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DiscovIR-GC ™. The Epidemic is coming (Tucson News KOLD/KMSB). Synthetic Analog Problem. DEA Temporary Placement of JWH-018, JWH-073, JWH-200, CP47,497 and CP47,497 C8 homolog, MDPV, Mephedrone, Methylone on Schedule 1 H.R. 1254: Synthetic Drug Control Act of 2011

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synthetic analog problem
Synthetic Analog Problem
  • DEA Temporary Placement of JWH-018, JWH-073, JWH-200, CP47,497 and CP47,497 C8 homolog, MDPV, Mephedrone, Methylone on Schedule 1
  • H.R. 1254: Synthetic Drug Control Act of 2011
  • AK S 17: Classifies certain synthetic cannabinoids as schedule IIA controlled substances.
  • AL H 158, S 207 and S 208: Relates to schedule I controlled substances; provides legislative findings relating to controlled substance analogs; adds cathinone compounds, certain named chemical compounds of synthetic cannabinoids, and controlled substance analogs to the schedule I controlled substances list subject to regulation and penalties in the same manner as other controlled substances.
  • AZ S 1043: Relates to dangerous drugs; relates to definition.
  • AZ H 2388: Adds AM-2201 and JWH-122 to the definition of “dangerous drugs” and to schedule I. Relates to authority to define the chemical composition of controlled substances included in drug schedules; provides for authority to include chemical variations of those substances as necessary; provides consideration of a substance’s potential for abuse, pharmacological effect, current scientific knowledge and the risk to public health; requires written report; exempts the board of pharmacy from rulemaking requirements.
  • CA A 2420: Provides that every person who possesses, under circumstances that do not include possession for sale as proscribed pursuant to existing law, 28.5 grams or less of any synthetic cannabinoid or any synthetic stimulant compound, or any synthetic stimulant derivative is guilty of an infraction punishable by a specified fine.
  • HI S 1305: Adds HU-210, JWH-018, JWH-073 to controlled substances provisions.
multiple isomers to choose from a cannabinoid example
Multiple isomers to choose from !!! A cannabinoid Example

Class 1: Classic Cannabinoid

Class 2: Basic non classic Cannabinoid

Class 3: Naphtoylindole

Class 4: Phenylacetylindole

Class 5: Benzoylindole

slide8

DiscovIR-GC

Positional Isomers

JWH-250

JWH-302

JWH-201

slide14

Other Cannabimimetics spectra recently acquired on the DiscovIR-GC

JWH-237

JWH-206

JWH-018

JWH-018 1’napthyl isomer

JWH122

AM2201

AM2201 2’napthyl isomer

JWH-098

JWH-210

AM694 4-iodo isomer

JWH-022

JWH-016

JWH-020

JWH-015

JWH-007

JWH-018 adamantyl

RCS-4 C4 homolog

JWH-203

JWH-081

JWH-398

RCS-8

RCS-8 3-methoxy isomer

RCS-8 4-methoxy isomer

JWH-200

JWH-200 2’ napthyl isomer

AM-694

AM-694 3-iodo isomer

JWH-251

RCS-4

RCS-4 3-methoxy isomer

RCS-4 2-methoxy isomer

JWH-073

JWH-073 2’napthyl isomer

JWH-250

JWH-201

JWH-302

slide15

DiscovIR-GC™ The Solution for Designer Drugs

GC typical

Step #1 Separation by Gas Chromatography

Step #2 Controlled Deposition - unique solid phase deposition.

Step #3 Chemical Identification - using FTIR specificity (positional and stereoisomers)

polystyrene calibration
Polystyrene Calibration

Infrared beam

NIST Traceable polystyrene film

for daily calibration test

Acquisition of solid phase transmission spectra through

ZnSe disc

disc track pointer
Disc Track Pointer

Infrared beam fixed in position

Start Sample 2 RT= 0.0 min

End Sample 2 RT= 20.0 min

ZnSE Disc rotates

counterclockwise

Records linear position

and rotary position for

For every spectra

slide21

Cryogenic LN2

IR Detector

PCB

Interferometer

ABB Bomem

MCT

Sample deposit ZnSe window

Vacuum

chamber

Precision Vacuum Backplate

Optical path

discovir vacuum chamber 10 4 torr
DiscovIR VACUUM CHAMBER, (10-4 torr)

Sample collection mechanism

Resistive Heaters +/-5oC

Disc auto load/unload

4 inch diameter ZnSe disc, washable & reusable Holds 50 hours of chromatography in spiral track Auto location, Checks for sample, Post dep. analysis

slide27

Chromatogram Trace

Spectrum Trace

Spectrum Trace

slide28

QA/QC / Performance Qualification

  • Voltage check to ensure detector is working properly
  • Noise check to ensure proper signal/noise ratio
  • NIST traceable polystyrene scan is performed
  • A test mix (amphetamine, phentermine, pseudoephedrine, caffeine, cocaine and alprazolam) enables :
      • GC check (proper separation)
      • IR detector (proper identification)
slide30

Typical Case Work Sample Preparation

  • Sample preparation
    • Sample can be extracted/prepared as if analyzing via GC/MS
    • MeOH (dilute and shoot type)
    • Basic CHCl3, Basic Hex, Acidic CHCl3
    • Acidic Hex
  • Normal GC/MS vials can be used

no real change of procedure needs to be employed

methamphetamine via shake and bake method analysis of a field sample by gc ir
Methamphetamine via Shake and Bake method:Analysis of a field sample by GC-IR

Pseudoephedrine

Methamphetamine

CMP

diastereomers in meth synthesis
Diastereomers in Meth Synthesis

Ephedrine

Pseudoephedrine

pseudoephedrine ir spectrum direct deposition vs solid phase reference
Pseudoephedrine IR SpectrumDirect Deposition VS. Solid Phase Reference

Comparable To Solid phase/condensed phase IR spectra run with:

- ATR

- KBR pellet

- Nujol Mull

bath salt sample analysis
Bath salt sample Analysis

advantage of solid phase dd gc ir1
Advantage of Solid Phase DD GC-IR

Noise or Split Band?

Sample at

RT 21.9 minutes

after 600 scans

Rescan enables increases SNR for Decision

slide55

Clandestine Tablets

Most clandestine tablets are mixtures

Can obtain an infrared spectra for each component

With the DB-35 column can separate BZP, TFMPP and MDMA (see figures 4-7)

Isomer determination for MDMA, TFMPP and CPP (to name just a few)

why use discovir gc
Why use DiscovIR-GC?

Resolve and identify mixed analytes in a single instrument and procedure.

GC-FTIR provides two analytical methods in one operation.

High resolution solid phase spectra

Self-cleaning IR disk. No need to manually clean off old samples.

Automatic operation up to 50 hours: Autosampler-compatible.

Spectral identification library software.

Nanogram sensitivity.

Flow splitting: can interface with existing GC–MS instrumentation.

Real-time or post-run data collection. Allows re-analysis of deposited samples

slide59

Substances Routinely Analyzed via GCIR system

  • Methamphetamine (includes clan lab, powder and residues)
  • Amphetamine
  • Codeine cough syrup
  • Heroin
  • Morphine (residues from spoons, straws, syringes etc)
  • Cocaine
  • Clandestine tablets
  • Oxycodone (residues from spoons, straws, syringes, etc)
  • Tryptamines and phenethylamines
  • Bath Salts
  • Cannabinoids