.
Sincere regards are due to Dr. Amarjeet Singh (Senior Extension Engineer) and
Dr.Satish Kumar (Professor) Dean PGS Nominee for providing necessary departmental facilities
for the smooth conduct of this investigation.
Special thanks to Dr. T.C.Mittal (Senior Extension Engineer), Dr. M.S.Alam (Sr.
Research Engineer), Department of Processing and Food Engineeringfor their insight and support
throughout this experience.
I would also like to thank Office Assistant Mr.Purshotam and Lab Technician
Mr.Harbans Singh, Mr. Inderjeet Singh, Mr. Harpal Singh for providing me all the help during
my research work.
It is often said good friends are rare to get. In this context I find myself very lucky to have
friends like Gurnaz, Khalid Gul, Sandhya Mam, Beena, Asima, Awsi, Arshdeep, Amanpreet
Kaur, Gurpreet Kaur, Navjot, Gagan, Karanveer Gill, Ritika, Insha, Kulsum, Khalid Bashirfor
helping me when I was in need. They are all a fun bunch with lots of enthusiasm and optimism.
I especially thank my parentsMrs. And Mr. Gayas ud din Shahmiri and brother (Adil
Zaheem) for their unconditional love and care. I would not have made it this far without them.
Special thanks to the newest addition to my family, Faizan Rafiq, my fiancée as well as his
wonderful family who have been supportive and caring.
I take opportunity to sincerely acknowledge the financial assistance provided by MANF
(Maulana Azad National Fellowship), UGC, New Delhi, which buttressed me to perform my work
comfortably.
Date:
Place: (Bazilla Gayas)

4
Title of the Thesis : Ultrasound assisted extraction of oil from apricot
kernels (Prunus armeniaca L.)

Name of the Student : Bazilla Gayas
and Admission No : L-2013-AE-110-D
Major Subject : Processing and Food Engineering
Minor Subject : Food Science and Technology
Name and Designation : Dr. (Mrs.) Gagandeep Kaur Sidhu
of Major Advisor Senior Research Engineer
Degree to be Awarded : Ph. D
Year of award of Degree : 2017
Total Pages in Thesis : 97 + Annexures (i-viii) + VITA
Name of University : Punjab Agricultural University, Ludhiana-141 004

ABSTRACT

In the present study different process parameters for extraction of apricot kernel oil using ultrasound
assisted extraction (UAE) method were optimized. The different operational parameters for UAE
method viz., temperature (30-60oC), extraction time (30-50 minutes) and solvent to sample ratio
(15:01-25:01) were optimized using Box-Behnken technique combined with response surface
methodology. The optimum extraction parameters obtained were extraction time (43.95 min),
extraction temperature (51.71oC), and solvent to sample ratio (19.8:01) at fixed frequency of 40
kHz. The oil extracted using UAE was compared with non sonicated methods (Soxhlet and
mechanical extraction), on the basis of different physico chemical properties, FT-IR and fatty acid
composition of oil. The recovery of oil from UAE method was 97.21% while as for ME the oil
recovery was 76.21%. The main fatty acid present in apricot kernel oil were oleic acid which were
significantly (p<0.05) different for all extraction methods and accounted for 67.45% for ME,
66.87% for SE and 66.85% for UAE. The meal obtained after the extraction of oil was analyzed for
proximate composition and SEM was carried out to obtain the morphological properties of kernel
meal. Defatted meal constituted high protein content 43.08% for SE, 45.13% for UAE and 40.12%
for ME. The packaging of oil was done in amber colored, colorless and plastic bottles and stored at
ambient conditions. Various quality parameters of stored oil were determined at regular interval of
one month for 180 days. The acid value was observed to increase steadily in SE oil packed in plastic
bottles (6.12mgKOH/g) as compared to UAE (5.49mgKOH/g). The iodine value was observed to be
declining during the storage period. Oil stored in amber bottles has better nutritional quality than
that of colorless bottles and plastic bottles and can be stored at ambient temperature for more than 6
months without any major impairment on quality of oil.

Keyword: Apricot kernel oil, FT-IR, Fatty acid, Quality parameters, SEM, UAE method.

