Development And Validation Of Two Innovative Liquid Chromatography Tandem Mass Spectrometry Methods For Forensic Toxicology Laboratories

Chromatography has many roles in forensic science, ranging from toxicology to environmental analysis. In particular, high-performance liquid chromatography (HPLC) is a primary method of analysis in many types of laboratories. Maintaining a balance between practical solutions and the theoretical considerations involved in HPLC analysis, Forensic App

Co-published with the American Academy of Forensic Sciences, Forensic Science presents comprehensive international discussion of key issues and future directions within the forensic sciences. Written by accomplished and respected specialists in approximately eleven distinct areas of the forensic sciences, the volume will examine central issues within each discipline, provide perspective on current debate and explore current and proposed research initiatives. It will also provide the forensically involved international community with current in-depth perspective on the key issues in the contemporary practice of the forensic sciences.

The 2021 National Institute of Justice (NIJ) Forensic Science Research and Development (R&D) Symposium is intended to promote collaboration and enhance knowledge transfer of NIJ-funded research. The NIJ Forensic Science R&D Program funds both basic or applied R&D projects that will (1) increase the body of knowledge to guide and inform forensic science policy and practice or (2) result in the production of useful materials, devices, systems, or methods that have the potential for forensic application. The intent of this program is to direct the findings of basic scientific research; research and development in broader scientific fields applicable to forensic science; and ongoing forensic science research toward the development of highly discriminating, accurate, reliable, cost-effective, and rapid methods for the identification, analysis, and interpretation of physical evidence for criminal justice purposes.

The 2019 National Institute of Justice (NIJ) Forensic Science Research and Development (R&D) Symposium is intended to promote collaboration and enhance knowledge transfer of NIJ-funded research. The NIJ Forensic Science R&D Program funds both basic or applied R&D projects that will (1) increase the body of knowledge to guide and inform forensic science policy and practice or (2) result in the production of useful materials, devices, systems, or methods that have the potential for forensic application. The intent of this program is to direct the findings of basic scientific research; research and development in broader scientific fields applicable to forensic science; and ongoing forensic science research toward the development of highly discriminating, accurate, reliable, cost-effective, and rapid methods for the identification, analysis, and interpretation of physical evidence for criminal justice purposes.

Practitioners of forensic toxicology are expected to detect, confirm, and quantify a chemically diverse range of drugs and poisons covering a number of orders of magnitude in concentration in challenging biological matrices. Developments in LC–MS have enabled a wider range of compounds to be analyzed using fewer extraction processes, practically eliminating the requirement for derivatization steps and with fewer instrumental analysis stages. This chapter provides the reader with a broad overview of the current capabilities offered by LC in this branch of analytical chemistry—as well as its limitations.

Microextraction Techniques in Analytical Toxicology provides the information readers need to include about cutting-edge sample preparation techniques into their everyday analytical practice, including comprehensive information about principles and state-of-the-art microextraction sample preparation techniques for the analysis of drugs and poisons in biological specimens, especially in forensic and clinical settings. This book also focuses on theoretical discussions of solid-based and liquid-based microextraction techniques, their method development, validation, and applications. A detailed compilation of analytical protocols based on published microextraction procedures to aid in method development, synthesis, and the application of green solvents (ionic liquids and deep eutectic solvents) and new sorbents, such as molecularly imprinted polymers, and their application in microextraction techniques are also covered. Features: Provides a systematic review of microextraction techniques applied in analytical toxicology A comprehensive guide for the practical implementation of microextraction techniques in forensic, clinical, and analytical laboratories Contains figures and tables for easy understanding and quick adaptation of the parameters of microextraction techniques Fundamentals, development, and applications of microextraction techniques as a sample preparation procedure are discussed in detail Extremely useful for the researchers and academicians engaged in analytical method development using microextraction techniques This book appeals to a wide readership of forensic, clinical, and analytical toxicologists, as well as academicians and researchers. Written by eminent scientists and leading experts on sample preparation techniques, this book serves as a desk reference for routine laboratory analysis and as an indispensable teaching tool in the classroom for graduate and Ph.D. students.

