Laboratory Research Overview Forensic Science Research Federal Stakeholders Meeting February 2018 Jeffrey H Comparin Laboratory Director Drug Enforcement Administration Special Testing and Research Laboratory ID: 932173
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DEA Special Testing and Research LaboratoryResearch Overview Forensic Science Research Federal Stakeholders Meeting February 2018
Jeffrey H. ComparinLaboratory DirectorDrug Enforcement AdministrationSpecial Testing and Research Laboratory
Slide2The 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
MissionLab System –
STRL
Vision
Global Leader in Forensic Science
Slide3Dedicated Research GroupGroup Supervisor and Seven GS-14 Senior Research ChemistsThree support existing Special Programs
and conduct novel researchTwo are technology specificNMRIRMSOne is an organic synthetic chemistOne specializes in clandestine laboratoriesAcademic Backgrounds Vary~20 Current ProjectsProgram 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
Special Testing and Research Laboratory
Slide4Research BudgetRelevant, pre-competitive fundamental research to drive innovation
Funding is leveraged to provide maximum value to industry, academia, and governmentSpecial Testing and Research Laboratory
Slide5Fentanyl Signature Profiling Program
MissionGather Strategic and Tactical IntelligenceLink SeizuresDetermine Synthetic Route Determine Trafficking Routes
Develop “Consolidated Priority Organization Targets” (CPOT)
Research Projects
Organic Synthesis
Characterization of Unknown Compounds
Slide6Quantitative Determination via NMR
Counterfeit oxycodone tabletsA=Acetaminophen = 26.1%C=Caffeine = 3.2%D=Dipyrone = 17.4%
F=Fentanyl = 1.3%
L=Lactose = 15.6%
Solvent=D
2
O
Maleic acid=ISTD
Slide7GC-MS Impurity Profiles
Relatively clean profiles = 87% of samplesFentanyl
High purity fentanyl
+ Adulterants =
12%
of samples
Fentanyl-related impurities enriched
<1%
of samples
Slide8Static Headspace-GC-MS
ISTDCH2Cl2 (0.073%)
ISTD
Acetone (0.301%)
trace CH
2
Cl
2
(0.002%)
EtOH
(0.009%)
MeOH
(0.195%)
EtOAc
(0.001%)
MeOAc
(0.006%)
Slide9Fentanyl Moiety Isotopes
Fentanyl
4-ANPP C
3
H
5
O
δ
15
N
δ
13
C
δ
15
N
δ
13
C
δ
13
C
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
Slide102 Separate Seizures (Linked)
08-22-16
IN
2 kg
08-14-16
CA
24 kg
6.0% Fentanyl
44.8% Dipyrone
20.1% Mannitol
24.0% Lactose
6.0% Fentanyl
45.4% Dipyrone
25.5% Mannitol
22.8% Lactose
Dipyrone
artifacts
Fentanyl
δ
15
N=1.8
δ
13
C=-28.5
Fentanyl
δ
15
N=1.8
δ
13
C=-28.5
Identical solvent profiles:
Acetone
CH
2
Cl
2
Toluene
Mesityl
oxide
4-ANPP
322-1
N-
phenylpropanamide
Slide11Acetaminophen
Caffeine
Dipyrone Artifact
C-24 ISTD
4-ANPP
Fentanyl
δ
13
C
=-29.8
Caffeine
δ
13
C
=-32.2
Benzylfentanyl
(
J
)
Acetylfentanyl
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*
06-23-16
CA
4.6 kg
1.2% Fentanyl
18.7% Dipyrone
25.5% Acetaminophen
3.2% Caffeine
12.5% Mannitol*
Fentanyl
δ
13
C
=-29.8
Caffeine
δ
13
C
=-32.2
Slide12Samples Examined and Linkages
41
Sets of
seizure linkages made to date that include:
73
different cases/seizures
169
different exhibits
Over
300 kg fentanyl
originating
from
China
and
Mexico
Over 1,100 illicit fentanyl samples examined
Slide13Cocaine Signature Program
MissionOrigin Determination by Chemical Analyses
Research Projects
CSP
Operation Breakthrough
Cocaine IRMS
Differentiation of Growing Regions
Slide14Cocaine Signature Program History
More than
30
years of research producing over
100
scientific publications in peer-reviewed journals
Slide1519 Growing Regions
Amazonas
Antioquia
Apurimac
Arauca
Caquetá
Cauca
Chapare
Chocó
Guaviare
Huallaga
Meta
Nariño
Norte de
Santander
Putumayo
San
Lucas
Santander
Valle
de Cauca