_____________________ ____________________
Signature of Major Advisor Signature of the Student

5
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krSwx

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97 + AMiqkwvW (i-viii) + vItw
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XUnIvristI dw nwm : pMjwb KyqIbwVI XUnIvristI, luiDAwxw – 141004,
pMjwb, Bwrq [
swr-AMS
mOjUdw AiDAYn iv`c KurmwnI bIj qoN qyl k`Fx leI AltrwswaUNf shwiek krSwx (XU.ey.eI.)
ivDI iv`c v`K-v`K pRosYs mwpdMfW dw Fu`kvIkrn kIqw igAw[ v`K-v`K pircwlk mwpdMf ijvyN
qwpmwn (30-60°C), krSwx smW (30-50 imMt) Aqy ivlwiek sYNpl Anupwq (15:01-25:01) nUM
bwks bYNkn qknIk Aqy pRqIikirAw sqhI pRxwlI dy sumyl nwl Fu`kvIkrn kIqw igAw[ Fu`kvyN
krSwx mwpdMf iv`c krSwx smW (43.93 imMt) krSwx qwpmwn (51.71°C) Aqy ivlwiek sYNpl
Anuswr (19:8:01) sB qoN v`D Fu`kvyN pwey gey[ v`K-v`K BOiqkI-rswiexkI KwsIAqW dy AwDwr qy
XU.ey.eI. Aqy ZYr sonIkytf ivDIAW rwhIN pRwpq qyl dI qulnw kIqI geI[ X.Uey.eI. ivDI rwhIN qyl
dI vsUlI 97.21% jdik AY~m.eI. rwhIN 76.21% hI sI[ KurmwnI bIj qyl iv`c mu`K PYtI eyisf
aulyiek eyisf sI jo AY~m.eI., AY~s.eI. Aqy XU.ey.eI. leI kRmvwr 67.45%, 66.87% Aqy
66.85% sI[ qyl k`Fx qoN bwAd bcI &l nUM Anumwinq sMrcnw leI ivSlyisq kIqw igAw Aqy
^l dIAW AwikRqI sbMDI ivSySqwvW leI AYm.eI.AYs.eI. sYm ivDI kIqw igAw[ qyl inSkwiSq
^l iv`c pRotIn mwqrw AY~s.eI. iv`c 43.08% sB qoN izAwdw, X.U ey.eI. leI 45.13% Aqy
AY~m.eI. leI 40.12% sI[ qyl n UM kxvMny, rMghIx plwsitk boqlW iv`c pYk krky kmry dy
qwpmwn qy BMfwrn kIqw igAw[ iek mhIny dy AMqrwl qy 180 idnW q`k leI BMfwr kIqy qyl dy
guxv`qw mwpdMfW nUM priKAw igAw[ eyisf mwqrw XU.ey.eI. dy mukwbly AY~s.eI. qyl jo plwsitk
boqlW iv`c pYk kIqw igAw sI iv`c hOlI-hOlI vDdw igAw[ BMfwrn smyN d y nwl AwEfIn mwqrw
Gtdw igAw[ kxkvMnIAW boqlW iv`c BMfwr kIq y qyl dI poSk guxv`qw rMghIn Aqy plwsitk
boqlW dy mukwbly vDIAw sI[ KurmwnI bIj qyl nUM ies qrHW guxv`qw au~pr koeI Kws smJOqw nw
krdy hoey 6 mhIn y qoN izAwdw smyN leI kmr y dy qwpmwn qy BMfwr kIqw jw skdw hY [

mu`K Sbd: KurmwnI bIj qyl, AYP.tI.-AweI.Awr., PYtI eyisf, guxv`qw mwpdMf, XU.ey.eI.

__________________ ________________
mu`K slwhkwr d y hsqwKr iv`idAwrQI dy hsqwKr

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CONTENTS

CHAPTER TITLE PAGE NO.

I INTRODUCTION 1-5
II REVIEW OF LITERATURE 6-26
2.1 Engineering properties of apricot kernel 6-10
2.2 Mechanical oil extraction 10-13
2.3 Solvent oil extraction 13-15
2.4 Ultrasound assisted extraction 15-21
2.5 Rheological properties of oil 21-24
2.6 Storage of oil 24-26
III MATERIAL AND METHODS 27-43
3.1 Experimental design and equipment used 27-28
3.2 Procurement of raw materials 28
3.3 Determination of different engineering properties of apricot 29-32
kernels
3.3.1 Moisture content estimation 29
3.3.2 Geometric mean diameter 29
3.3.3 Arithmetic mean diameter 29
3.3.4 Sphericity 30
3.3.5 Surface area 30
3.3.6 Bulk density 30
3.3.7 True density 30
3.3.8 Porosity 31
3.3.9 Thousand grain weight 31
3.3.10 Frictional properties 31
3.3.11 Coefficient of internal friction 31
3.3.12 Coefficient of external friction 31-32
3.3.13 Angle of repose 32
3.4 Determination of proximate composition of apricot kernels 32-34
3.4.1 Determination of protein content 32
3.4.2 Determination of crude fibre content 33
3.4.3 Determination of total ash content 33-34
3.4.4 Determination of mineral content 34
3.5 Extraction of oil from apricot kernels 34-35
3.5.1 Mechanical extraction 34
3.5.2 Soxhlet extraction 34
3.5.3 Ultrasound assisted extraction 34
3.6 Experimental design for optimization of independent parameters 36-37
3.7 Recovery of oil 37