Kratom is a tree originating in Southeast Asia, and has a history of usage among farmers. The leaves of the tree were chewed and used by farmers as a stimulant in order to work long days. Over the years, the popularity of the drug spread worldwide and has risen in recent years. In 2016, kratom was put on a Drugs of Concern list by the United States Drug Enforcement Administration (DEA). A lack of research including studies for mitragynine and 7-hydroxymitragynine has been observed, and there are even fewer postmortem case studies in the literature. The rise in kratom usage was noticed in the casework of the Office of the Chief Medical Examiner (OCME) Toxicology Laboratory in Oklahoma. The number of cases involving mitragynine, an alkaloid in kratom, has risen over recent years, but the OCME did not have a validated method for quantitation. The importance of this thesis project was to validate a method for the quantitation of mitragynine and qualitative identification of 7-hydroxymitragynine, assess the stability of the two alkaloids in three different storage conditions (ambient, refrigerated, and frozen), and examine real world cases coming through the OCME. The extraction utilized in this method was a phosphate buffer followed by filtering the samples using 3 mL columns containing diatomaceous earth. Extracts were then concentrated by drying them down, reconstituted, and washed with hexanes. The samples were then analyzed using liquid chromatography paired with tandem mass spectrometry (LC/MS-MS). The method for quantitation of mitragynine was validated with the criteria of interferences, bias, precision, ion suppression/enhancement, limit of detection, carryover, calibration model, and stability taken into consideration. The validation criteria for 7-hydroxymitragynine were interferences, ion suppression/enhancement, limit of detection, carryover, and stability. All criteria were met and deemed acceptable by the OCME lab’s Quality Assurance Program. The stability study demonstrated that mitragynine is more stable in refrigerator conditions as opposed to freezer, and that 7-hydroxymitragynine went through an approximate 20% decrease over 65 days in the refrigerator in blood. The case studies had ranges of 130-1,400 ng/mL for heart blood, 130-1,300 ng/mL for femoral blood, and 220-7,000 ng/mL for liver. Central/Peripheral (C/P) and Liver/Peripheral (L/P) ratios were calculated to identify the potential for mitragynine to undergo postmortem redistribution (PMR). The C/P and L/P ratios were an average of 1.0 and 2.7 respectively, suggesting that mitragynine does not experience significant PMR. This thesis project will be adding to the body of knowledge concerning mitragynine and 7-hydroxymitragynine which will help researchers and postmortem labs assess the storage conditions of their specimen and help with interpretation of toxicology results in death investigations.

Several areas of forensic science use the technique of gas chromatography, ranging from fire analysis to the investigation of fraudulent food and perfumes. Covering the essentials of this powerful analytical technique, Forensic Applications of Gas Chromatography explains the theory and shows applications of this knowledge to various realms of forensic science. Topics include: A brief introduction to gas chromatography and its use in forensic science Various components that make up the gas chromatographic instrumentation The theory of the separation process, along with the chemistry underpinning the process Method development, with a specific example of a separation of eight different compounds using a gas chromatography-flame ionization detector Quality assurance and method validation—with information applicable to many types of analytical testing laboratories Troubleshooting in gas chromatography systems New developments in gas chromatography and advances in columns and detectors Real examples supplement the text, along with questions in each chapter. The book includes examples of applications of gas chromatography in drugs, toxicology, fire, paint, food, and fragrance. Each application is presented as an individual case study with specific focus on a particular sample preparation technique. This allows each technique to be discussed with respect to its theory, instrumentation, solvent selection, and function, as appropriate. Each case study provides readers with suitable practical information to allow them to perform experiments in their own laboratory either as part of a practical laboratory class or in a research context. The final chapter provides answers to the questions and encourages further study and discussion.