Vaupés
Vichada
Slide16Authentic Leaf Samples
Slide17Isoscapes
δ
13
C
δ
15
N
δ
2
H
Slide18Alkaloidscapes
Tropacocaine
Trimethoxycocaine
Total
Truxillines
Slide19Cocaine
PLS_1
Chapare
UHV
CUSCO
Valle de Cauca
Antioquia
Meta
PLS_1A
PLS_1A01
PLS_3
PLS_3A
W-Caqueta
San Lucas
Arauca
NDS(I)
PLS_2
PLS_2A
PLS_2A01
PLS_2A02
PLS_3A01
Vaupes
Narino
Santander
PLS_4
PLS_4A
PLS_4A01
NDS(II)
Vichada
Amazonas
PLS_5
PLS_5A
E-Caqueta
Guaviare
Putumayo
Cauca
PLS_6
PLS_6A
PLS_6A01
PLS_1A01A
PLS_1A01B
PLS_1A01B1
Bolivia/Peru
Colombian
PLS_5A01
Choco
Final Solution
Slide20Impacts of Sub-Regional Data
Slide21CY 2016 Sub-Regional Classifications
Slide22Heroin Signature Program
MissionOrigin 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
Slide23Monitoring 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 samplesProvides the
foundation
for Heroin Signature and Opium Signature
methodologies
Heroin Signature Program Research
Slide24Collaborations 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).
Heroin Signature Program Research
Slide25Methamphetamine Profiling ProgramMissionDetermine Synthetic RoutesMonitor Precursor ChemicalsMonitor Reagents and SolventsTrack Manufacturing
Trends
Research Projects
MPP
ICPMS
Synthesis of Phenethylamines and Tryptamines
Slide26PSE-Based Meth versus P2P-Based Meth
Percentage of Samples
Slide27MPP has been tracking this chemistry since approximately 2014Nitrostyrene (NTS) is the pre-precursor Other essential chemicals:Benzaldehyde (BNZ)Nitroethane (NTE)Iron Powder
(BNZ + NTENTSP2PMeth)Note: Mono-methylamine is needed from P2P to Meth.
New P2P-Based Profile from Mexico
Slide28Research into specific instrumentation or agency-driven initiativesInstrument EvaluationLiquid Phase
SeparationsReference MaterialsNuclear Magnetic Resonance SpectroscopyIsotope Ratio Mass SpectrometryOrganic SynthesisOpportunities to collaborate?
Special Testing and Research Laboratory
Slide29Research into Field-Deployable InstrumentationNeeds: adapt to potential threat facing LEOAgents require presumptive indications Colorimetric test kits no longer permittedField-deployable instruments neededRequirementsEasy-to use
LightweightShort analysis timeDiscrimination power
Slide30EvaluationsRequest For Information placedRaman spectrophotometersMass spectrometersEvaluated forIntuitive user interface (technical and non-technical users)Compatibility with known samples/matricesUser-added spectral library freedom
Raman
Sample in bag
Slide31Research using Liquid Phase SeparationsMethod Development: Abundance of
Porphyroxine in Opium from Heroin Producing Regions by UHPLC-MS/MSPorphyroxine is 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.
Slide32No 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 InterpretationEI - FragmentationAccu-TOF DART – Exact mass & fragmentationSalt Form, Isomer and other tests as appropriate
23 compounds structurally elucidated in 2016
Structural Elucidation Research
Slide33SWGDRUG MonographsGeneral InformationIUPAC Name SynonymsChemical and Physical Data
Qualitative DataNMRGC/MSFTIRSample preparation
Instrument parameters
Additional Resources
Links to other resources
Article citations
250 since 2012
Slide34Ongoing Research InitiativesResearch Associate Laboratory DirectorPartner with Universities and Other Federal Agencies
Seek Outside Funding StreamsConduct Internal Review and Modify Project Initiation ProtocolsContinue to Explore Basic and Applied Research OpportunitiesSpecial Testing and Research Laboratory
Slide35Thank You for Your AttentionJeffrey H. Comparin
Laboratory DirectorDrug Enforcement AdministrationSpecial Testing and Research Laboratory22624 Dulles Summit CourtDulles, VA 20166
jeffrey.h.comparin@usdoj.gov