Detection and Identification of Illicit Drugs and Cutting Agents in - - PowerPoint PPT Presentation

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Detection and Identification of Illicit Drugs and Cutting Agents in - - PowerPoint PPT Presentation

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Detection and Identification of Illicit Drugs and Cutting Agents in Seized Street Drugs: Benchtop NMR Spectrometer & Databasing Software ACD/Labs User Meeting Susanne D. Riegel, Alexander F. G. Maier, Dimitris Argyropoulos, Marie Lange,

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ACD/Labs User Meeting

Baltimore, MD March 8th, 2020

Detection and Identification of Illicit Drugs and Cutting Agents in Seized Street Drugs: Benchtop NMR Spectrometer & Databasing Software

Susanne D. Riegel, Alexander F. G. Maier, Dimitris Argyropoulos, Marie Lange, Marion Baumgarte

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NMR Instruments and Field Strength

Dalitz, F.; Cudaj, M.; Maiwald, M.; Guthausen, G.; Prog. Nuc. Mag. Reson. Spec. 2012, 60, 52 2

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Illegal Drugs

  • Typically classified by:

– Legal Classification – e.g., Schedule I, Class A – Effect – e.g., depressant, stimulant, hallucinogen – Molecular Structure – e.g., cannabinoids, opioids, phenethylamines

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Amphetamine Stimulant Methamphetamine Stimulant MDMA Psychedelic, entactogen

  • Designer Drugs – synthetic analog of a legal restricted or prohibited drug devised to

avoid drug detection and identification.

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New Psychoactive Substances* (from 2-phenyethylamine)

4 * Defined by EU 2015/1535 ‘Act to combat the distribution of new psychoactive substance’

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Why Benchtop NMR Spectroscopy?

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Nik Wipes IR HPLC High-field NMR Benchtop NMR Sample Prep ✓ Easy ✓ Easy X Tedious ✓ Easy ✓ Easy Sample Conc ~ Medium ~ Low-medium ✓ Low ~ Low-medium ~ Medium Analysis Time ✓ <1 min ✓ <1 min X >15 min ✓ <1 min ✓ <1 min Location ✓ On-site ✓ On-site X Off-site X Off-site ✓ On-site Standards X Required X Required X Required ✓ Not Required ✓ Not Required Quantitative X X with calibration X with calibration ✓ w/o calibration ✓ w/o calibration Capital Cost $ $ $$ $$$$ $$ Operating Expenditure $ $ $$ $$$ $

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SLIDE 6

Considerations for Mobile Laboratory

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  • Stability – temperature (AC & simple heating block), vibration (soft or hard)
  • Mounting
  • Power consumption
  • Automation
  • Accuracy/reliability
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Sample Preparation and 1H NMR Acquisition

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1D 1H NMR spectrum at 60 MHz

Unknown Search Queries

  • ~30 mg of an unknown drug sample

dissolved/suspended in vials of ~0.6 mL DMSO-d6 and D2O

  • Vials were capped and agitated for 1 min
  • Liquid phase transferred to NMR tube

Reference Standards

  • 60 µmol of sample dissolved in

~0.6 mL DMSO-d6 or D2O (if insoluble)

  • Vial capped and agitated until dissolved

completely.

  • Transferred to NMR tube

SAMPLE PREP:

1H NMR DATA ACQUISITION (performed at LKA):

SW = 80 ppm SW center = 20 ppm np = 8192 scan delay = 1 s ns = 16 or 64 time = 1 min or 4 min

  • Zero Fill
  • Phase

PRE-PROCESSING (ACD/Labs Macro for automatic processing):

  • Baseline
  • solvent detection
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Database

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Creating a Macro

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Creating a Macro

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Creating a Macro

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Automated Preprocessing: Apply Macro

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Automated Preprocessing: Apply Macro

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Case Study: Unknown Street Drug

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  • 1. Sample Prep of Unknown:
  • Spatula of unknown added to vial of ~0.6 mL D2O
  • Sealed and agitated for 1 min
  • Liquid phase transferred to NMR tube
  • 2. 1H NMR Spectra Acquisition
  • 3. Load into ACD/Spectrus
  • Auto Preprocessing Macro
  • Peak Search with ACD/Spectrus DB
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Open Unknown 1H NMR Spectra into ACD/Labs

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Search Database

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Database Search Options

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Database Search

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First Database Hits: Cocaine

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Auto Select Best Hits

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Database Best Hits

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Adjust Intensity

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Optimize Hit

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Optimize hit for Cocaine

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Residuals of Best Fit for Unknown & Cocaine Std

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Optimize Hit for Lactose

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Manually Change Intensity

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Manually Change Intensity

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Manually Change Intensity

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Visualize Sum Instead of Residuals

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Sum of Database Components on Unknown

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Manually Investigate Other Potential Hits

32 N N O NH CH3 CH3 Cl

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Visualize Inspect Benzydiamine HCl

33 N N O NH CH3 CH3 Cl

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Visually Inspect bk-2C-B HCl

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Br O CH3 O H3C O NH3 Cl

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Visually Inspect Caffeine

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Optimize Intensity

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Horizontal Offset Adjustment

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Line Broadening Adjustment

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Optimize Hit

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Caffeine Optimized

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Visually Inspect Sorbitol

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OH OH OH OH OH HO

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Visually Inspect D-Mannitol

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Visually Inspect Citric Acid

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OH O OH O OH O HO

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Select all Matching Components

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Inspect Matching Components: Sum

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Case Study: Cocaine cont.

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Case Study: Cocaine cont.

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Report: Street Drug Cocaine HCl

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Compare with GC-MS analysis:

  • Cocaine HCl (41.9%)
  • Caffeine
  • Lactose
  • D-mannitol/sorbitol

Cocaine HCl

83.33 match

Lactose

50.00 match

Caffeine

33.33 match

D-Mannitol

16.67 match

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SLIDE 49

Conclusions and Future Work

  • Successfully acquired and built database for 150+ illicit drugs and cutting agents
  • Peak pick allowed relatively automatic identification of peaks
  • Want to develop fingerprinting/similarity structures flags

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SLIDE 50

Thanks and Acknowledgments

Nanalysis

Juan Araneda Terry Chu Paul Hui Neal Gallagher Adam Paulson Amro Hussein

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Kriminaltechnisches Institut

Christian Vidal Nicole Lehnert

ACD/Labs

Michel Riese