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ABSTRACT YOKUS, MURAT A. Multiplexed Biochemical And ABSTRACT YOKUS, MURAT A. Multiplexed Biochemical and Biophysical Sensing Systems for Monitoring Human Physiology. (Under the direction of Dr. Michael A. Daniele and Dr. Tushar Ghosh). Noninvasive access to biochemical biomarkers of human physiology is one of the most challenging tasks in digital health. Today, measurement of the biomarkers of health, wellness, or even diseases requires frequent lab visits for routine blood or urine test panels for full-body screening. Treatment or medical prescription is usually provided based on the measured metrics and patient’s recall of symptoms. However, some of these test panels are still deemed invasive, painful, or inconvenient, and most importantly, they do not offer real-time measurement physiological data. Thus, addressing these challenges requires the development of multiplexed wearable systems that converge biochemical and biophysical sensing functionalities into a single platform and provide real-time measurement of biomarkers of human physiology in daily settings. In this dissertation, we provide wireless, wearable health monitoring systems that can noninvasively and continuously measure the biomarkers of human physiology. The developed systems can measure metabolites (glucose, lactate), pH, and other physical signals (skin temperature, heart rate, and tissue oxygenation) via electrochemical sweat analysis and optical methods. The dissertation introduces the fabrication of flexible sensing arrays, fabrication and characterization of biosensors, design and validation of the wearable electronic systems, and off- body multiplexed analysis of artificial and collected real sweat samples. The developed wearable systems provide multimodal, noninvasive analysis of biomarkers of metabolism and respiration, extending its applications from diet management and performance monitoring to the prolonged assessment of overall health and wellness in ambulatory settings. © Copyright 2020 by Murat Abdurrahim Yokus All Rights Reserved Multiplexed Biochemical and Biophysical Sensing Systems for Monitoring Human Physiology by Murat A. Yokus A dissertation submitted to the Graduate Faculty of North Carolina State University in partial fulfillment of the requirements for the degree of Doctor of Philosophy Electrical Engineering & Fiber and Polymer Science Raleigh, North Carolina 2020 APPROVED BY: _______________________________ _______________________________ Dr. Michael A. Daniele Dr. Tushar Ghosh Committee Co-Chair Committee Co-Chair _______________________________ _______________________________ Dr. Alper Bozkurt Dr. Veena Misra DEDICATION To my family for their endless support ii BIOGRAPHY Murat Yokus received a B.Sc. degree in Textile Engineering (summa cum laude) with a minor in Industrial Engineering in 2011 from Uludag Univesity in Turkey. He completed the last year of his bachelor’s degree at Polytechnic University of Valencia (Spain) and the University of Manchester (England). Later that year, he received Fulbright Scholarship from the U.S. Department of State's Bureau of Educational and Cultural Affairs to pursue his M.Sc. degree in Textile Engineering at North Carolina State University. Then, he pursued a Ph.D. program at North Carolina State University, majoring in Electrical Engineering and co-majoring in Fiber and Polymer Science. He initially worked in NEXT Research Group on wearable electronic textiles. Afterward, he joined BioInterface Lab under the direction of Dr. Michael Daniele. His research interests include wearable and implantable electronics, biosensors, and integrated circuit design for biomedical applications. iii ACKNOWLEDGMENTS First, I would like to thank my advisor and a close friend, Dr. Michael Daniele. Four and half years ago, you gave me the opportunity to join the BioInterface Lab and supported my ideas and research interest. I am very thankful for your help and guidance throughout my graduate studies. I am very grateful for your time and effort in transitioning me to an independent researcher. I also would like to thank the rest of my advisory committee members for their guidance and support: Dr. Alper Bozkurt, Dr. Tushar Ghosh, Dr. Veena Misra, and Dr. Brendan O’Connor. Specifically, I would like to thank Dr. Ghosh for being my dissertation co-chair and Dr. Bozkurt for the helpful research discussions throughout my Ph.D. This research has been possible with funding from the NSF Engineering Research Center for Advanced Self-Powered Systems of Integrated Sensors and Technologies (ASSIST). I would like to thank everyone in the ASSIST Center, Veena, Mehmet, Tom, Casey, Elena, Roy, Jason, Scott, Clay, for providing the students with the resources for professional and personal development. Special thanks to Dr. Rajinder Khosla and Dr. Mehmet Ozturk for the pleasant talks. To