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DiscovIR-GC™
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The Epidemic is coming (Tucson News KOLD/KMSB)
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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.
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Multiple isomers to choose from !!! A cannabinoid Example
Class 1: Classic Cannabinoid Class 2: Basic non classic Cannabinoid Class 3: Naphtoylindole
Class 4: PhenylacetylindoleClass 5: Benzoylindole
(+-)CP 47,497 (1R,3S) or (1S,3R)
CP47,497 Diastereomers and Homologs
JWH-250
JWH-302
JWH-201
DiscovIR-GC
Positional Isomers
JWH 302 vs JWH-201
Analysis of a K-2 Sky Sample
Plant Extract/ Fatty Acids
Identification of JWH-203
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
Other Cannabimimetics spectra recently acquired on the DiscovIR-GC
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
Step #3 Chemical Identification - using FTIR specificity (positional and stereoisomers)
Step #2 Controlled Deposition - unique solid phase deposition.
GC typical
How does it work ?
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GC-IR System optics
Polystyrene CalibrationInfrared beam
NIST Traceable polystyrene filmfor daily calibration test Acquisition of solid phase
transmission spectra through ZnSe disc
Disc Track Pointer
End Sample 2 RT= 20.0 min
Start Sample 2 RT= 0.0 min
Records linear positionand rotary position forFor every spectra
Infrared beam fixed in position
ZnSE Disc rotatescounterclockwise
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Sample deposit ZnSe window
Optical path
Vacuum chamber
ABB BomemMCT
Precision Vacuum Backplate
Cryogenic LN2
IR Detector
Interferometer PCB
Heated Transfer line
GC-IR/MS
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Loading the sample disk
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DiscovIR VACUUM CHAMBER, (10-4 torr)
4 inch diameter ZnSe disc, washable & reusable Holds 50 hours of chromatography in spiral track Auto location, Checks for sample, Post dep. analysis
Resistive Heaters +/-5oC
Disc auto load/unload
Sample collection mechanism
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Data Acquisition and Instrument Control software based on Thermo GRAMS™
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Spectrum Trace
Spectrum Trace
Chromatogram Trace
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 preparationSample can be extracted/prepared as if
analyzing via GC/MSMeOH (dilute and shoot type)Basic CHCl3, Basic Hex, Acidic CHCl3Acidic 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
CMP
MethamphetaminePseudoephedrine
Diastereomers in Meth Synthesis
Pseudoephedrine
Ephedrine
Pseudoephedrine IR SpectrumDirect 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
Sample at RT 21.9 minutesafter 600 scans
Advantage of Solid Phase DD GC-IR
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)AmphetamineCodeine cough syrupHeroinMorphine (residues from spoons, straws, syringes etc)CocaineClandestine tabletsOxycodone (residues from spoons, straws, syringes, etc)Tryptamines and phenethylaminesBath Salts Cannabinoids