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Direct Analysis of Volatile Compounds During Coffee and Tea Brewing with Proton Transfer Reaction Time of Flight Mass Spectrometry

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Direct Analysis of Volatile Compounds During Coffee and Tea Brewing with Proton Transfer Reaction Time of Flight Mass Spectrometry Direct analysis of volatile compounds during coffee and tea brewing with Proton Transfer Reaction Time of Flight Mass Spectrometry Cumulative Dissertation To obtain the academic degree doctor rerum naturalium (Dr. rer. nat.) of the Faculty of Mathematics and Natural Sciences of the University of Rostock by José Antonio Sánchez López Born on 08.02.1982 in Castellón de la Plana (Spain) Rostock, September 2016 1. Reviewer: Prof. Dr. Ralf Zimmermann Universität Rostock 2. Reviewer: Prof. Dr. Elke Richling Technische Universität Kaiserslautern Date of submission: 31.08.16 Date of defense: 17.01.17 ii ERKLÄRUNG Ich versichere hiermit an Eides statt, dass ich die vorliegende Arbeit selbstständig angefertigt und ohne fremde Hilfe verfasst habe. Dazu habe ich keine außer den von mir angegebenen Hilfsmitteln und Quellen verwendet und die den benutzten Werken inhaltlich und wörtlich entnommenen Stellen habe ich als solche kenntlich gemacht. Die vorliegende Dissertation wurde bisher in gleicher oder ähnlicher Form keiner anderen Prüfungsbehörde vorgelegt und auch nicht veröffentlicht. Rotterdam, 20 August 2016 ____________________ José Antonio Sánchez López iii iv CONTRIBUTION TO THE MANUSCRIPTS THAT FORM THIS CUMULATIVE THESIS José A. Sánchez‐López has been author of the following manuscripts. His contribution to each one is described below. Insight into the Time‐Resolved Extraction of Aroma Compounds during Espresso Coffee Preparation: Online Monitoring by PTR‐TOF‐MS Analytical Chemistry, Volume 86, Issue 23, 2014, Pages 11696–11704. DOI: 10.1021/ac502992k José A. Sánchez‐López designed and performed all the experiments. He also performed the data analysis and prepared the manuscript. His work to this publication accounts for approximately 90%. Extraction kinetics of coffee aroma compounds using a semi‐automatic machine: On‐line analysis by PTR‐ToF‐MS International Journal of Mass Spectrometry, Volume 401, 2016, Pages 22–30. DOI: 10.1016/j.ijms.2016.02.015 José A. Sánchez‐López was involved in the design and execution of the experiments. He performed the data analysis and prepared the manuscript. His work to this publication accounts for approximately 80%. Rapid and direct volatile compound profiling of black and green teas (camellia sinensis) from different countries with PTR‐ToF‐MS Talanta, Volume 152, 2016, Pages 45–53. DOI: 10.1016/j.talanta.2016.01.050 José A. Sánchez‐López was involved in the design and execution of the experiments. He collaborated on the data analysis and the preparation of the manuscript. His work to this publication accounts for approximately 40%. Extraction Dynamics of Tea Volatile Compounds as a Function of Brewing Temperature, Leaf Size and Water Hardness: On‐Line Analysis by PTR‐ToF‐MS. Submited to Talanta on 06.04.2016 José A. Sánchez‐López was involved in the design and execution of the experiments. He performed data analysis and prepared the manuscript. His work to this publication accounts for approximately 70%. Rotterdam, 20.08.2016 ___________________________________________ José Antonio Sánchez López v vi This thesis is based on work done in the time between April 2013 and March 2016 at the Institute of Chemistry and Biotechnology of the Zürcher Hochschule für Angewandte Wissenschaften and at the Division of Analytical Chemistry of the University of Rostock under supervision of Prof. Dr. R. Zimmermann. vii viii Acknowledgements First of all, I would like to thank Prof. Dr. Ralf Zimmermann for giving me the opportunity to conduct my PhD program under his supervision. I would also like to give special thanks to my thesis advisor Prof. Dr. Chahan Yeretzian, for his unconditional trust, allowing me to fully manage this research. I would like to thank my colleagues at the Analytical Chemistry department of ZHAW, especially to Dr. Marco Wellinger and Dr. Samo Smrke for their support, sharing their knowledge and the fruitful discussions in coffee science, analytical techniques and life in general. I would like to thanks Dr. Franco Biasioli for giving me the opportunity of perform some of my research in his group. Dr. Biasioli and his entire group make me feel like home. I would like to thank specially Dr. Sine Yener for working hand in hand with me, and showing me the beauty of Trentino and the Dolomites. I would like to acknowledge the PIMMS (Proton Ionisation Molecular Mass Spectrometry) ITN supported by the European Commission's 7th Framework Programme under Grant Agreement Number 287382. I would like to thank to Prof. Christopher Mayhew for all his effort starting this network and keeping it together. I am thankful for knowing all the members in this network, all