DiscovIR-GC ™

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The Epidemic is coming (Tucson News KOLD/KMSB)

Synthetic Analog Problem

3         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

5 Class 1: Classic Cannabinoid Class 2: Basic non classic Cannabinoid Class 3: Naphtoylindole Class 4: Phenylacetylindole Class 5: Benzoylindole

(+-)CP 47,497 (1R,3S) or (1S,3R)

CP47,497 Diastereomers and Homologs

DiscovIR-GC Positional Isomers JWH-250 JWH-302 JWH-201

JWH 302 vs JWH-201

Analysis of a K-2 Sky Sample

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Plant Extract/ Fatty Acids

Identification of JWH-203

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

DiscovIR-GC ™ The Solution for Designer Drugs

Step #1 Separation by Gas Chromatography GC typical Step #2 Controlled Deposition - unique solid phase deposition.

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

How does it work ?

GC-IR System optics

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Polystyrene Calibration

Infrared beam NIST Traceable polystyrene film for daily calibration test Acquisition of solid phase transmission spectra through ZnSe disc

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

Sample deposit ZnSe window Vacuum chamber

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Precision Vacuum Backplate Optical path Cryogenic LN2 IR Detector Interferometer PCB M C T ABB Bomem

Heated Transfer line

GC-IR/MS

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Loading the sample disk

Sample collection mechanism

DiscovIR VACUUM CHAMBER, (10 -4 torr)

Resistive Heaters +/-5 o C Disc auto load/unload

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

Data Acquisition and Instrument Control software based on Thermo GRAMS ™

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Spectrum Trace Spectrum Trace Chromatogram Trace 27

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)

Example of a Daily Test Mix Chromatogram

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

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Amphetamine mixture Chromatogram

Amphetamine & Methamphetamine

Fingerprint Region

MDA & MDMA

Phentermine & Methamphetamine

Methamphetamine via Shake and Bake method: Analysis of a field sample by GC-IR

Methamphetamine Pseudoephedrine CMP

Diastereomers in Meth Synthesis

Ephedrine Pseudoephedrine

Pseudoephedrine IR Spectrum Direct Deposition VS. Solid Phase Reference

Comparable To Solid phase/condensed phase IR spectra run with: - ATR - KBR pellet - Nujol Mull

FTIR Specificity: Pseudoephedrine hit list

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Emerging Threat 2C-Phenethylamines

Bath salt sample Analysis

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4-fluoromethcathinone overlaid with 3 fluoromethcathinone

Solid Phase Mid-IR Spectrum of Mephedrone

Solid Phase Mid-IR Spectrum of Lidocaine

Solid Phase Mid-IR Spectrum of MDPV

Presence of one Cannabinoids: JWH-018

Advantage of Solid Phase DD GC-IR

Advantage of Solid Phase DD GC-IR

Sample at RT 21.9 minutes after 600 scans

Noise or Split Band?

Rescan enables increases SNR for Decision

JWH-073 and JWH-015 isomers MW 327.4

JWH-073 overlaid with JWH-015 isomer

Library search of JWH-15 versus library of 40 cannabinoids results in quality score of 0.97

Tryptamines

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)

Exhibit containing BZP, TFMPP, MDMA and Caffeine

Clandestine Tablet: Containing BZP, TFMPP, MDMA and Caffeine

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

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