Quality Oriented Drying of Lemon Balm (Melissa Officinalis L.)
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FORSCHUNGSBERICHT AGRARTECHNIK des Fachausschusses Forschung und Lehre der Max-Eyth-Gesellschaft Agrartechnik im VDI (VDI-MEG) 498 Sandra Patricia Cuervo-Andrade Quality oriented drying of Lemon Balm (Melissa officinalis L.) Dissertation Witzenhausen 2011 ISSN 0931-6264 Universität Kassel Fachbereich Ökologische Agrarwissenschaften Fachgebiet Agrartechnik Prof. Dr. Oliver Hensel Quality oriented drying of Lemon Balm (Melissa officinalis L.) Dissertation zur Erlangung des akademischen Grades einer Doktorin der Agrarwissenschaften (Dr. agr.) von Dipl.-Ing. Sandra Patricia Cuervo-Andrade aus Bogotá, Kolumbien 2011 Die vorliegende Arbeit wurde vom Fachbereich Ökologische Agrarwissenschaften der Universität Kassel als Dissertation zur Erlangung des akademischen Grades „Doktorin der Agrarwissenschaften“ angenommen. Tag der mündlichen Prüfung: 21.03.2011 Erster Gutachter: Prof. Dr. Oliver Hensel Zweiter Gutachter: Prof. Dr. Werner Hofacker Mündliche Prüfer: PD Dr. Jens Gebauer PD Dr. Johannes Kahl Alle Rechte vorbehalten. Die Verwendung von Texten und Bildern, auch auszugsweise, ist ohne Zustimmung des Autors urheberrechtswidrig und strafbar. Das gilt insbesondere für Vervielfältigung, Übersetzung, Mikroverfilmung sowie die Einspeicherung und Verarbeitung in elektronischen Systemen. © 2011. Im Selbstverlag: Sandra Patricia Cuervo Andrade Bezugsquelle: Universität Kassel, FB Ökologische Agrarwissenschaften Fachgebiet Agrartechnik Nordbahnhofstr. 1a 37213 Witzenhausen Acknowledgements This work was developed in the department of agricultural engineering at the University of Kassel in Witzenhausen led by Prof.Dr.Oliver Hensel. I particularly want to thank to Prof.Dr. Oliver Hensel for his continued support in carrying out the work. His technical suggestions were crucial to the successful conclusion of the work. His good sense of humor always kept me motivated to continue and overcome the difficulties inherent in the research. I also want to thank to Prof.Dr. Werner Hofacker , to PD Dr. Jens Gebauer and to PD Dr. Johannes Kahl for their participation in the supervisory committee. A special gratefulness to the STIBET scholarship program for their financial support for the latest stage of my doctoral work. Special thanks to the members of the department of agricultural engineering in Witzenhausen, for their contributions and help during my stay in Germany, mainly to Christian, Heiko, Petra, Uwe and Franz. I appreciate the support of my friend Mr. Christian Schellert, who helped me both in technical and personal aspects during my stay in Witzenhausen. I thank to my friends for the support and to share cheerful times during my stay and that of my family in Germany. Especially to Sonia, Alexander, Javier, Esteban, Achim, Beatriz, Hernando, Victor and Yolanda. I thank my parents Socorro and Dionisio who have always offered me their support to achieve my formation goals. Also I want to thank to my husband Carlos Julio whose support was fundamental for the development and culmination of this project. Thanks to my children Juliana Patricia and Sebastian Camilo for their patience, great support and motivation also for the whole time that they have given me of their company to finish this work. Sandra Patricia Cuervo Andrade Witzenhausen, March 2011 Contents 1 Introduction 3 2 Problem outline 5 2.1 Background . 5 2.2 Problem de¯nition . 6 2.3 Research objectives . 8 2.4 Methodology . 9 3 State of the Art 11 4 Fundamentals 15 4.1 Importance and purposes of drying . 15 4.2 Drying process . 15 4.3 Water activity and sorption isotherms . 17 4.4 Kinetics of the drying . 18 4.5 Characteristics of Lemon Balm . 23 4.5.1 Uses of Lemon Balm . 24 4.5.2 Loss of essential oil . 24 4.5.3 Color change of leaves by drying . 25 4.5.4 Quality attributes of Lemon Balm . 25 5 Measurement of quality characteristics 27 5.1 Moisture Content Determination . 27 5.2 Essential oils content . 27 5.3 Measurement of Color . 28 6 Experimental determination and mathematical ¯tting of sorption isotherms 31 6.1 Materials and methods . 31 6.2 Results . 34 6.3 Mathematical models evaluation . 35 6.4 Analysis of results . 37 7 Drying kinetics 43 7.1 Materials and methods . 43 7.2 Results and discussion . 45 7.2.1 Influence of air drying temperature . 45 7.2.2 Influence of relative humidity . 49 7.2.3 Drying behavior for di®erent conditions of the product . 50 7.3 Fitting to mathematical models . 51 7.4 Behavior of the leaves temperature . 54 i Contents 8 Drying by using stepwise process control 55 8.1 Description of the process . 55 8.2 Materials and methods . 56 8.3 Results and discussion . 58 8.3.1 Drying curves . 58 8.3.2 Influence of temperature on drying time . 61 8.3.3 E®ects of drying on essential oil content . 62 8.3.4 E®ects of drying on color di®erence . 63 8.3.5 Energy consumption . 64 8.3.6 Process recommendation . 66 9 Multiobjective optimization of drying process 67 9.1 Materials and methods . 