False positive results from on-scene illicit drug analysis using presumptive color tests have caused numerous wrongful arrests (Lieblein 2018). In many states, forensic laboratories do not ever receive the sample for confirmative identification unless the defendant goes to trial, which makes it impossible to know the severity of this problem. Additionally, some defendants take a plea deal, which can result in these defendants spending months or years in prison for a crime they did not commit. Improving the reliability of on-scene illicit drug testing by incorporating confirmatory methods capable of achieving very low limits of detection such as gas chromatography-mass spectrometry (GC-MS) into the field could help reduce these wrongful arrests. The purpose of this research was to build a spectral library of illicit drugs and additive spectra for a commercially available portable ion-trap GC-MS, the Torion T-9 from Perkin-Elmer. Due to the potential for space charge and ion-ion interactions in ion trap mass spectrometers, the resulting MS spectra produced can be different than standard quadrupole MS. Thus, a customized library for this type of field application is critical. Over fifty (50) illicit drugs and fifteen (15) additives were used to create a GC-MS library after repeated testing. This customized GC-MS library was then used to test the ability to detect and identify illicit substances and their additives in seized drug samples, provided by the Connecticut State Police K9 Unit, which had not undergone laboratory testing. In addition, results were compared with data generated from the same samples using a field-portable quadrupole GC-MS. Of the twelve (12) samples tested, a positive identification for a controlled substance was made for ten (10) of them, using spectral data in the customized GC-MS library. The other two (2) contained unknown peaks that were not identified by any available GC-MS or MS library. Future studies should work on refining the retention time for each drug, performing tests with different versions of the Torion T-9 to ensure robustness of the GC-MS library, and continuous addition of illicit drug and additive standards to further expand the GC-MS library.

Monitoring current illicit drug trends and consumption rates of pharmaceuticals using a non-invasive collection technique is needed to address the present drug use and the growing drug epidemic. Reliance on self-reporting drug use surveys is not always a practical measure of illicit drug use. Wastewater analysis has been used globally as a targeted method for monitoring the consumption of specific illicit drugs. Current existing analytical techniques for wastewater analysis focus on the use of targeted liquid chromatography-mass spectrometry (LC-M.S.) based techniques. Few gas chromatography (GC) procedures exist for wastewater analysis, and those that do concentrate their methods on a single class of drugs operating their mass spectrometer (MS) in selective ion monitoring (SIM) mode. This study aims to develop an untargeted, underivatized, full scan gas chromatography-mass spectrometry (GC/MS) method for the analysis of wastewater. Solid phase extraction (SPE) was performed with UCT mixed mode, 15 mL Clean Screen DAU columns with 500 mg sorbent to extract a 500 mL wastewater sample. Sample extracts were reconstituted in ethyl acetate and analyzed on a Shimadzu GCMS-QP2020 gas chromatograph-mass spectrometer (GC/MS) installed with an Agilent J & W HP-5MS (30 m × 0.25mm, 0.25 æm) column. Injection volume, flow rate, oven temperature, and ion source scan rate were optimized to develop an untargeted full scan method for the detection of pharmaceuticals. Calibration curves were developed for 42 targeted drugs. A 1 æL sample volume is run with a splitless injection utilizing helium as the carrier gas and the instrument operated in constant flow mode at a rate of 1.0 mL/min. The GC oven program is held at the initial temperature of 70°C for 2 min then ramped at 15°C/min to 300°C and held for 10 min for a total run time of 27.33 min. The injection port, transfer line, and source were set at 250°C, 280°C, and 200°C respectively. The MS operated in full scan mode, scanning ions from 35-550 m/z at an event time of 0.20 seconds from 3.50-27.33 minutes. Out of a 42 drug panel, over 75% of the generated calibration curves were suitable for quantitation with coefficients of determination greater than 0.9875. Limits of detection for most drugs ranged from 0.10-1.0 ng/mL, on par with many targeted liquid chromatography methods. The optimized untargeted method is able to detect a wide range of compounds in addition to those in the drug panel. The untargeted full scan MS method supports monitoring a wider range of pharmaceuticals overlooked in traditional targeted waste water methods such as changing trends in novel psychoactive substances.

Illicit drugs are an emerging class of environmental contaminants and mass spectrometry is the technique of choice for their analysis. This landmark reference discusses the analytical techniques used to detect illicit drugs in wastewater and surface water, details how to estimate the levels of contaminants in the environment, and explores the behavior, fate, and toxic effects of this new class of contaminants, now a ubiquitous presence in wastewater and surface water. The book details how an estimate of illicit drug consumption in a given population can be developed from an analysis of the residues of illicit drugs in wastewater. An important resource for analytical chemists, environmental researchers, forensic scientists, biologists, and toxicologists.

