UNIVERSITI PUTRA MALAYSIA

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1 UNIVERSITI PUTRA MALAYSIA OPTIMISED APPLICATION OF THE MICROWAVE EXTRACTION TECHNIQUE OF ESSENTIAL OILS FROM AQUILARIA MALACCENSIS LAMK WOOD AND CYMBOPOGON NARDUS (L.) RENDLE LEAVES BIBI SABRINA BINTI YAHAYA FS

2 OPTIMISED APPLICATION OF THE MICROWAVE EXTRACTION TECHNIQUE OF ESSENTIAL OILS FROM AQUILARIA MALACCENSIS LAMK WOOD AND CYMBOPOGON NARDUS (L.) RENDLE LEAVES By BIBI SABRINA BINTI YAHAYA Thesis Submitted to the School of Graduate Studies, University Putra Malaysia, in Fulfillment of the Requirements for the Degree of Master of Science May 2011

3 Abstract of thesis presented to the Senate of University Putra Malaysia in fulfillment of the requirement for the degree of Master of Science OPTIMISED APPLICATION OF THE MICROWAVE EXTRACTION TECHNIQUE OF ESSENTIAL OILS FROM AQUILARIA MALACCENSIS LAMK WOOD AND CYMBOPOGON NARDUS (L.) RENDLE LEAVES Chairman Faculty By BIBI SABRINA BINTI YAHAYA May 2011 : Prof. Haji Kaida bin Khalid, PhD. : Science In this study, the important process parameters such as microwave power, temperature and extraction time of MET are controlled to obtain the highest yield of extracted essential oil. The microwave extraction method for the essential oil from gaharu and citronella grass is compared with the conventional extraction technique (CET). In such a way to obtain the first droplet of distillation, it is necessary to heat up only 10 to 13 minutes with MET against 25 to 45 minutes with CET for Aquilaria malaccensis wood while for Cymbopogon nardus extraction, it requires 3 to 7 minutes for MET and about 12 to 20 minutes for CET to obtain the first droplet of oil. After 1 hour of extraction, MET gives higher percentage yield of oil with 0.016% for wet distillation for Aquilaria malaccensis and 1.21% for Cymbopogon nardus while the percentage yield of oil obtained by the CET is only 0.140% for Aquilaria malaccensis and 3.51% for Cymbopogon nardus after 8 hours of extraction. Another parameter is day of soaking for the samples. It plays an important role in the extraction where by the long time the sample was soaked, the more yield were collected. The highest yield was 0.116% which ii

4 obtained in ten days of soaking. Identification of the chemical component was based on comparison of calculated retention indices and mass spectral data with literature values. The tested result of the oils showed some variation and differences in terms of GC profiles, concentration and chemical derivatives. In gaharu essential oil, the composition of oil isolated by the hydro distillation (MET) is dominated by dodecanoic acid, ethenyl ester, lauric acid, and vinyl ester yielding 12.75%. while in citronella essential oil, the composition is dominated by 6-octenal, 3,7-dimethyl and citronellal yielding 24.68% This project is also looking for the various techniques of extraction process such as hydro (HD), dry (DD) and steam (SD) distillation techniques. The results from each technique were presented. The project has successfully proved that MET is more efficient than CET in terms of rapidity and the quantity of the yield. iii