67 9.2 Experimental design and response surface methodology (RSM) . 68 9.3 Regression models . 72 9.3.1 Drying time . 72 9.3.2 Color di®erence . 75 9.3.3 Essential oil content . 77 9.3.4 Required energy . 79 9.4 Multiobjective process optimization . 81 9.4.1 Drying time as priority . 83 9.4.2 Essential oil content as priority . 85 9.4.3 Color di®erence as priority . 86 9.4.4 Required energy as priority . 88 9.4.5 Same priority for all responses . 89 9.4.6 Quality characteristics as priorities . 91 10 E®ect of solar drying parameters on quality characteristics 95 10.1 Description of process and equipment . 95 10.2 Materials and methods . 97 10.3 Experimental design . 98 10.4 Results and discussion . 100 10.4.1 Drying time . 100 10.4.2 Color di®erence . 103 10.4.3 Essential oil content . 104 10.5 Regression models . 107 10.5.1 Drying time . 107 10.5.2 Color di®erence . 110 10.5.3 Essential oil content . 113 11 Overall discussion 117 11.1 Sorptions isotherms . 117 11.2 Drying kinetics . 117 11.3 Drying by stepwise . 118 11.4 Optimization of drying . 119 11.5 Solar drying . 120 ii Contents 12 Summary 121 13 Zussamenfasung 123 Bibliography 125 A Chi-square test and determination coe±cient 137 B Polynomial regression in multiobjective optimization of drying process 138 C Regression models for quality characteristics in solar drying 142 C.1 Drying time . 143 C.2 Color di®erence . 143 C.3 Essential oil content . 144 iii Nomenclature Symbol Unit Meaning aw - Water activity A m2 Area Ao Empirical coe±cient Ci kj=kgh speci¯c heat Co - Covering D - Overall desirability d - Individual desirability 2 Dm m =s Di®usion coe±cient d:m: Dry matter d(y) Desirability function DR - Dimensionless drying rate Ko coe±cient 2 Ld g=m Drying Load M g Mass ma kgair=h Mass flow rate MCw:b: % Moisture content (wet base) MR Moisture ratio mw g Mass of water Oc % Essential oil content QW Heat transferred qr kJ Required energy R2 Determination coe±cient Rd gwater=gd:mh Drying rate 1 Contents Symbol Unit Meaning t h Time td h Drying time T K Temperature Va m=s Air velocity x m Distance X gwater=gd:m Moisture content (dry base) Xe Equilibrium moisture content Xo Initial moisture Xp m Position in solar tunnel L¤ - Brightness b¤; a¤ - Chromatic coordinates ¢E - Color di®erence ' % Relative humidity υ ±C Drying temperature Acronyms Meaning EMC Equilibrium moisture content MSI Moisture sorption isotherm RSM Response surface methodology CCD Central composite design 2 1 Introduction The ¯rst objective of drying is to remove water and hence to stabilize the biological products. However, during drying of medicinal plants, many changes occur simultaneously resulting in a modi¯ed overall quality. In general, drying leads to reduction of visual, organoleptic and functional characteristics that a®ect signi¯catively the ¯nal quality. Reactions lead to well-known changes in the fresh biological products during drying: change of color, loss of aroma, textural changes, reduction of essential oil content, cracking and altering of shape. These reactions are caused by both the increase in product temperature and the removal of moisture. For these reasons, it is necessary to purpose adequate drying strategies and to known the optimal values of the process parameters in order to obtain the required quality characteristics and the decrease of the energy consumption. This research work is related to the quality oriented drying of Lemon Balm (Melissa o±cinalis L.). Di®erent strategies and aspects have been considered and treated experi- mentally and mathematically in order to obtain the best conditions to reach an adequate productivity and the required quality characteristics in terms of color change and essential oil content. In Chapter 2 relevant aspects of problem outline are presented. The chapter is focused on background of the problematic and the problem de¯nition which describes the consequences on quality due to an inadequate selection of drying parameters in processing medicinal plants by using dryers based on forced convection with hot air and solar tunnels. Starting from this problem de¯nition, the research objectives and the methodology are purposed. The methodology considers the obtaining of sorption isotherms and drying kinetics of lemon Balm and the corresponding ¯tting to mathematical models. Likewise a stepwise drying strategy was analyzed as alternative to obtain better results in terms of quality and energy consumption. Additionally an experimental design by using response surface methodology was purposed for multi objective optimization of quality characteristics and required energy. Finally, in order to observe the influence of drying parameters on product quality by using a solar tunnel, design of experiments techniques were considered. In Chapter 3 presents the state of the art, contempled as main aspect the research on drying of medicinal plants focused on Lemon Balm; sorption models, techniques for the determination of quality characteristics, analysis of drying process and e®ects of drying on quality and strategies for quality drying and energy saving.