OUTLINE - Spectra Analysis

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DiscovIR-GC™
The Epidemic is coming (Tucson News
KOLD/KMSB)
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Synthetic Analog Problem
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H.R. 1254: Synthetic Drug Control Act of 2011
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AK S 17: Classifies certain synthetic cannabinoids as schedule IIA controlled substances.
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DEA Temporary Placement of JWH-018, JWH-073, JWH-200, CP47,497 and CP47,497 C8
homolog, MDPV, Mephedrone, Methylone on Schedule 1
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
Class 1: Classic Cannabinoid
Class 2: Basic non classic Cannabinoid
Class 4: Phenylacetylindole
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Class 3: Naphtoylindole
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
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
Step #2 Controlled Deposition - unique solid phase
deposition.
Step #3 Chemical Identification - using FTIR
specificity (positional and stereoisomers)
GC
typical
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
Cryogenic LN2
IR Detector
Interferometer
ABB Bomem
M
C
T
Sample deposit
ZnSe window
Vacuum
chamber
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Precision Vacuum
Backplate
Optical path
PCB
Heated Transfer line
GC-IR/MS
Loading the sample disk
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Sample collection mechanism
DiscovIR VACUUM CHAMBER, (10-4 torr)
Resistive Heaters +/-5oC
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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Chromatogram Trace
Spectrum Trace
Spectrum Trace
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QA/QC / Performance Qualification
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Voltage check to ensure detector is working properly
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Noise check to ensure proper signal/noise ratio
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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)
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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
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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
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Amphetamine & Methamphetamine
Fingerprint Region
MDA & MDMA
Phentermine & Methamphetamine
Methamphetamine via Shake and Bake method:
Analysis of a field sample by GC-IR
Pseudoephedrine
Methamphetamine
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 3fluoromethcathinone
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?
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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
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