staff and individuals of the NNF, AIF, ECE department, BME department, and College of Textiles, thank you for providing assistance and training for the tools and equipment. Your expertise allowed me to learn the required skills needed for the research in this dissertation. I would like to extend my sincere thanks to my research collaborators, Talha Agcayazi, Tanner Songkakul, and Tamoghna Saha, for their great friendship and significant contribution to the work presented in this dissertation. I would like to thank the undergraduates who afforded me the chance to mentor them (Kristi, Nathan, Rachel, Grace, Cheyanne, Kendal, and Matt). Special thanks to Rachel Foote for her excitement and contribution to the research on stretchable printed interconnects. iv To all of the BioInterface Lab, iBionics Lab, and NEXT Research Lab members, thanks for making the labs an exciting place to learn and explore. Your friendship and useful research discussions will not be forgotten. Special thanks to Ashlyn Young, Vladimir Pozdin, Parthiban Rajan, James Dieffenderfer, Talha Agcayazi, Tanner Songkakul, Peter Sotory, Evan Williams, Parvez Ahmmed, Tahmid Latif, Michael McKnight, Ryan Hodges, Halil Akyildiz, and Jonathan Halbur. All the students from the ASSIST Center, Francisco, Michael Lim, Abhishek, Tim, Saba, Amanda, Namita, Jose, Rita, Akhilesh, Xiao Zhang, Marzana, Michael Wilkins, Rafael Silva…. and everyone else, thanks for the enjoyable moments and great memories. I also would like to thank to the Turkish community and friends, Alper, Safak, Rana, Halil, Ozkan, Emrah, Ramiz, Serdar, Mehmet, Nihat, Musab, Tugrul, Elif, and Cemile, for their friendship and great memories. My concluding statement of the most profound gratitude is for my family. Thank you, dad, thank you, mom, and thank you, my dear sisters. I couldn’t be here where I am today without your help, support, and guidance throughout my life. Thank you. v TABLE OF CONTENTS LIST OF TABLES ..................................................................................................................... viii LIST OF FIGURES ..................................................................................................................... ix CHAPTER 1: Introduction ........................................................................................................ 1 1.1. Objective ............................................................................................................................. 1 1.2. Dissertation Outline ............................................................................................................ 4 CHAPTER 2: Literature Review ............................................................................................... 7 2.1. Introduction ........................................................................................................................ 7 2.2. Wearable Biochemical Sensors ........................................................................................ 12 2.2.1. Sweat Extraction and Sampling Methods in Wearable Sensors ................................ 12 2.2.2. Biochemical Sensing in Current Wearable Devices .................................................. 18 2.2.2.1. Metabolites ......................................................................................................... 18 2.2.2.2. pH and Electrolytes ............................................................................................ 24 2.2.2.3. Oxygen ............................................................................................................... 28 2.2.2.4. Other Chemical Biomarkers ............................................................................... 33 2.3. Wearable Biophysical Sensors ......................................................................................... 35 2.3.1. Sweat Rate ................................................................................................................. 35 2.3.2. Temperature ............................................................................................................... 40 2.4. Wearable Systems with Multimodal Sensing ................................................................... 42 2.5. Summary and Outlook ...................................................................................................... 46 2.6. References ........................................................................................................................ 50 CHAPTER 3: Wearable Multiplexed Biosensor System Toward Continuous Monitoring of Metabolites ...................................................................................................... 61 3.1. Abstract ............................................................................................................................
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