copyrightpsasir.upm.edu.my/id/eprint/41275/1/fstm 2013 1r.pdf · 62.5 °briks larutan sukrosa...
TRANSCRIPT
© COPYRIG
HT UPM
UNIVERSITI PUTRA MALAYSIA
MOHAMED NAZIM BIN ANVARALI
FSTM 2013 1
PRODUCTION, OPTIMIZATION, CHARACTERIZATION AND STORAGE STABILITY OF ROSELLE CONCENTRATE
© COPYRIG
HT UPM
PRODUCTION, OPTIMIZATION,
CHARACTERIZATION AND STORAGE
STABILITY OF ROSELLE CONCENTRATE
MOHAMED NAZIM BIN ANVARALI
MASTER OF SCIENCE
UNIVERSITI PUTRA MALAYSIA
2013
© COPYRIG
HT UPM
PRODUCTION, OPTIMIZATION, CHARACTERIZATION AND
STORAGE STABILITY OF ROSELLE CONCENTRATE
By
MOHAMED NAZIM BIN ANVARALI
Thesis Submitted to the School of Graduate Studies, Universiti Putra
Malaysia, in Fulfilment of the Requirements for the Degree of Master
Science
February 2013
© COPYRIG
HT UPM
COPYRIGHT
All material contained within the thesis, including without limitation text,
logos, icons, photographs and all other artwork, is copyright material of
Universiti Putra Malaysia unless otherwise stated. Use may be made of any
material contained within the thesis for non-commercial purposes from the
copyright holder. Commercial use of material may only be made with the
express, prior, written permission of Universiti Putra Malaysia.
Copyright © Universiti Putra Malaysia
© COPYRIG
HT UPM
Abstract of thesis presented to the Senate of Universiti Putra Malaysia
in fulfilment of the requirement for the degree of Master of Science
PRODUCTION, OPTIMIZATION, CHARACTERIZATION AND
STORAGE STABILITY OF ROSELLE CONCENTRATE
By
MOHAMED NAZIM BIN ANVARALI
February 2013
Chairman: Professor Tan Chin Ping, PhD
Faculty: Food Science and Technology
Three different extraction techniques were used to determine the suitability
and efficiency of the roselle extraction techniques for the development of
roselle concentrate. These extraction techniques were 1) hot water extraction
(HWE), 2) puree extraction (PE) and 3) osmotic extraction (OE). Data from
preliminary comparative studies suggested that the osmotic solution (OS)
from the OE technique can be used for the development of roselle
concentrate as it has a significantly (p<0.05) higher anthocyanin content, D-
malic and L-malic acid with the value of 100.00 ± 0.43 mg/L as expressed in
delphinidin-3-glucoside, 4043.60 ± 11.17 and 2946.90 ± 16.69 (ppm/L);
respectively, compared to HWE and PE. Further studies were conducted
© COPYRIG
HT UPM
using response surface methodology (RSM) in order to determine the optimal
processing parameters of the OE technique. The parameters affecting the
roselle extraction process were optimized for the color of the roselle
concentrate (red purplish), a taste with minimum sharpness and a high
anthocyanin content. A central composite design (CCD) with a quadratic
model consisted of three independent variables: extraction time, osmotic
solution concentration and extraction temperature. The response variables
were used to determine the Hunter lab color index – L*, a*, b*, acidity
percentage, total anthocyanin content, color density, color degradation index
and sensory attributes, which included the color, grassy (odor), fruity (taste),
sharpness (taste) and overall acceptability of all of the roselle concentrates
and juices. A total of 20 different combinations (including six replicates of the
center point each with coded value 0) were chosen at random according to a
Central Composite Design (CCD) configuration for three factors. The results
suggested that for the production of red to purple color of roselle
concentrate, the extraction should be carried under the following conditions:
70 °C (extraction temperature), 205 minutes (extraction time) and 62.5 °Brix of
sucrose solution (as a medium of extraction). Meanwhile, the storage
temperature yielded significant (p<0.05) negative effects on the total quality
of the roselle concentrate when compared to the duration of storage. High
temperatures during storage may cause dramatic changes in anthocyanin
© COPYRIG
HT UPM
content and the color of the osmotic solution due to the degradation of
anthocyanins. Roselle concentrate stored for 8 weeks at 5 °C retains up to
74.8% of its total anthocyanin content (compared to the initial value; 4334.15
mg/L); these values are significantly (p<0.05) higher than those of roselle
concentrate that were stored at 25 °C and 45 °C (31.1% and 6.5% of its initial
anthocyanin content at the end of storage, respectively). This research shows
that the osmotic solution, which is normally not reused and is considered as
industrial waste in the fruit osmotic dehydration (OD) process, exhibits the
highest amount of total anthocyanin (p<0.05). The osmotic solution may be
used as an ingredient as a healthy roselle concentrate. Proper storage at low
temperature can ensure its appearance and taste qualities, and the functional
properties of the concentrate will be stabilized, which will allow roselle juice
to be accepted as a functional drink.
