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Classification of Silicone-Based Personal and Condom Lubricants Using Dart-Tofms

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Classification of Silicone-Based Personal and Condom Lubricants Using Dart-Tofms University of Central Florida STARS Electronic Theses and Dissertations, 2004-2019 2016 Classification of Silicone-Based ersonalP and Condom Lubricants Using DART-TOFMS Lauren Harvey University of Central Florida Part of the Forensic Science and Technology Commons Find similar works at: https://stars.library.ucf.edu/etd University of Central Florida Libraries http://library.ucf.edu This Masters Thesis (Open Access) is brought to you for free and open access by STARS. It has been accepted for inclusion in Electronic Theses and Dissertations, 2004-2019 by an authorized administrator of STARS. For more information, please contact [email protected]. STARS Citation Harvey, Lauren, "Classification of Silicone-Based ersonalP and Condom Lubricants Using DART-TOFMS" (2016). Electronic Theses and Dissertations, 2004-2019. 5257. https://stars.library.ucf.edu/etd/5257 CLASSIFICATION OF SILICONE-BASED PERSONAL AND CONDOM LUBRICANTS USING DART-TOFMS by LAUREN ASHLEY HARVEY B.S. University of Central Florida, 2016 A thesis submitted in partial fulfillment of the requirements for the degree of Master of Science in the Department of Chemistry in the College of Science at the University of Central Florida Orlando, Florida Fall Term 2016 Major Professor: Candice Bridge © 2016 Lauren A. Harvey ii ABSTRACT Sexual lubricants are used to enable sexual encounters. There are different types of sexual lubricants such as water-based, oil-based, and silicone-based. They come pre-applied to condoms and separately in bottles as personal lubricants. Although sexual lubricants are intended for consensual use, they are also unfortunately used during the commission of sexual assaults. The analysis of sexual lubricants facilitates sexual assault investigations. With the increased usage of condoms in sexual assault cases, the potential of collected DNA evidence in each case is reduced. In the absence of biological evidence, the presence of sexual lubricants after a sexual assault can provide an additional link between a suspect and the crime scene and/or victim. Having the ability to compare known and unknown sexual lubricants may be the only actionable information available for investigators. Current lubricant analysis only classifies samples into lubricant types based on the major component such as glycerol, petrolatum, and polydimethylsiloxane for water-based, oil-based, and silicone-based lubricants respectively. Differentiation within major types has not been explored. Previously, protocols have been developed to detect and categorize personal lubricants using Fourier transform infrared (FTIR) spectroscopy, gas chromatography-mass spectrometry (GC-MS), liquid chromatography mass spectrometry (LC-MS), and pyrolysis GC-MS. FTIR is routinely used as a screening tool to detect peaks of the major lubricant components and the mass spectrometry (MS) techniques are commonly used to confirm the presence of some of the major components, excluding PDMS. This thesis focused on the differentiation of silicone-based personal and condom lubricants because it is a common type of lubricant due to its ability to reduce friction for a longer period of time. Fifty-six (56) silicone personal and condom lubricants were analyzed to iii identify unique characteristics that can be used to determine individual sub-classes and test those sub-classes. Direct analysis in real time-time of flight mass spectrometry (DART-TOFMS) was utilized because minor and unique molecular ions that could be attributed to different sub-groups can easily be distinguished from the major sample peaks. This is primarily based on the direct mass spectrometry design of the instrumentation that can differentiate minor components from major components that might not be observed using traditional chromatographic separation. The DART source creates molecular ions for individual components in mixed samples under atmospheric conditions in either positive or negative mode. The TOF-MS, which is capable of high resolution and accurate mass analysis, allows more accurate and precise detection of molecular component ions. Additionally, no sample preparation is required to analyze neat samples, which minimizes potential contamination issues. Attenuated total reflectance-FTIR (ATR-FIR) was used to analyze the training set personal lubricants to compare previous methods of analysis to the newly developed DART-TOFMS method of analysis. Principle component analysis (PCA) and cluster analysis were used to identify potential sub-groups and subsequently a classification scheme. Linear discriminant analysis was utilized to conduct leave one out cross validation and to categorize test samples. Eight sub-groups were developed based on the presence and/or absence of PDMS and minor component peaks observed. A classification scheme was developed using the eight sub-groups identified through PCA and cluster analysis. This classification scheme was tested using LDA to classify blind samples. One group includes a scented personal lubricant. Another group includes flavored condom lubricants. The other groups were developed based on the relative intensity of PDMS peaks and minor component peaks. Variation of the intensity of PDMS peaks between and iv within samples of different lot numbers causes some misclassification of samples. This classification scheme also doesn’t take into account real-world factors such as dilution and biodegradation. Although further research is required to create a more stable classification scheme, the identified sub-groups are a good foundation for the creation of a lubricant database and finalized classification scheme. v ACKNOWLEDGMENTS First, I would like to thank my mentor and advisor, Dr. Candice Bridge. Your advice, support, and patience were invaluable throughout this journey. I couldn’t have asked for a better advisor. I would also like to thank Dr. Michael Sigman, Dr. Andres Campiglia, and Dr.Cherie Yestrebsky for serving on my thesis committee. To Dr. Mark Maric, I thank you for your continual assistance in my research whenever I hit a wall. To my remaining colleagues at NCFS, thank you for making the office a wonderful place to work and socialize. Professor Mattheu Miller, Dr. Matthieu Baudelet, and Dr. Tamra Legron-Rodriguez, thank you for providing employment as a GTA and listening whenever I needed to vent about the students. Judith Stout, thank you for always being there when I need a candy pick-me-up. Last but certainly not least, I would like to thank my friends and family. I would especially like to thank my parents, who have endlessly given me love, support, and a friendly ear whenever it all seems overwhelming. vi TABLE OF CONTENTS LIST OF FIGURES ........................................................................................................................ x LIST OF TABLES ....................................................................................................................... xiv CHAPTER ONE: INTRODUCTION ............................................................................................. 1 CHAPTER TWO: LITERATURE REVIEW ................................................................................ 3 2.1 Lubricants Background ................................................................................................. 3 2.2 Attenuated Total Reflectance-FTIR Background ......................................................... 8 2.3 Direct Analysis in Real Time-MS Background ............................................................ 9 2.4 Statistical Techniques ................................................................................................. 13 2.4.1 Principal Component Analysis ............................................................................ 13 2.4.2 Cluster Analysis .................................................................................................. 15 2.4.3 Analysis of Variance Test ................................................................................... 16 2.4.4 Linear Discriminant Analysis .............................................................................. 17 CHAPTER THREE: MATERIALS AND METHODS ............................................................... 19 3.1 Materials ..................................................................................................................... 19 3.2 Methods....................................................................................................................... 22 3.2.1 Sample Acquisition Parameters for ATR-FTIR .................................................. 22 3.2.2 Sample Acquisition Parameters for DART-TOFMS .......................................... 22 3.2.3 DART-TOFMS Mass Spectral Data Processing ................................................. 24 3.2.4 Chemometric Analysis ........................................................................................ 25 vii CHAPTER FOUR: ATR-FTIR RESULTS .................................................................................. 28 4.1 Instrumental Data ........................................................................................................ 28 4.2 Chemometric Analysis ................................................................................................ 29 4.2.1 Cluster Analysis .................................................................................................. 30 4.2.2 PCA Analysis ...................................................................................................... 31 4.3 Conclusion .................................................................................................................
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