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Why LC/MS/MS? • Why Liquid Chromatography? – Analysis of Labile Analytes – Analysis of More Polar Compounds Without Derivatization

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Why LC/MS/MS? • Why Liquid Chromatography? – Analysis of Labile Analytes – Analysis of More Polar Compounds Without Derivatization The author(s) shown below used Federal funds provided by the U.S. Department of Justice and prepared the following final report: Document Title: Enhanced Studies of LC/MS/MS Capabilities to Analyze Toxicology Postmortem Samples Author: George Herrin, Jr., Ph.D., Lisa Holt, M.S., A. Michael Morrison, M.S., Lori Nix, B.A., Joseph Austin, Ph.D., Troy Dettmering, B.S., Jon Stephenson, B.S., Jessica Mehan, M.S., Jacquelyn Orlandino, M.S., Ken Smith, Ph.D., Cynthia Lewallen, M.S., Donald Dicks, B.S., Mary Jo Brasher, B.S., Teresa Bull, B.S., Katherine Dietzel, M.S., S. Zyed Ali, Ph.D., Daphne Ristau, B.S., David Golz, B.S. Document No.: 230032 Date Received: March 2010 Award Number: 2006-DN-BX-K015 This report has not been published by the U.S. Department of Justice. To provide better customer service, NCJRS has made this Federally- funded grant final report available electronically in addition to traditional paper copies. Opinions or points of view expressed are those of the author(s) and do not necessarily reflect the official position or policies of the U.S. Department of Justice. This document is a research report submitted to the U.S. Department of Justice. This report has not been published by the Department. Opinions or points of view expressed are those of the author(s) and do not necessarily reflect the official position or policies of the U.S. Department of Justice. Enhanced Studies of LC/MS/MS Capabilities to Analyze Toxicology Postmortem Samples National Institute of Justice Research and Development Award# 2006-DN-BX-K015 Final Technical Report Project Director: George Herrin, Jr., Ph.D. Forensic Toxicologists: Lisa Holt, M.S., A. Michael Morrison, M.S., Lori Nix, B.A., Joseph Austin, Ph.D., Troy Dettmering, B.S., Jon Stephenson, B.S., Jessica Mehan, M.S., Jacquelyn Orlandino, M.S., Ken Smith, Ph.D., Cynthia Lewallen, M.S., Donald Dicks, B.S., Mary Jo Brasher, B.S., Teresa Bull, B.S., Katherine Dietzel, M.S., S. Zyed Ali, Ph.D., Daphne Ristau, B.S., David Golz, B.S. February2010 Georgia Bureau of Investigation-Division of Forensic Sciences 3121 Panthersville Road; Decatur, GA 30034 This document is a research report submitted to the U.S. Department of Justice. This report has not been published by the Department. Opinions or points of view expressed are those of the author(s) and do not necessarily reflect the official position or policies of the U.S. Department of Justice. Table of Contents AbstractU U ............................................................................................................................................ i ExecutiveU SummaryU ........................................................................................................................ ii OverviewU U ..................................................................................................................................... ii MaterialsU and MethodsU ...............................................................................................................iii ProjectU StudiesU ...........................................................................................................................iii DiscussionU U ................................................................................................................................... v LiteratureU CitedU .......................................................................................................................... vi ChapterU 1: Background and WorkshopsU ........................................................................................ 1 BackgroundU U ................................................................................................................................. 1 TrainingU WorkshopsU.................................................................................................................... 2 TableU 1: Workshop AttendeesU ..................................................................................................... 3 LiteratureU CitedU ........................................................................................................................... 4 ChapterU 2. THC AnalysisU ............................................................................................................... 5 IntroductionU U ................................................................................................................................. 5 MaterialsU and MethodsU ................................................................................................................ 5 SampleU preparationU ................................................................................................................. 5 SampleU analysisU ....................................................................................................................... 5 ResultsU U ......................................................................................................................................... 6 SampleU Separation and AnalysisU ............................................................................................. 6 Linearity,U Limit of Detection, and Limit of QuantificationU .................................................... 6 ConcordanceU StudyU ................................................................................................................. 6 DiscussionU U ................................................................................................................................... 7 FigureU 1. Typical Enhanced Product Ion (EPI) scan of THC.U .................................................... 8 FigureU 2. Typical Enhanced Product Ion (EPI) scan of 11-OH-THC.U ........................................ 9 FigureU 3. Typical Enhanced Product Ion (EPI) scan of THCA.U ............................................... 10 FigureU 4. Typical Enhanced Product Ion (EPI) scan of internal standard THC-d3.U ................. 11 FigureU 5. Typical Enhanced Product Ion (EPI) scan of internal standard THCA-d9.U .............. 12 FigureU 6. Typical Calibration Curve for THC.U ......................................................................... 13 FigureU 7. Typical Calibration Curve for 11-OH-THC.U ............................................................. 14 FigureU 8. Typical Calibration Curve for THCA.U....................................................................... 15 2006-DN-BX-K015 Technical Report - 1 - This document is a research report submitted to the U.S. Department of Justice. This report has not been published by the Department. Opinions or points of view expressed are those of the author(s) and do not necessarily reflect the official position or policies of the U.S. Department of Justice. TableU 2. Mobile phase profiles for THC Analysis.U ................................................................... 16 TableU 3. Data for THC Limit of Quantitation studyU ................................................................. 17 TableU 4. Data for THC control studyU ........................................................................................ 18 TableU 5. THC concordance data.U............................................................................................... 19 LiteratureU CitedU ......................................................................................................................... 20 ChapterU 3. Opioid AnalysisU .......................................................................................................... 21 IntroductionU U ............................................................................................................................... 21 MaterialsU and MethodsU .............................................................................................................. 21 InstrumentationU U ..................................................................................................................... 21 ChromatographyU U ................................................................................................................... 21 BiologicalU SpecimensU............................................................................................................ 21 SampleU PreparationU ............................................................................................................... 21 InstrumentU ParametersU .......................................................................................................... 22 ResultsU U ....................................................................................................................................... 22 OptimizationU of InstrumentationU ........................................................................................... 22 ChromatographyU U ................................................................................................................... 22 RegionU of Ion SuppressionU .................................................................................................... 22 LimitsU of Identification (LOI)U ............................................................................................... 23 InterferenceU StudyU ................................................................................................................. 23 LimitsU of QuantiationU ............................................................................................................ 23 ReproducibilityU U ....................................................................................................................
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