2 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 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. 3 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 Class 1: Classic Cannabinoid Class 2: Basic non classic Cannabinoid Class 3: Naphtoylindole Class 4: Phenylacetylindole Class 5: Benzoylindole 5
(+-)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
Plant Extract/ Fatty Acids
Identification of JWH-203
Other Cannabimimetics spectra recently acquired on the DiscovIR-GC JWH-237 AM694 4-iodo isomer JWH-081 JWH-251 JWH-206 JWH-022 JWH-398 RCS-4 JWH-018 JWH-016 RCS-8 RCS-4 3-methoxy isomer JWH-018 1 napthyl isomer JWH-020 RCS-8 3-methoxy isomer RCS-4 2-methoxy isomer JWH122 JWH-015 RCS-8 4-methoxy isomer JWH-073 AM2201 JWH-007 JWH-200 JWH-073 2 napthyl isomer AM2201 2 napthyl isomer JWH-018 adamantyl JWH-200 2 napthyl isomer JWH-250 JWH-098 RCS-4 C4 homolog AM-694 JWH-201 JWH-210 JWH-203 AM-694 3-iodo isomer 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 18
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
Cryogenic LN2 IR Detector Interferometer PCB Sample deposit ZnSe window M C T ABB Bomem Vacuum chamber 21 Precision Vacuum Backplate Optical path
Heated Transfer line
GC-IR/MS
24 Loading the sample disk
Sample collection mechanism DiscovIR VACUUM CHAMBER, (10-4 torr) Resistive Heaters +/-5 o C Disc auto load/unload 25 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 26
Chromatogram Trace Spectrum Trace Spectrum 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
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
Emerging Threat 2C-Phenethylamines
Bath salt sample Analysis
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 Noise or Split Band? Sample at RT 21.9 minutes after 600 scans 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