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Jeffrey H. Comparin Laboratory Director Drug Enforcement Administration

DEA Special Testing and Research Laboratory Research Overview Forensic Science Research Federal Stakeholders Meeting February 2018. Jeffrey H. Comparin Laboratory Director Drug Enforcement Administration Special Testing and Research Laboratory. Mission. Lab System – STRL.

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Jeffrey H. Comparin Laboratory Director Drug Enforcement Administration

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  1. DEA Special Testing and Research LaboratoryResearch OverviewForensic Science Research Federal Stakeholders Meeting February 2018 Jeffrey H. Comparin Laboratory Director Drug Enforcement Administration Special Testing and Research Laboratory

  2. Mission Lab System – STRL The mission of the Drug Enforcement Administration’s Office of Forensic Sciences is to deliver quality forensic information and services to counter the global drug threat Vision Global Leader in Forensic Science

  3. Special Testing and Research Laboratory Dedicated Research Group • Group Supervisor and Seven GS-14 Senior Research Chemists • Three support existing Special Programs and conduct novel research • Two are technology specific • NMR • IRMS • One is an organic synthetic chemist • One specializes in clandestine laboratories • Academic Backgrounds Vary • ~20 Current Projects • Program support, standalone projects, answer urgent agency questions • Research Activities Funded by Operational and Outside Funding • In 2017, for the first time, a separate budget line item for research • Outcomes • Strategic and tactical results for DEA, policymakers and the counterdrug IC • Scientific manuscripts

  4. Special Testing and Research Laboratory Research Budget • Relevant, pre-competitive fundamental research to drive innovation • Funding is leveraged to provide maximum value to industry, academia, and government

  5. Fentanyl Signature Profiling Program • Mission • Gather Strategic and Tactical Intelligence • Link Seizures • Determine Synthetic Route • Determine Trafficking Routes • Develop “Consolidated Priority Organization Targets” (CPOT) • Research Projects • Organic Synthesis • Characterization of Unknown Compounds

  6. Quantitative Determination via NMR Counterfeit oxycodone tablets A=Acetaminophen = 26.1% C=Caffeine = 3.2% D=Dipyrone = 17.4% F=Fentanyl = 1.3% L=Lactose = 15.6% Solvent=D2O Maleic acid=ISTD

  7. GC-MS Impurity Profiles Fentanyl Relatively clean profiles = 87% of samples High purity fentanyl + Adulterants = 12% of samples Fentanyl-related impurities enriched <1% of samples

  8. Static Headspace-GC-MS ISTD CH2Cl2 (0.073%) ISTD Acetone (0.301%) trace CH2Cl2 (0.002%) MeOAc (0.006%) MeOH (0.195%) EtOAc (0.001%) EtOH (0.009%)

  9. Fentanyl Moiety Isotopes Fentanyl 4-ANPP C3H5O δ15Nδ13Cδ15Nδ13Cδ13C Low -5.6 -31.5 -5.6 -31.6 -32.0 High 6.2 -26.4 6.2 -26.3 -18.7 Avg 2.1 -28.5 2.0 -28.0 -24.6 STDEV 2.4 1.0 2.4 1.2 2.5 Range 11.8 5.1 11.8 5.3 13.3

  10. 2 Separate Seizures (Linked) Dipyrone artifacts Fentanyl 6.0% Fentanyl 44.8% Dipyrone 20.1% Mannitol 24.0% Lactose 08-22-16 IN 2 kg δ15N=1.8 δ13C=-28.5 4-ANPP 322-1 Fentanyl 6.0% Fentanyl 45.4% Dipyrone 25.5% Mannitol 22.8% Lactose 08-14-16 CA 24 kg δ15N=1.8 δ13C=-28.5 Identical solvent profiles: Acetone CH2Cl2 Toluene Mesityl oxide N-phenylpropanamide

  11. 2 Separate Counterfeit Tablet Seizures (Linked) 05-05-16 AZ 5 kg 1.2% Fentanyl 17.4% Dipyrone 26.1% Acetaminophen 3.2% Caffeine 15.6% Lactose* Fentanyl δ13C=-29.8 Caffeine δ13C=-32.2 Caffeine 4-ANPP C-24 ISTD Dipyrone Artifact Acetylfentanyl 06-23-16 CA 4.6 kg 1.2% Fentanyl 18.7% Dipyrone 25.5% Acetaminophen 3.2% Caffeine 12.5% Mannitol* Fentanyl δ13C=-29.8 Caffeine δ13C=-32.2 Benzylfentanyl (J) Acetaminophen

  12. Samples Examined and Linkages Over 1,100 illicit fentanyl samples examined 41 Sets of seizure linkages made to date that include: • 73 different cases/seizures • 169 different exhibits • Over 300 kg fentanyl originating from Chinaand Mexico

  13. Cocaine Signature Program Mission Origin Determination by Chemical Analyses • Research Projects • CSP • Operation Breakthrough • Cocaine IRMS • Differentiation of Growing Regions

  14. Cocaine Signature Program History More than 30 years of research producing over 100 scientific publications in peer-reviewed journals

  15. 19 Growing Regions Putumayo San Lucas Santander Valle de Cauca Vaupés Vichada Amazonas Antioquia Apurimac Arauca Caquetá Cauca Chapare Chocó Guaviare Huallaga Meta Nariño Norte de Santander

