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UNIVERSITI PUTRA MALAYSIA

MOHAMED NAZIM BIN ANVARALI

FSTM 2013 1

PRODUCTION, OPTIMIZATION, CHARACTERIZATION AND STORAGE STABILITY OF ROSELLE CONCENTRATE

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PRODUCTION, OPTIMIZATION,

CHARACTERIZATION AND STORAGE

STABILITY OF ROSELLE CONCENTRATE


MASTER OF SCIENCE

UNIVERSITI PUTRA MALAYSIA

2013

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PRODUCTION, OPTIMIZATION, CHARACTERIZATION AND

STORAGE STABILITY OF ROSELLE CONCENTRATE

By


Thesis Submitted to the School of Graduate Studies, Universiti Putra

Malaysia, in Fulfilment of the Requirements for the Degree of Master

Science

February 2013

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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

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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


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

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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

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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.

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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


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

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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

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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.

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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.

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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

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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



(Internal Examiner)

Yus Aniza Yusof, PhD

Associate Professor

Faculty of Engineering


(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


Date:

http://foodclicks.upm.edu.my/dbase/academician/papar_cv_user.php?id=A00875

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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



(Chairman)

Nazimah Binti Sheikh Abdul Hamid, PhD

Lecturer



(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


Date:

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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.


Date: 22 February 2013

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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

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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


3.3.2 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


4.2.1 Roselle calyxes extraction process 66

4.2.2 Colour measurement 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

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a* value of roselle concentrate

4.3.3 Effects of temperature, time and sucrose 82

solution concentration on acidity

percentage of roselle concentrate


sucrose solution concentration on the QDA

color of roselle extract


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


5.2.1 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

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