the supervisors and ESRs. Special thanks to Michael Reber, for listening to all my complaints and providing me with coffee and beer when needed. Your friendship helped to survive to boring Wädenswil. And my greatest thanks to Eva Tarrasón, for not killing me when I moved to Switzerland and support me in all aspects of life. T’estim! ix x Abstract Coffee and tea are the two most consumed beverages in the world. Reasons for consuming them are varied and include the energy boost from their caffeine content, multiple health benefits and, above all, a pleasant sensory experience while drinking a cup of tea or coffee. Aroma is one of the main contributors to the sensory perception, and therefore of utmost importance for both coffee and tea. This thesis work focuses on the development of simple, fast, sensitive and reliable methods based on PTR-TOF-MS for the analysis of volatile organic compounds and how they are extracted into the liquid phase during the brewing of both coffee and tea. In a first study, an on-line method to analyze extracted volatiles directly from the coffee flow was developed and applied to the study of single dose coffee capsules. Volatile concentration could be followed at 1 Hz resolution during the 42 seconds that the coffee extraction last. Differences in extraction between compounds were revealed, implying an aroma profile that changed with extraction time. Coffee capsules could be differentiated according to their extraction profiles by unsupervised statistical methods (Principal component analysis, PCA; and Hierarchical Cluster Analysis, HCA). A follow up study was performed using a semi-automatic coffee machine and varying the brewing parameters (temperature and pressure). The different brewing conditions resulted in different time- intensity profiles that could be differentiated by PCA. Furthermore, all the compounds extracted were grouped according to their extraction profiles into 5 families by HCA and Self Organizing Three Algorithm (SOTA), with compounds in the same family sharing their physicochemical characteristics (mainly water solubility and volatility). An increase in either brewing pressure or temperature resulted in an increase in compound extraction. However, differences were only significant in the second part of the extraction (after 10-15 seconds) and more pronounced in the less polar compounds. In the case of tea, a preliminary study was performed in order to obtain the volatile profiles of a large number of commercial teas. In that study, an automated headspace sampling method was used in combination with PTR-TOF-MS to allow the screening of a large amount of samples in a short time. The aroma profiles of 63 black teas and 38 green teas were analyzed for both full leaves and the infusion obtained after brewing the leaves. Differences between leaves and infusions were found, indicating incomplete extraction of some compounds (e.g. terpenes) and formation of others (e.g. alcohols) during hot water extraction. Using multivariate analysis, black and green teas were successfully discriminated. Also the origin of the samples could be partially discriminated although with some miss-assignments, mainly between neighboring countries. The extraction of volatiles from tea leaves and how it is affected by several parameters (leaf size, temperature, brewing time and water composition) was further studied. Tea aliquots were taken every 30 seconds during five minutes and the headspace was analyzed with PTR-TOF-MS coupled to an autosampler. An increase in brewing temperature resulted in increased volatile extraction, with differences more pronounced at longer brewing times. Reduced leaf size resulted in faster extraction, a difference that was more significant during the first minute of brewing. On the other hand, water mineralization had low impact on the extraction kinetics and the volatile aroma content in the cup. Using PCA and HCA, not only the impact of brewing parameters was assessed but also different sets of brewing conditions resulting in analogous volatile profiles (i.e. same aroma profile) were identified. xi The positive outcomes of this thesis support the use of PTR-TOF-MS to follow the extraction of volatile aroma compounds during preparation of hot beverages, both on-line and off-line. The use of multivariate methods on the dynamic data increased the applicability of the methods allowing differentiation of samples according to its composition (e.g. coffee capsules), country of origin (e.g. tea origins) or parameters used for preparation (e.g. temperature-pressure combinations). xii Table of contents Acknowledgements ............................................................................................................................................................. ix Abstract ................................................................................................................................................................................
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