MASS SPECTROMETRY: INVESTIGATION of SAMPLING DEVICES for ILLICIT DRUG DETECTION and QUANTIFICATION by Chau Bao Nguyen
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PAPER SPRAY - MASS SPECTROMETRY: INVESTIGATION OF SAMPLING DEVICES FOR ILLICIT DRUG DETECTION AND QUANTIFICATION by Chau Bao Nguyen A Thesis Submitted to the Faculty of Purdue University In Partial Fulfillment of the Requirements for the degree of Master of Science Department of Forensic and Investigative Sciences at IUPUI Indianapolis, Indiana July 2021 THE PURDUE UNIVERSITY GRADUATE SCHOOL STATEMENT OF COMMITTEE APPROVAL Dr. Nicholas E. Manicke, Chair Department of Chemistry and Chemical Biology Dr. John V. Goodpaster Department of Chemistry and Chemical Biology Dr. Frédérique T. Deiss Department of Chemistry and Chemical Biology Approved by: Dr. John V. Goodpaster 2 This thesis is dedicated to my beloved parents and my sister, who continually provide their moral, emotional, and financial support, and to my partner, who is always there for me. 3 ACKNOWLEDEGMENTS First of all, I would like to thank my supervisor, Dr. Nicholas Manicke for giving me the opportunity to carry out my graduate work in his lab. His supervisory style is a perfect balance between guidance and independence, which gives me room to learn and grow in the right direction. His knowledge, enthusiasm, and patience helped a lot in my personal and career growth. I would also like to thank my committee members, Dr. Goodpaster and Dr. Deiss for their insightful comments, helpful ideas, and informative discussion throughout my time in my master’s program. Many thanks to my lab colleagues in the Manicke group, especially Greta Ren, Christine Skaggs, Sarah Dowling, Magnus Rydberg, and Hannah Zimmerman for putting up with me and providing me with endless words of encouragement as well as countless technical and practical support when I first started. A thank you to Kitty O’Doherty and Beverly Hewitt for all their help with administrative paperwork and forms. I would also like to thank Nam Lai from BaySpec for all his technical support. Without him, a part of my project would not have been possible. I especially want to show my gratitude to the U.S. Army DEVCOM Chemical Biological Center for their work and their help during my project. I consider myself extraordinarily lucky to be a part of Nick’s group and to work with so many great colleagues and collaborators during my time here at IUPUI. Funding for this study was provided by the U.S. Army Combat Capabilities Development Command Chemical Biological Center (DEVCOM CBC) Explosives Forensics Program. 4 TABLE OF CONTENTS LIST OF TABLES .......................................................................................................................... 8 LIST OF FIGURES ........................................................................................................................ 9 LIST OF ABBREVIATIONS ....................................................................................................... 11 ABSTRACT .................................................................................................................................. 13 INTRODUCTION .............................................................................................. 14 Mass Spectrometry ......................................................................................................... 14 Ambient Ionization ......................................................................................................... 15 Paper Spray – Mass Spectrometry .................................................................................. 17 Paper Spray – Mass Spectrometry in Drug Screening ................................................... 20 References ...................................................................................................................... 23 PRESSURE-SENSITIVE ADHESIVE PAPER FOR LOW-COST COLLECTION AND ANALYSIS OF DRUG RESIDUES ON SURFACES ............................ 28 Abstract ........................................................................................................................... 28 Introduction .................................................................................................................... 29 Method ............................................................................................................................ 31 2.3.1 Materials .................................................................................................................. 31 2.3.2 Preparation of Working Solutions ........................................................................... 31 2.3.3 PSA Paper Spray Tip Preparation ........................................................................... 32 2.3.4 Drugs Deposit and Samples Collection ................................................................... 32 2.3.5 Paper Spray – Mass Spectrometry and Data Analysis ............................................ 33 Results and Discussion ................................................................................................... 36 2.4.1 Method Development .............................................................................................. 36 2.4.2 Adhesive Versus Non-Adhesive Paper ................................................................... 38 2.4.3 Dabbing Sequences Comparison ............................................................................. 41 2.4.4 Detection Limits Determination .............................................................................. 44 Conclusions .................................................................................................................... 49 References ...................................................................................................................... 50 PRESSURE-SENSITIVE ADHESIVE COMBINED WITH PORTABLE MASS SPECTROMETER FOR DRUG SCREENING ON SURFACES ............................................... 53 Abstract ........................................................................................................................... 53 5 Introduction .................................................................................................................... 54 Method ............................................................................................................................ 56 3.3.1 Materials .................................................................................................................. 56 3.3.2 Preparation of Working Solutions and Calibration Solutions ................................. 56 3.3.3 Preparation of PSA Paper Tickets ........................................................................... 57 3.3.4 Calibrants Preparation and Drug Deposition for “Realistic” Scenarios .................. 57 3.3.5 Portable Mass Spectrometer Calibration, PS-MS analysis, and Data Processing ... 58 Results and Discussions ................................................................................................. 62 3.4.1 Optimization of Instrument Settings ....................................................................... 62 3.4.2 Calibration Curves and Detection Limits ................................................................ 63 3.4.3 “Realistic Scenarios” on Surfaces ........................................................................... 67 Conclusions .................................................................................................................... 69 References ...................................................................................................................... 70 DEVELOPING SNAP-IN SOLID-PHASE-EXTRACTION CARTRIDGE FOR AUTOMATED SYSTEM ............................................................................................................ 74 Abstract ........................................................................................................................... 74 Introduction .................................................................................................................... 75 Methods .......................................................................................................................... 77 4.3.1 Materials .................................................................................................................. 77 4.3.2 Making Sampling Devices and Snap-In SPE Columns .......................................... 77 4.3.3 Preparation of Working Solutions and Calibrators ................................................. 78 4.3.4 Paper Spray Analysis and Data Processing ............................................................. 78 Results and Discussion ................................................................................................... 81 4.4.1 Limits of Detection Using Snap-In SPE Column .................................................... 81 4.4.2 Future Works ........................................................................................................... 85 Conclusions .................................................................................................................... 85 References ...................................................................................................................... 86 OVERALL CONCLUSIONS AND FUTURE DIRECTIONS .......................... 88 Overall Conclusions ....................................................................................................... 88 Future Directions ............................................................................................................ 89 5.2.1 PSA Sampling ........................................................................................................