© COPYRIG
HT UPM
Abstrak tesis yang dikemukakan kepada senat Universiti Putra Malaysia
sebagai memenuhi keperluan untuk ijazah Master Sains
PENGELUARAN, PENGOPTIMUMAN, PENCIRIAN DAN KESTABILAN
PENYIMPANAN PEKATAN ROSELLE
Oleh
MOHAMED NAZIM BIN ANVARALI
Februari 2013
Pengerusi: Profesor Tan Chin Ping, PhD
Fakulti: Sains dan Teknologi Makanan
Tiga teknik pengekstrakan yang berbeza telah digunakan untuk menentukan
kesesuaian dan kecekapan teknik pengekstrakan roselle untuk pembangunan
roselle pekat. Teknik-teknik pengekstrakan tersebut adalah 1) pengekstrakan
air panas (HWE), 2) pengekstrakan puri (PE) dan 3) pengekstrakan osmotik
(OE). Data daripada kajian perbandingan awal mencadangkan bahawa
larutan osmotik (OS) daripada teknik OE boleh digunakan untuk
pembangunan pekat roselle kerana ia mempunyai secara nyata (p <0.05)
lebih tinggi kandungan antosianin, asid D-malik dan L-malik dengan nilai
100.00 ± 0.43 mg / L yang dinyatakan sebagai delphinidin-3 glukosida,
4043.60 ± 11.17 dan 2946.90 ± 16.69 (ppm / L), masing-masing, berbanding
HWE dan PE. Kajian lanjutan dijalankan dengan menggunakan kaedah
© COPYRIG
HT UPM
gerak balas permukaan (RSM) untuk menentukan parameter pemprosesan
optimum bagi teknik EO. Parameter yang mempengaruhi proses
pengekstrakan roselle yang perlu dioptimumkan menjurus kepada hasilan
pekatan roselle dengan warna merah keunguan, rasa ketajaman yang terhad
dan kandungan antosianin yang tinggi. Satu reka bentuk pusat komposit
(CCD) dengan model kuadratik terdiri daripada tiga pembolehubah bebas:
masa pengekstrakan, kepekatan larutan osmotik dan suhu pengekstrakan.