  16. Authentic Leaf Samples

  17. Isoscapes δ13C δ2H δ15N

  18. Alkaloidscapes Tropacocaine Trimethoxycocaine Total Truxillines

  19. Final Solution Cocaine Bolivia/Peru PLS_1 Chapare PLS_1A CUSCO PLS_1A01 PLS_1A01A Valle de Cauca PLS_1A01B W-Caqueta PLS_2A01 UHV PLS_1A01B1 San Lucas PLS_2 PLS_2A Arauca PLS_2A02 NDS(I) Choco PLS_3 PLS_3A Antioquia PLS_4 PLS_4A Vaupes PLS_3A01 Meta Narino PLS_4A01 Colombian Santander NDS(II) PLS_5 PLS_5A Vichada Amazonas PLS_5A01 PLS_6 E-Caqueta PLS_6A Guaviare Putumayo PLS_6A01 Cauca

  20. Impacts of Sub-Regional Data

  21. CY 2016 Sub-Regional Classifications

  22. Heroin Signature Program Mission Origin Determination by Chemical Analyses • Research Projects • Operation Breakthrough • Heroin Sig II Compounds • Opium and Heroin Processing • Opium and Heroin Synthesis • Opium Signature • Heroin and Opium Origin Determination

  23. Heroin Signature Program Research • Monitoring Opium Poppy Cultivation: • Conduct ongoing assessment of illicit and licit opium cultivation • Monitor via opium poppy field surveys and with analysis of hundreds of opium samples • Provides the foundation for Heroin Signature and Opium Signature methodologies

  24. Heroin Signature Program Research • Collaborations with Universities through CTTSO funding: • Heroin geo-sourcing using opium poppy DNA (with Syracuse University). The developed method is getting published in Nature Scientific Reports. • Heroin geo-sourcing using Sr isotope ratios and trace elemental analysis (with Florida International University and University of Miami).

  25. Methamphetamine Profiling Program Mission Determine Synthetic Routes Monitor Precursor Chemicals Monitor Reagents and Solvents Track Manufacturing Trends • Research Projects • MPP • ICPMS • Synthesis of Phenethylamines and Tryptamines

  26. PSE-Based Meth versus P2P-Based Meth Percentage of Samples

  27. New P2P-Based Profile from Mexico • MPP has been tracking this chemistry since approximately 2014 • Nitrostyrene (NTS) is the pre-precursor • Other essential chemicals: • Benzaldehyde (BNZ) • Nitroethane (NTE) • Iron Powder (BNZ + NTENTSP2PMeth) Note: Mono-methylamine is needed from P2P to Meth.

  28. Special Testing and Research Laboratory Research into specific instrumentation or agency-driven initiatives • Instrument Evaluation • Liquid Phase Separations • Reference Materials • Nuclear Magnetic Resonance Spectroscopy • Isotope Ratio Mass Spectrometry • Organic Synthesis • Opportunities to collaborate?

  29. Research into Field-Deployable Instrumentation Needs: adapt to potential threat facing LEO • Agents require presumptive indications • Colorimetric test kits no longer permitted • Field-deployable instruments needed • Requirements • Easy-to use • Lightweight • Short analysis time • Discrimination power

  30. Evaluations Sample in bag • Request For Information placed • Raman spectrophotometers • Mass spectrometers • Evaluated for • Intuitive user interface (technical and non-technical users) • Compatibility with known samples/matrices • User-added spectral library freedom Raman

  31. Research using Liquid Phase Separations • Method Development: Abundance of Porphyroxine in Opium from Heroin Producing Regions by UHPLC-MS/MS • Porphyroxineis an alkaloid that can be used to differentiate opium samples from diverse cultivars of poppies. • Research continues to quantitate trace alkaloids such as laudanosine, codamine, etc. in both opium and heroin samples.

  32. Structural Elucidation Research 23 compounds structurally elucidated in 2016 No available reference materials and no comparable data: • NMR Experimentation (1D & 2D) • Proton NMR (HNMR) • Carbon NMR (CNMR) • Correlation Spectroscopy (COSY) • Heteronuclear Single Quantum Coherence (HSQC) • Heteronuclear Multiple Bond Correlation (HMBC) • MS Interpretation • EI - Fragmentation • Accu-TOF DART – Exact mass & fragmentation • Salt Form, Isomer and other tests as appropriate

  33. SWGDRUG Monographs General Information • IUPAC Name • Synonyms Chemical and Physical Data Qualitative Data • NMR • GC/MS • FTIR • Sample preparation • Instrument parameters Additional Resources • Links to other resources • Article citations • 250 since 2012

  34. Special Testing and Research Laboratory Ongoing Research Initiatives • Research Associate Laboratory Director • Partner with Universities and Other Federal Agencies • Seek Outside Funding Streams • Conduct Internal Review and Modify Project Initiation Protocols • Continue to Explore Basic and Applied Research Opportunities

  35. Thank You for Your Attention Jeffrey H. Comparin Laboratory Director Drug Enforcement Administration Special Testing and Research Laboratory 22624 Dulles Summit Court Dulles, VA 20166 jeffrey.h.comparin@usdoj.gov

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