The identification of illicit drugs presents many problems to the forensic laboratory because there is a broad range of possibilities which must be considered in order for a chemist to arrive at a definite identification. Obviously, this is a task that requires a constant search for new analytical techniques to meet such demands. Furthermore, these new techniques must not only facilitate the testing procedure but must provide the necessary confidence in their results as required by our court system.

The primary goal of the forensic drug examiner is the unequivocal identification of any controlled substance present in a drug exhibit. Most forensic laboratories routinely employ Gas Chromatography/ Mass Spectrometry (GC/MS) as the preferred method for this examination. The technique provides a rapid, semi-automated analysis of the sample and typically yields sufficient information to identify the compounds in question. However, the application of GC/MS for drug analysis does have its limitations. Certain drugs yield minimal mass spectral fragmentation patterns using electron impact MS, while other compounds, such as some diastereomers and positional isomers, are not readily differentiated technique to mass spectroscopy. Infrared spectroscopy (IR, meaning FTIR) provides an alternate technique to mass spectroscopy for the identification of organic compounds. Recent improvements in the hyphenated technique, Gas Chromatography/Infrared Spectroscopy (GC/IR) may provide a simple alternative or supplemental approach to GC/MS for identification of certain compounds. A newly introduced instrument collects GC effluent on a liquid nitrogen cooled, IR transparent window that allows the direct analysis of the deposited solid material. This technique is superior to the IR light pipe in sensitivity, IR spectral quality, and allows direct comparison of the collected spectra to existing IR databases. Our research developed procedures and protocols for the analysis of drugs and determined the benefits and limitations of this technology. The research focused on the routine identification of commonly encountered drugs, designer drugs, closely related drug isomers, as well as the fundamentals of the gas chromatography and infrared systems. Statement of purpose: The research was undertaken to develop this technology into a viable technique for the forensic community. The instrument was studied for repeatability, sensitivity, and selectivity while optimizing for analysis of a wide range of drug samples. Based upon this work the instrument proved to be a powerful forensic tool providing complimentary data to GC/MS. Acceptable levels of sensitivity, linearity, and reproducibility were achieved using the GC split-less injection mode. Concern about cross contamination of samples on the collection disk were dispelled as the deposited GC vapor produced solid "tracks" that were unique to each sample and appropriately documented by the instrument. Analytical methods were developed for the routine analyses of drugs and synthetic cannabinoids. Through these studies the instrument was verified for casework analysis and is presently in operational use in our laboratory. Software limitations hindered research progress, although software and hardware upgrades were made by the vendor (Spectra Analysis) some of which were driven by feedback provided by staff at the Vermont Forensic Laboratory (VFL).

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.

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

There is a dramatic rise of novel drug use due to the increased popularity of so-called designer drugs. These synthetic drugs can be illegal in some countries, but legal in others and novel compounds unknown to drug chemistry emerge monthly. This thoughtfully constructed edited reference presents the main chromatographic methodologies and strategies used to discover and analyze novel designer drugs contained in diverse biological materials. The methods are based on molecular characteristics of the drugs belonging to each individual class of compounds, so it will be clear how the current methods are adaptable to future new drugs that appear in the market.

When a dose of drug is administered, three main phases of drug action may be distingushed. In the "pharmaceutical" phase the dosage form disintegrates, the active substance dissolves and becomes available for absorption. The second phase ("pharmaco kinetic" phase) includes absorption, distribution, metabolism, and excretion. That fraction of the dose which finally reaches the circulation after absorption will be available for biological action in the third, or "pharmacodynamic" phase when the drug reaches the target tissues and a drug-receptor interaction takes place. The objectives in studies of drug metabolism are: (a) to identify the pathways by which drugs are transformed in the body; (b) to ascertain quantitatively the importance of each pathway and intermediate; (c) to identify and quantify endogenous constituents influenced by the drug or its metabolites which may interfere with common metabolic processes. Since metabolites usually differ from their precursors by only a single chemical group, the resulting metabolic pathways generally consist of a series of closely related compounds. Mass spectrometry is uniquely suited for the analysis of drugs and metabolites for several reasons: only a minimal amount of sample preparation is needed, closely related compounds can be analyzed in a single step, structures can often be deduced directly from the mass spectra without the need for pure reference spectra, and constituents can be quantified with relative ease even when present in fractional nanogram quantity.

Mass spectrometry is an important tool used in many different disciplines and settings that include forensics, drug discovery, environmental analysis, and proteomics. Gas chromatography - mass spectrometry (GC-MS) and matrix assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI - TOF MS) are two of the most important instruments used for analysis of compounds. Chapters 1 and 2 of this discussion use GC-MS for the investigation of synthetic cannabinoids in ̀K2' incense products and the detection of metabolites in urine samples from individuals suspected of consuming these mixtures. Analytical standards were synthesized and used for identification and confirmation of structures. Detection of these compounds and their metabolites is important since ̀K2' products are banned nationwide as a Schedule 1 substance. Chapter 3 uses LDI-TOF MS for the analysis of triacylglycerol (TAG) degradation products in fingermark samples exposed to light/dark conditions on four different surfaces: stainless steel, glass, plastic, and iron. A standard of triolein was used for identification of products with the detection of C7:0 and C8:0 aldehyde and carboxylic acids through tandem mass spectrometry analysis. The age of a fingermark was estimated through comparison of unsaturated and saturated TAGs. Analysis of TAGs in fingermarks is important as a possible dating technique which could provide investigative leads or a timeline of events in a criminal investigation. Chapter 4 uses MALDI-TOF MS for the development of a rapid separation technique to overcome suppression effects of TAGs by phosphatidylcholine (PC). A solid phase extraction (SPE) technique was developed to separate these classes of compounds using reference lipids and real samples (beef, egg yolk) as models. Because lipids play important roles in biological systems, a method to clearly detect and overcome suppression effects is important. Chapter 5 uses GC-MS for the analysis of fatty and resin acids in biomass fermentation process waters. An extraction procedure was developed for detection and quantification of these compounds. Monitoring these acids in water samples is important because they can negatively impact environmental and industrial pathways.

Clear, comprehensive, and state of the art, the groundbreaking book on the emerging technology of direct analysis in real time mass spectrometry Written by a noted expert in the field, Direct Analysis in Real Time Mass Spectrometry offers a review of the background and the most recent developments in DART-MS. Invented in 2005, DART-MS offers a wide range of applications for solving numerous analytical problems in various environments, including food science, forensics, and clinical analysis. The text presents an introduction to the history of the technology and includes information on the theoretical background, for exampleon the ionization mechanism. Chapters on sampling and coupling to different types of mass spectrometers are followed by a comprehensive discussion of a broad range of applications. Unlike most other ionization methods, DART does not require laborious sample preparation, as ionization takes place directly on the sample surface. This makes the technique especially attractive for applications in forensics and food science. Comprehensive in scope, this vital text: -Sets the standard on an important and emerging ionization technique -Thoroughly discusses all the relevant aspects from instrumentation to applications -Helps in solving numerous analytical problems in various applications, for example food science, forensics, environmental and clinical analysis -Covers mechanisms, coupling to mass spectrometers, and includes information on challenges and disadvantages of the technique Academics, analytical chemists, pharmaceutical chemists, clinical chemists, forensic scientists, and others will find this illuminating text a must-have resource for understanding the most recent developments in the field.