Pembolehubah sambutan telah digunakan untuk menentukan indeks warna
makmal Hunter - L *, a*, b *, peratusan keasidan, jumlah kandungan
antosianin, kepadatan warna, indeks kemerosotan warna dan sifat-sifat
deria, termasuk warna, bau rumput, rasa kebuah-buahan , rasa ketajaman
dan penerimaan keseluruhan bagi semua pekatan roselle dan jus. Sejumlah
20 kombinasi berbeza (termasuk enam replikasi titik pusat berkod 0) telah
dipilih secara rawak mengikut Rekabentuk Pusat Komposit (CCD)
konfigurasi dengan tiga faktor. Keputusan mencadangkan bahawa bagi
penghasilan pekatan roselle berwarna merah ungu, pengekstrakan roselle
perlu diproses dengan menggunakan parameter optimum seperti berikut
berikut: 70 °C (suhu pengekstrakan), 205 minit (masa pengekstrakan) dan
62.5 °Briks larutan sukrosa (sebagai medium pengekstrakan). Sementara itu,
suhu penyimpanan memberikan kesan negatif yang signifikan (p <0.05)
kepada kualiti pekatan roselle jika dibandingkan dengan tempoh
© COPYRIG
HT UPM
penyimpanan. Suhu tinggi semasa penyimpanan boleh menyebabkan
perubahan dramatik dalam kandungan antosianin dan warna larutan
osmotik yang disebabkan oleh kemusnahan antosianin. Roselle yang
disimpan selama 8 minggu pada suhu 5 °C mengekalkan sehingga 74.8%
daripada jumlah asal kandungan antosianin (berbanding dengan nilai awal;
4334.15 mg / L), nilai kandungan yang signifikan (p <0.05) lebih tinggi
berbanding kordial roselle yang disimpan pada suhu 25 °C dan 45 °C (31.1%
dan 6.5% daripada jumlah asal kandungan antosianin yang diukur pada
akhir tempoh penyimpanan, masing-masing). Kajian ini menunjukkan
bahawa larutan osmosis, yang biasanya tidak diguna semula dan dianggap
sebagai sisa dari perindustrian dehidrasi buah osmotik (OD), mengandungi
jumlah kandungan antosianin yang tinggi (p <0.05). Ia boleh digunakan
sebagai ramuan dalam penghasilan pekatan roselle yang sihat dan berwarna
merah. Penyimpanan yang betul pada suhu rendah boleh memastikan
penampilan dan kualiti rasa, serta ciri-ciri fungsi kekal stabil, di mana ini
membolehkan jus roselle boleh diterima sebagai minuman berfungsi.
© COPYRIG
HT UPM
ACKNOWLEDGEMENTS
Praise be to Allah SWT, by the grace of God, and his guidance, I am able to
complete this Master of Science thesis.
This thesis is specially dedicated to both of my parents, Mr. Anvarali Bin
Ibramsha, and Mrs. Balkis Binti Abd. Kader. Their love and support given to
me, and their enthusiasm and attention have helped me tremendously
during this study. Their prayers have changed my life for the better. I would
like to thank my other family members (my brother, Fazil; my sister, Fadzila,
my sister in law, Razia; and my most lovely nieces and nephews, Nur
Nabilah, Mohd Afiq, Nadia Amirah and Mohd Danish) who have made my
life more meaningful, all of you are everything to me. Hopefully, this
achievement will soon open up more opportunities and inspire the young
ones in my family in the pursuit of education and knowledge grasping.
Insha Allah…
I have my utmost respect and gratitude to Prof. Dr. Tan Chin Ping, for being
my main supervisor. He is a very responsible educator, always willing to
share his knowledge and has been relentless in providing assistance to his
students. Without the tutelage and guidance from him, it is impossible for me
to complete my Master studies. A billion thanks to Prof. Dr. Tan Chin Ping.
© COPYRIG
HT UPM
To Prof. Dr. Salmah Yusof, who had opened the door way and given me the
opportunity to start my postgraduate studies at the Faculty of Food Science
and Technology, I will never forget your support. Your motherly guidance,
love and attention help us to be an excellent student. Thank you Professor.
Dr. Salmah Yusof.
Not forgetting, Dr. Nazimah Sheikh Abdul Hamid who had contributed
ideas and guidance and support during my Master studies. Thank you very
much.
To Mrs. Hasimah in MARDI, where I now serve as a Research Officer, I will
never forget your support and encouragement to me in the completion of this
thesis. And to my very best friends in MARDI, Reza, Saiful and Raja Arief, as
well as the girls in the Food Technology Research Centre (TM1 & TM2) you
really brightened my life, you are a diamond in my heart.