5 Abstrak tesis yang dikemukakan kepada Senat sebagai memenuhi keperluan untuk ijazah Master Sains APLIKASI OPTIMUM MIKRO GELOMBANG BAGI PENGEKSTRAKAN MINYAK PATI DARIPADA KAYU AQUILARIA MALACCENSIS LAMK DAN DAUN CYMBOPOGON NARDUS (L.) RENDLE Pengerusi Fakulti Oleh BIBI SABRINA BINTI YAHAYA Mei 2011 : Profesor Haji Kaida bin Khalid PhD. : Sains Dalam kajian ini, parameter-parameter proses penting seperti kuasa mikrogelombang, suhu dan masa dalam MET dikawal sepanjang proses pengekstrakan untuk memperoleh ekstrak minyak pati yang maksimum dan berkualiti tinggi. Kaedah mikrogelombang (MET) untuk ekstrak minyak pati dari kayu gaharu dan daun serai wangi dibandingkan dengan kaedah lama atau Conventional Extraction Technique (CET). Didapati titisan minyak pati pertama yang jatuh untuk adalah antara minit ke-10 dan ke-13 bagi MET dan antara minit ke 25 dan minit ke 45 bagi CET untuk sampel Aquilaria malaccensis. Manakala bagi sampel Cymbopogon nardus pula, adalah antara minit ke-3 dan minit ke- 7 untuk MET dan antara minit ke-12 hingga minit ke-20 untuk CET. Selepas tempoh pengekstrakan selama 60 minit menggunakan gelombang mikro MET memberikan peratusan ekstrak yang lebih tinggi dengan 0.016% bagi Aquilaria malaccensis dan 1.21% untuk Cymbopogon nardus, manakala peratusan hasil ekstrak daripada CET hanya 0.14% untuk Aquilaria malaccensis dan 3.51% bagi Cymbopogon nardus selepas tempoh 8 jam tempoh pengekstrakan. Parameter lain adalah hari rendaman untuk iv

6 sampel. Hal ini memainkan peranan penting dalam pengekstrakan di mana lebih lama sampel direndam, hasil lebih banyak minyak diperoleh. Keputusan tertinggi adalah 0.116% yang diperoleh dalam sepuluh hari rendaman. Komponen kimia dikenalpasti melalui perbandingan pengiraan indeks retensi dan data spektrum jisim dengan nilai rujukan. Keputusan ujian menunjukkan beberapa variasi dan perbezaan dalam profil GC, kepekatan dan terbitan bahan kimia. Dalam minyak pati gaharu, komposisi minyak yang diperoleh dari penyulingan basah (MET) didominasi oleh asid dodecanoic, ester etenil, asid laurik, dan ester vinyl menghasilkan 12.75%. Manakala dalam minyak pati serai, komposisi didominasi oleh 6-octenal, dimetil 3,7-dan citronelal menghasilkan 24.68%. Projek ini juga mengenalpasti pelbagai teknik penyulingan seperti hidro (HD), kering (DD) dan wap (SD). Hasil kajian bagi setiap teknik dibentangkan. Projek ini telah berjaya membuktikan bahawa proses MET lebih cekap berbanding CET dari segi kecekapan dan kuantiti hasil ekstrak. v

7 ACKNOWLEDGEMENTS Alhamdulillah, all praise is due to Allah. In the name of Allah Most Gracious, Most Merciful that always opens to us the path of knowledge and Him who has given me strength and patience to finish my Masters degree. I would like to express my deepest gratitude to my beloved supervisor Professor Dr. Haji Kaida bin Khalid who is also the Chairman of the Research Committee for his countless support, invaluable thoughts, brilliant suggestions and patience throughout my Masters program. His infinite knowledge guided my research on some parts on occasions. Also, I would like to express my appreciation and special thanks to my co-supervisor, Professor Dr. Haji Aspollah Haji Md. Sukari for his help, guidance and knowledge throughout the research. I would like to thank University s Research Park (TPU) for the samples supplied. I would also like to thank all the lecturers and staff of Pyhsics Department, UPM especially the Applied Electromagnetic Lab staff, En. Roslim and En. Zulambiar and also the staff from Chemistry department especially En. Abbas, En. Isharuddin and En. Zainal for their various practical help and encouragement throughout the study. My deepest gratitude to my labmates for the invaluable help and co-operation in sharing information and ideas concerning my dissertation and to others who had helped me throughout this project. Thank you to those who are involved directly or indirectly in this project. I am blessed that we had have such a beautiful friendship and support of many people throughout my studies. Last but not least my sincere gratitude to my family especially my beloved parents, Juma Bee Abdul Hamid and my late father for their prayers, love and supports. May Allah bless them and reward them all the best rewards Herein and Hereafter. vi