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3.8 Determination of different physico chemical characteristics of oil 37-42
3.8.1 Acid value 37
3.8.2 Saponification of oil 37-38
3.8.3 Ester value 38
3.8.4 Refractive index 38
3.8.5 Iodine value 39
3.8.6 Peroxide value 39-40
3.8.7 Scanning electron microscopy 40
3.8.8 Fourier transform infrared (FT-IR) analysis 41
3.8.9 Fatty acid composition 41
3.8.10 Rheological test 42
3.9 Storage of apricot kernel oil 42-43
3.10 Statistical analysis 43
3.11 Economic analysis 43
IV RESULTS AND DISCUSSION 44-82
4.1 Engineering properties and proximate composition of apricot kernels 44-48
4.1.1 Different engineering properties of fresh apricot pits and kernels 44
4.1.2 Proximate composition of apricot kernels 45-48
4.2 Extraction of apricot kernel oil 48
4.3 Effect of operational parameters on oil and physico chemical properties 48-61
of apricot kernel oil using ultrasound assisted extraction (UAE) method
4.3.1 Oil yield 49-52
4.3.2 Physico chemical properties of apricot kernel oil 53-61
4.4 Optimization of optimum solution for various process parameters for 62-63
extraction of apricotkernel oil
4.5 Rheological properties of Ultrasound assisted extracted apricot kernel oil 63-64
4.6 Comparison of oil extracted by ultrasound assisted extraction method with 65-72
mechanical andsolvent method
4.6.1 FT-IR analysis of apricot kernel oil 69-70
4.6.2 Gas chromatography for apricot kernel oil obtained by different 71
extraction methods
4.7 Effect of extraction processes on structural and proximate composition of 72-74
defatted kernelpowder
4.7.1 Morphological characteristics of kernel meal 72-73
4.7.2 Proximate composition of defatted apricot kernel meal 73-74
4.8 Storage of oil 74-81
4.9 Economic analysis 81-82
V SUMMARY 83-86
REFRENCES 87-96
APPENDIX-1 i-viii

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LIST OF TABLES

Table No. Title Page No.

3.1 Experimental design 27
3.2 Equipments used during research 28
3.3 Experimental combination for response surface analysis of apricot kernel oil 36
4.1 Different engineering properties of fresh apricot pits and kernels 45
4.2 Proximate composition of apricot kernels 46
4.3 Mineral content of apricot kernels 46
4.4 Anti-nutrients in apricot kernels 47
4.5 Variables and their level for the experimental design 49
4.6 Experimental combination for three factors (actual) response surface analysis 49
4.7 Three level Box Behnken with three independent variables and experimental 50
and predicted responses
4.8 Estimated regression coefficient 51
4.9 Optimum solution for various process parameters for extraction of apricot 63
kernel oil
4.10 Combinations used for ultrasound assisted extraction of apricot kernel oil 64
4.11 Comparision of mechanical, solvent and optimum solution of UAE extracted 66
apricot kernel oil properties
4.12 Fatty acid composition of apricot kernel oil extracted by different extraction 72
methods
4.13 Proximate composition of defatted apricot kernel oil 73

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LIST OF FIGURES

Figure Title Page No.

3.1 Apricot pits 29
3.2 Apricot kernels 29
3.3 Hot air oven 30
3.4 Mini oil expeller 35
3.5 Soxhlet apparatus 35
3.6 Ultrasonicator 35
3.7 Abbe’s refractometer 38
3.8 Scanning electron microscopy 40
3.9 Ion coating machine for SEM 40
3.10 Gas chromatography- Mass spectrometry 41
3.11 Bohlin rhemoter 42
3.12 Apricot kernel oil packed in three different packaging materials 43
4.1 Proximate composition of apricot kernels 47
4.2 Mineral content of apricot kernels 47
4.3 Anti-nutrients in apricot kernels 48
4.4 Contour plots for effect of different factors on oil yield of apricot 52
kernel oil
4.5 Response 3D plots for effect of different factors on oil yield of apricot 53
kernel oil
4.6 Contour plots for effect of different factors on acid value of apricot 54
kernel oil
4.7 Response 3D plots for effect of different factors on acid value of apricot 55
kernel oil
4.8 Contour plots for effect of different factors on free fatty acid of apricot 55
kernel oil
4.9 Response 3D plots for effect of different factors on free fatty acid of 56
apricot kernel oil
4.10 Contour plots for effect of different factors on specific gravity of 57
apricot kernel oil
4.11 Response 3D plots for effect of different factors on specific gravity of 58
apricot kernel oil
4.12 Contour plots for effect of different factors on saponification value of 59
apricot kernel oil
4.13 Response 3D plots for effect of different factors on saponification value 59
of apricot kernel oil

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