Finally, to all the staff of the Faculty of Food Science and Technology,
Universiti Putra Malaysia, I would like to thank you all. The help, support
and cooperation I received from the laboratories during my Master studies
including the assistance and cooperation from the administrators of the
Graduate School Office, I would like to sincerely thank you each one of you.
21st March 2013
© COPYRIG
HT UPM
I certify that an Examination Committee has met on 22nd February 2013 to
conduct the final examination of Mohamed Nazim Bin Anvarali on his
Master of Science thesis entitled " Production Optimization, Characterization
And Storage Stability Of Roselle Concentrate" in accordance with the
Universities and University College Act 1971 and the Constitution of the
Universiti Putra Malaysia [P. U. (A) 106] 15 March 1998. The Committee
recommends that the student be awarded the Master of Science.
Members of the Thesis Examination Committee were as follows:
Badlishah Sham Baharin
Associate Professor
Faculty of Food Science and Technology
Universiti Putra Malaysia
(Chairman)
Roselina Karim, PhD
Associate Professor
Faculty of Food Science and Technology
Universiti Putra Malaysia
(Internal Examiner)
Yus Aniza Yusof, PhD
Associate Professor
Faculty of Engineering
Universiti Putra Malaysia
(Internal Examiner)
Irwandi, PhD
Professor
Kulliyyah Of Engineering,
International Islamic University Malaysia Malaysia
(External Examiner)
Seow Heng Fong, PhD
Professor and Deputy Dean
School of Graduate Studies
Universiti Putra Malaysia
Date:
© COPYRIG
HT UPM
This thesis was submitted to the Senate of Universiti Putra Malaysia and has
been accepted as fulfilment of the requirement for the degree of Master of
Science. The members of the Supervisory Committee were as follows:
Tan Chin Ping, PhD
Professor
Faculty of Food Science and Technology
Universiti Putra Malaysia
(Chairman)
Nazimah Binti Sheikh Abdul Hamid, PhD
Lecturer
Faculty of Food Science and Technology
Universiti Putra Malaysia
(Member)
Salmah Yusof, PhD
Professor
Faculty of Science and Technology
Universiti Sains Islam Malaysia
(Member)
BUJANG BIN KIM HUAT, PhD
Professor and Dean
School of Graduate Studies
Universiti Putra Malaysia
Date:
© COPYRIG
HT UPM
DECLARATION
I declare that the thesis is my original work except for quotations and
citations which have been duly acknowledged. I also declare that it has not
been previously, and is not concurrently, submitted for any other degree at
Universiti Putra Malaysia or at any other institutions.
MOHAMED NAZIM BIN ANVARALI
Date: 22 February 2013
© COPYRIG
HT UPM
TABLE OF CONTENTS
Page
ABSTRACT ii
ABSTRAK v
ACKNOWLEDGEMENTS viii
APPROVAL x
DECLARATION xiii
LIST OF TABLES xvii
LIST OF FIGURES xix
LIST OF ABBREVIATIONS xx
CHAPTER
1 INTRODUCTION 1
2 LITERATURE REVIEW 5
2.1 Fruit and Beverage Industries 5
2.1.1 Market Trend-Fruit Concentrate in Malaysia 7
2.1.2 Scenario in Malaysia 8
2.2 Roselle (Hibiscus sabdariffa L.) 11
2.2.1 Origin and distribution of roselle 11
2.2.2 Botanical description 12
2.2.3 Environment 13
2.2.4 Planting 14
2.2.5 Harvest 14
2.2.6 Traditional medicinal uses 15
2.2 Variables in processing of roselle concentrate 16
and effects on the juice quality