Mass spectrometry is one of the most versatile analytical techniques due to the vast range of analytes that it can detect and quantify and, as such, for its contribution to a significant number of life science fields. The legal and forensics community has certainly benefited from this technique, which has been able to provide reliable evidence in court cases. Liquid Chromatography/Gas Chromatography–Mass Spectrometry (LC/GC–MS) still have a dominant role in the provision of forensic intelligence. However, in the past decade new and exciting MS-based techniques have emerged and are or have evolved to be at an operational deployment maturity, enabling either fast, ambient, non-destructive, or portable screening (or encompass all of these features). In this book, developments of LC–MS and GC–MS based techniques are covered with respect to operational practice and new applications, accompanied by other MS-based techniques that are increasing forensic opportunities and that operate on a variety of evidence types. Whilst the underpinning working principles of each relevant mass spectrometry technique are summarised, each chapter primarily focuses on its implementation in criminal investigation and court cases. In the last chapters, this book additionally covers emerging MS technologies that are at the beginning of their operational implementation journey as well as niche applications outside the fields of traditional forensic science but with a clear potential to impact future investigations (forensics beyond the courtroom). This book provides an up-to-date reference for the mass spectrometry-based tools that are currently available both as established and as emerging methods within forensic practice. It will help casework commissioning managers and forensic providers worldwide to make more informed decisions as to the forensic strategy and workflow when examining exhibits. It is also recommended to postgraduates and early career investigators with reference to the contribution that these techniques and methods could make if applied to classic forensic science practice.

Gas chromatography mass spectrometry (GC-MS) has been the technique of choice of analytical scientists for many years. The latest developments in instrumentation, including tandem mass spectrometry (MS-MS) and time-of-flight (TOF) detectors, have opened up and broadened the scope of environmental analytical chemistry. This book summarizes the major advances and relevant applications of GC-MS techniques over the last 10 years, with chapters by leading authors in the field of environmental chemistry. The authors are drawn from academia, industry and government. The book is organized in three main parts. Part I covers applications of basic GC-MS to solve environmental-related problems. Part II focuses on GC-MS-MS instrumentation for the analyses of a broad range of analysis in environmental samples (pesticides, persistent organic pollutants, endocrine disruptors, etc.). Part III covers the use of more advanced GC-MS techniques using low- and high-resolution mass spectrometry for many applications related to the environment, food and industry. - Summarizes the major advances of GC-MS techniques in the last decade - Presents relevant applications of GC-MS techniques - Covers academic, industrial and governmental sectors

The second edition of Gas Chromatography and Mass Spectrometry: A Practical Guide follows the highly successful first edition by F.G. Kitson, B.S. Larsen, and C.N. McEwen (1996), which was designed as an indispensible resource for GC/MS practitioners regardless of whether they are a novice or well experienced. The Fundamentals section has been extensively reworked from the original edition to give more depth of an understanding of the techniques and science involved with GC/MS. Even with this expansion, the original brevity and simple didactic style has been retained. Information on chromatographic peak deconvolution has been added along with a more in-depth understanding of the use of mass spectral databases in the identification of unknowns. Since the last edition, a number of advances in GC inlet systems and sample introduction techniques have occurred, and they are included in the new edition. Other updates include a discussion on fast GC and options for combining GC detectors with mass spectrometry. The section regarding GC Conditions, Derivatization, and Mass Spectral Interpretation of Specific Compound Types has the same number of compound types as the original edition, but the information in each section has been expanded to not only explain some of the spectra but to also explain why certain fragmentations take place. The number of Appendices has been increased from 12 to 17. The Appendix on Atomic Masses and Isotope Abundances has been expanded to provide tools to aid in determination of elemental composition from isotope peak intensity ratios. An appendix with examples on "Steps to follow in the determination of elemental compositions based on isotope peak intensities" has been added. Appendices on whether to use GC/MS or LC/MS, third-party software for use in data analysis, list of information required in reporting GC/MS data, X+1 and X+2 peak relative intensities based on the number of atoms of carbon in an ion, and list of available EI mass spectral databases have been added. Others such as the ones on derivatization, isotope peak patterns for ions with Cl and/or Br, terms used in GC and in mass spectrometry, and tips on setting up, maintaining and troubleshooting a GC/MS system have all been expanded and updated. - Covers the practical instruction necessary for successful operation of GC/MS equipment - Reviews the latest advances in instrumentation, ionization methods, and quantitation - Includes troubleshooting techniques and a variety of additional information useful for the GC/MS practitioner - A true benchtop reference - A guide to a basic understanding of the components of a Gas Chromatograph-Mass Spectrometer (GC-MS) - Quick References to data interpretation - Ready source for information on new analyses