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Development and Characterization of Biodegradable Sutures Made DEVELOPMENT AND CHARACTERIZATION OF BIODEGRADABLE SUTURES MADE OF ELECTROSPUN FIBERS WITH AMPICILLIN by HANG LIU (Under the Direction of Dr. Karen K. Leonas) ABSTRACT Surgical sutures are one of the most frequently used devices in emergency rooms and operating theatres. Due to the large number of surgical site infections caused by suture implantations, there is an increasing need for the application of sutures with antimicrobial properties, especially biodegradable sutures with the controlled release of antimicrobial agents. A study was carried out to develop these suture fibers by electrospinning and evaluate selected properties of the fibers. As electrospinning is a relatively new spinning method and fundamental understanding of the technique has not been established, the spinning process and the influence of the processing parameters on the fiber properties were studied as well. Polycaprolactone, a biodegradable polymer used in biomaterials approved by the Food and Drug Administration (FDA), was the polymer selected. The antimicrobial agent, which was incorporated in the polymer solution to provide the produced fibers with antimicrobial properties, was ampicillin sodium salt. The selected fiber properties included physical and mechanical properties, antimicrobial properties, and the release of ampicillin from the fibers, as well as biodegradation properties. One of the major goals of the study was to establish methodologies to collect and characterize electrospun nanofibers, which could be physically manipulated as required for suture applications. The use of a thin disk as the electrospinning collector to collect nanofiber bundles has been proved to be a feasible method to achieve this goal. Other findings of the dissertation included the following. Fibers with a wide range of diameters and percentages of crystallinity could be produced by varying the polymer solution properties (the polymer concentration and the addition of ampicillin sodium salt) and the spinning processing parameters (voltage, feedrate, and the distance from the needle tip to the collector). The as-spun fibers showed antimicrobial effectiveness on both S. aureus and K. pneumoniae . The ampicillin release was completed in 96 hours. The mass loss of degraded fibers was less than 3% in 12 weeks, but surface morphological changes were observed in samples that had been exposed to the biodegradation environment for six weeks. INDEX WORDS: Electrospinning, Surgical sutures, Antimicrobial properties, Degradation properties, Nanofibers DEVELOPMENT AND CHARACTERIZATION OF BIODEGRADABLE SUTURES MADE OF ELECTROSPUN FIBERS WITH AMPICILLIN by HANG LIU B.S., China Textile University, China, July 1999 M.S., DongHua University, China, March 2002 A Dissertation Submitted to the Graduate Faculty of The University of Georgia in Partial Fulfillment of the Requirements for the Degree DOCTOR OF PHILOSOPHY ATHENS, GEORGIA 2008 © 2008 Hang Liu All Rights Reserved DEVELOPMENT AND CHARACTERIZATION OF BIODEGRADABLE SUTURES MADE OF ELECTROSPUN FIBERS WITH AMPICILLIN by HANG LIU Major Professor: Karen K. Leonas Committee: Helen H. Epps Joy B. Doran Peterson Guigen Zhang Yiping Zhao Electronic Version Approved: Maureen Grasso Dean of the Graduate School The University of Georgia August 2008 iv DEDICATION The dissertation is dedicated to my dear parents: Liu, Huizhong and Yu, Wenqing for their selfless and forever love. v ACKNOWLEDGEMENTS There are so many people that I would like to thank, who paved the way along with me to make this dissertation a success. Foremost, sincere thanks to my major professor, Dr. Karen Leonas, for her great insight in the planning of the research and her substantial assistance and guidance throughout my entire course of study at the University of Georgia, especially for her long-distance direction from Pullman, Washington in the last year. Special thanks to my committee members, Dr. Helen Epps, Dr. Joy Peterson, Dr. Guigen Zhang and Dr. Yiping, Zhao, who have provided valuable suggestions, ideas and supports from various aspects. Thanks for their willingness to assist me in the past three years. I am grateful to the faculty and staff in the department of Textiles, Merchandising and Interiors and the researchers and students in Dr. Yiping Zhao’s research group for their kindness and assistance. I would also like to thank AATCC Research Foundation for providing financial support for this project. My deep appreciation goes to my lovely families, my parents for their love and endless support, my sister for taking care of our parents to give me a peace mind from halfway around the globe. At last but not the least, I would like to thank my husband Ting Chi, for his emotional support and confidence on me. Without the help of any of them, it would not be possible for me to successfully complete the dissertation. THANKS! vi TABLE OF CONTENTS Page ACKNOWLEDGEMENTS.............................................................................................................v LIST OF TABLES....................................................................................................................... viii LIST OF FIGURES ....................................................................................................................... ix CHAPTER 1 Introduction....................................................................................................................1 1.1 Statement of Problem ..........................................................................................3 1.2 Objectives............................................................................................................5 2 Literature Review...........................................................................................................6 2.1 Sutures.................................................................................................................6 2.2 Sutures Commercially Available on Markets .....................................................6 2.3 Properties of Sutures ...........................................................................................7 2.4 Surgical Site Infections & Biofilm Formation on Sutures ................................23 2.5 Antimicrobial Agents and Their Working Mechanisms ...................................25 2.6 Sutures with Antimicrobial Properties ..............................................................27 2.7 Manufacturing of Synthetic Sutures..................................................................32 2.8 Electrospinning..................................................................................................33 3 Materials and Methods.................................................................................................49 3.1 Methodology .....................................................................................................49 3.2 Materials............................................................................................................50 vii 3.3 Methods.............................................................................................................53 4 Results and Discussion ................................................................................................68 4.1 Apparatus Design and Preliminary Experiment................................................68 4.2 Influence of the Spinning Parameters on Fiber Properties................................83 4.3 Physical and Mechanical Properties of Fibers ................................................101 4.4 Antimicrobial Properties and the Release of Ampicillin from Fibers.............113 4.5 Biodegradation Properties of Fibers................................................................129 5 Conclusion and Future Work.....................................................................................141 5.1 Conclusion.......................................................................................................141 5.2 Recommendations for Future Work ................................................................145 REFERENCES ............................................................................................................................147 APPENDICES .............................................................................................................................160 A The Influence of Spinning Parameters on Fiber Diameters.......................................160 B The influence of Ampicillin Concentration on Percentage of Crystallinity of Fibers ...............................................................................................................................170 C The Influence of Ampicillin Concentration on Yarn Tensile Properties...................172 viii LIST OF TABLES Page Table 2.1: Commercially Available Synthetic Absorbable Suture Materials..................................9 Table 2.2: Mechanical Properties of Absorbable Sutures..............................................................11 Table 2.3: Suture Size Classification.............................................................................................13 Table 3.1: Physical Properties of Chloroform and Methanol ........................................................51 Table 3.2: Absorbance of Ampicillin PBS Solution with Various Concentrations.......................64 Table 4.1: Diameter of Fibers Spun with Pure PCL......................................................................86 Table 4.2: Diameter of Fibers Spun with PCL Plus 5% Ampicillin..............................................86
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