2.3 Osmotic Dehydration 20
2.3.1 Overview of Sucrose and osmotic dehydration 20
2.3.2 Osmotic dehydration 21
2.3.3 Operating variables related to the sucrose 22
concentrated solution
2.3.4 Sucrose 24
2.3.5 Role of sucrose in aroma and flavor of foods 27
2.3.5.1 Interactions with acid-sour taste 28
2.3.5.2 Retention of Aromas 29
2.3.5.3 Interaction of sucrose-color-flavor 29
2.3.5.4 Fruit flavors 30
2.4 Storage Stability of Fruit Juice 31
2.5 Formulation Optimization Using Statistical Tool 36
© COPYRIG
HT UPM
2.5.1 Response Surface Methodology 36
3 COMPARISON OF DIFFERENT EXTRACTION TECHNIQUES
FOR PRODUCTION OF ROSELLE CONCENTRATE 39
3.1 Introduction 39
3.2 Materials and Methods 42
3.2.1 Materials 42
3.2.2 Processing of roselle concentrate 43
3.2.3 Total anthocyanin content 44
3.2.4 Determination of pH, total soluble solids and 45
titratable acidity
3.2.5 Ascorbic acid extraction and HPLC separation 46
3.2.6 Determination of organic acid 47
3.2.7 Sensory evaluation 47
3.2.8 Identification session of sensory characteristics 48
3.2.9 Statistical analysis 50
3.3 Results and discussion 51
3.3.1 Total anthocyanin content 51
3.3.2 Ascorbic acid content 53
3.3.3 Organic acid 54
3.3.4 pH and titratable acidity 56
3.3.5 Sensory attributes 57
3.4 Conclusion 60
4 DEVELOPMENT OF ROSELLE CONCENTRATE FROM
OSMOTIC
SOLUTION USING RESPONSE SURFACE METHODOLOGY 62
4.1 Introduction 62
4.2 Materials and Methods 66
4.2.1 Roselle calyxes extraction process 66
4.2.2 Colour measurement 67
4.2.3 Total anthocyanin content 67
4.2.4 Sensory analysis 68
4.2.5 Experimental design and statistical analysis 69
4.3 Results and Discussion 70
4.3.1 Dependent variables of roselle concentrates 72
4.3.2 Effects of temperature, time and 80
sucrose solution concentration on the
© COPYRIG
HT UPM
a* value of roselle concentrate
4.3.3 Effects of temperature, time and sucrose 82
solution concentration on acidity
percentage of roselle concentrate
4.3.4 Effects of temperature, time and 84
sucrose solution concentration on the QDA
color of roselle extract
4.3.5 Effects of temperature, time and 86
sucrose solution concentration on the sharpness
of taste (determined by QDA) of roselle extract
4.4 Optimization 88
4.5 Conclusion 89
5 EFFECTS OF STORAGE TIME AND TEMPERATURE ON THE
QUALITY OF ROSELLE CONCENTRATE 91
5.1 Introduction 91
5.2 Materials and Methods 92
5.2.1 Roselle calyxes extraction process 92
5.2.2 Storage 93
5.2.3 Determination of pH and Titratable Acidity 94
5.2.4 Total anthocyanin content, color density, 95
degradation of anthocyanin
5.2.5 Colour measurement 95
5.2.6 Sensory analysis 96
5.2.7 Statistical analysis 96
5.3 Results and Discussions 97
5.3.1 Changes in colour quality – L value 97
5.3.2 Changes in a* value 98
5.3.3 Changes in anthocyanin content 99
5.3.4 Changes in colour density 101
5.3.5 Sensory evaluation-colour 105
5.3.6 Sensory evaluation-grassy odour 107
5.3.7 Sensory evaluation-fruity taste 107
5.3.8 Sensory evaluation-overall acceptability 109
5.4 Conclusion 110
6 SUMMARY AND RECOMMENDATION FOR 112
FUTURE RESEARCH
6.1 Summary 112
6.2 Recommendations 115
© COPYRIG
HT UPM
REFERENCES 118
BIODATA OF STUDENT 141
LIST OF PUBLICATIONS AND AWARDS 143
APPENDIX 144