authentication of reference materials - nist · authentication of reference materials 1. ......
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Authentication of Reference Materials
Roxanne E. Franckowski Senior Forensic Chemist
Special Testing and Research Laboratory Drug Enforcement Administration
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DEA Special Testing and Research Laboratory Reference Materials Program
Topics
• Reference Material Sources
• Authentication Process
• Monographs
• Contact Information
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DEA Special Testing and Research Laboratory Reference Materials Program
Where do DEA Reference Materials come from?
• Purchased from commercial sources
• Synthesized in-house
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DEA Special Testing and Research Laboratory Reference Materials Program
Authentication of Reference Materials
1. Verify structure of the Reference Material (RM)
2. Determine the purity of the RM
Why??
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DEA Special Testing and Research Laboratory Reference Materials Program
Purity Determination
• Quantitative Nuclear Magnetic Resonance (NMR)
– Use a NIST traceable internal standard
– Multiple analyses in order to establish an uncertainty value
– Material must be ≥98.0% for quantitative reference materials & ≥90.0% for qualitative reference materials
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DEA Special Testing and Research Laboratory Reference Materials Program
Purity Determination
• Chromatography – Gas Chromatography/Flame Ionization
Detector (GC/FID)
– Liquid Chromatography/Photodiode Array Detector (UPLC/PDA)
– Capillary Electrophoresis (CE)
• Differential Scanning Calorimetry – Also provides Melting Point data
• Thermogravimetric Analysis (TGA) – Water of Hydration
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DEA Special Testing and Research Laboratory Reference Materials Program
Structural Confirmation
• Required:
– NMR
– Gas Chromatography/Mass Spectrometry (GC/MS)
– Infrared Spectroscopy (FTIR)
• As needed:
– Polarimetry/CE for isomer determination
– Microcrystalline tests/Optical crystallography
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DEA Special Testing and Research Laboratory Reference Materials Program
Structural Confirmation
• Data from identification techniques are compared to:
– Instrumental Data of Drug Analysis (IDDA)
– Clarke’s Analysis of Drugs and Poisons
– Peer reviewed articles
– Previous lots of reference materials
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DEA Special Testing and Research Laboratory Reference Materials Program
Authentication Process Recap
Reference Material (RM)
Received
Either Purchased or Synthesized
Entered into RM inventory
Purity Determination
NMR, Chromatography,
DSC, TGA
≥98.0% for quantitative
purposes
Structural Confirmation
NMR, MS, FTIR Compare to literature or
previous RM data
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DEA Special Testing and Research Laboratory Reference Materials Program
What happens when there is no previous
data for comparison? Structural Elucidation
Compare to literature or previous RM data?
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DEA Special Testing and Research Laboratory Reference Materials Program
Structural Elucidation
• 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
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DEA Special Testing and Research Laboratory Reference Materials Program
Authentication Process Recap
RM Received Authentication Structural
Elucidation (if needed)
Report written Peer review RM ready for
circulation
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DEA Special Testing and Research Laboratory Reference Materials Program
How can DEA assist other forensic laboratories?
• Provide spectra
– MS & IR data
• Provide drug monographs for SWGDRUG
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DEA Special Testing and Research Laboratory Reference Materials Program
SWGDRUG MONOGRAPHS
www.swgdrug.org
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DEA Special Testing and Research Laboratory Reference Materials Program
SWGDRUG MONOGRAPHS
www.swgdrug.org
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DEA Special Testing and Research Laboratory Reference Materials Program
SWGDRUG MONOGRAPHS
www.swgdrug.org
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DEA Special Testing and Research Laboratory Reference Materials Program
SWGDRUG MONOGRAPHS www.swgdrug.org
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DEA Special Testing and Research Laboratory Reference Materials Program
SWGDRUG MONOGRAPHS www.swgdrug.org
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DEA Special Testing and Research Laboratory Reference Materials Program
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DEA Special Testing and Research Laboratory Reference Materials Program
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DEA Special Testing and Research Laboratory Reference Materials Program
SWGDRUG MONOGRAPHS
Contain: General Information
Chemical and Physical Data
Additional Resources Links to websites
Article references
Qualitative Data Spectra for NMR, MS, & IR
Sample preparation and Instrumental conditions used
Any analytical observations during data collection
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DEA Special Testing and Research Laboratory Reference Materials Program
Contact Information
Questions regarding:
• Reference Materials:
• SWGDRUG Monographs:
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DEA Special Testing and Research Laboratory Reference Materials Program
Thank You