8 I certify that a Thesis Examination Committee has met on 27 May 2011 to conduct the final examination of Bibi Sabrina binti Yahaya on her thesis entitled Optimized Application of the Microwave Extraction Technique of Eessential Oils from Aquilaria malaccensis Lamk. Wood and Cymbopogon nardus (L.) Rendle Leaves in accordance with the Universities and University Colleges Act 1971 and the Constitution of the [P.U.(A) 106] 15 March The committee recommends that the student be awarded the Master of Science. Member of the Thesis Examination Committee were as follows: Mansor b. Hashim, PhD. Associate Professor Faculty of Science (Chairman) Azmi b. Zakaria, PhD Professor Faculty of Science (Internal Examiner) Jumiah bt Hassan, PhD Associate Professor Faculty of Science (Internal Examiner) Sahrim b. Haji Ahmad, PhD Professor Faculty Science and Technology Universiti Kebangsaan Malaysia Malaysia (External Examiner) SHAMSUDDIN SULAIMAN, PhD Professor and Deputy Dean School of Graduate Studies Date: vii

9 This thesis was submitted to the Senate of and has been accepted as fulfillment of the requirement for the degree of Master of Science. The members of the Supervisory Committee were as follows: Kaida bin Khalid, PhD Professor Faculty of Science (Chairman) Mohd Aspollah Hj Md. Sukari, PhD Professor Faculty of Science (Member) HASANAH MOHD GHAZALI, PhD Professor and Dean School of Graduate Studies Date: viii

10 DECLARATION I hereby declare that the thesis is my original work except for quotations and citation which have been duly acknowledged. I also declare that it has not been previously and is not concurrently submitted for any other degree at or other institutions BIBI SABRINA BINTI YAHAYA Date: 27 May 2011 ix

11 TABLE OF CONTENTS ABSTRACT ABSTRAK ACKNOWLEDGEMENTS APPROVAL DECLARATION LIST OF TABLES LIST OF FIGURES LIST OF SYMBOLS AND ABBREVIATIONS CHAPTER I II III Page ii iv vi vii ix x xii xv INTRODUCTION Research Background 1 Research Benefits and Potential 5 Literature Review Essential Oil 5 Manufacturing of Essetial Oils 6 Microwave Extraction Technique (MET) 7 Conventional Extraction Method ofagarwood Oils 8 and Citronella Oil Introduced Technique: Microwave Extraction System (MES) 10 Problem Statement 13 Objective 13 Thesis Contents 14 LITERATURE REVIEW Introduction 15 Gaharu Wood and Citronella Grass 16 Microwave Assisted Extraction 18 Conventional Heating Method 25 Conclusion 27 THEORY Introduction 28 Microwaves in General 29 Microwave Oven Energy Efficiency 30 How Microwaves in a Microwave Oven Works 30 Interaction between Microwaves and Materials 31 Dipole Rotation or Orientation Interaction 36 Dielectric Properties of Water 37 Heating and Drying Process in Microwave Oven Cavity 40 Absorption Power 42

12 Page IV Dielectric Mixture Model 44 Moisture Content of Sample 47 Estimation of Absorption Power of Mixture Fresh Woods 49 or Leaves, (PA/Vol) in (mfw) during DD and WD Input Data Calculate power output of heating source 50 Dielectric properties of water, ε * w at specific frequency 52 (0.13 GHz< T w =2.45GHz<20GHz) and temperature (26 o C<T w =90 o C<100 o C) Calculation of electric field strength inside the 54 microwave oven cavity Dielectric properties of mixture fresh woods 55 or leaves Dielectric properties of mixture fresh woods and fresh leaves 55 during DD and WD Electric field strength inside the mixture fresh woods 56 during DD and WD Absorption power inside the mixture fresh woods and fresh leaves 56 during DD and WD New absorption power inside of mixture fresh wood or leaves 57 during DD and WD Power Measurement Techniques 57 MATERIALS AND METHODOLOGY Introduction 61 Sample Preparation Method 64 Sample- Aquilaria malaccensis and Cymbopogon nardus 65 Methodology Moisture Content Measurements 66 Dielectric Measurements 69 Essential Oil Extraction 73 Microwave Extraction Method 74 Conventional Extraction Method 75 Chemical Analysis 84 Experimental Errors 86

13 V VI Page RESULTS AND DISCUSSION Introduction 88 Results of Moisture Content 89 Results of Dielectric Properties and Power Absorption 91 Results of Extraction and Chemical Analysis 102 CONCLUSION Further Research 113 REFERENCES 118 APPENDICES 123 BIODATA OF STUDENT 157 LIST OF PUBLICATIONS 158