1. DiscovIR-GC™

2. The Epidemic is coming (Tucson News KOLD/KMSB)

3. 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.

5. 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

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

7. CP47,497 Diastereomers and Homologs

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

9. JWH 302 vs JWH-201

11. Analysis of a K-2 Sky Sample 

12. Plant Extract/ Fatty Acids

13. Identification of JWH-203

14. 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 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

15. 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) 15 15

17. How does it work ?

18. GC-IR System optics
Sample streams onto cryogenic disk surface,where it freezes. Disk turns slowly, carries deposit into IR beam in 45 seconds. Continuous track of deposit on disk, IR spectrum every ½ second. All solvent removed, chromatograms generated from the IR spectra in real time.

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

20. Disc Track Pointer Infrared beam fixed in position ZnSE Disc rotates
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

21. Sample deposit ZnSe window
Cryogenic LN2
IR Detector
PCB
Interferometer
ABB Bomem
M C T
Sample deposit ZnSe window
Identify labeled elements
LN2 for cooling sample disk & Purge non vacuum optical path
Weighted cap to slightly pressurize N2 to drive purge
Electronics Board
7 Proportional Integral Temp Controllers & Many temperature sensors
2 Stepping motors for rotary and linear disk motion to create phonograph spiral
Roughing and Diffusion pump control
Communications
Vacuum gauging
onboard processor for control when PC is disconnected / buzy
IR Microscope Optics path
Interferometer
Collimated path through windows into vacuum chamber
Parabolic first surface aluminum mirrors
100 micron spot size
MCT Cryogenic Detector
Vacuum
chamber
Precision Vacuum Backplate
Optical path 21

22. Heated Transfer line

23. GC-IR/MS

24. Loading the sample disk

25. DiscovIR VACUUM CHAMBER, (10-4 torr)
Sample collection mechanism
DiscovIR VACUUM CHAMBER, (10-4 torr)
Resistive Heaters +/-5oC
Disc auto load/unload
Disk with temp control & automated ejection / loading
Sample deposition (show location)
Visual microscope of depostion tip
IR Microscope
Rotary coupling with Thermal conduction
Spindle heater
4 inch diameter ZnSe disc, washable & reusable Holds 50 hours of chromatography in spiral track Auto location, Checks for sample, Post dep. analysis 25

26. Data Acquisition and Instrument Control software based on Thermo GRAMS™

27. Spectrum Trace
Chromatogram Trace

28. 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)

29. Example of a Daily Test Mix Chromatogram

30. Typical Case Work 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

31. Amphetamine mixture Chromatogram     

32. Amphetamine & Methamphetamine
Fingerprint Region

33. MDA & MDMA

34. Phentermine & Methamphetamine

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

37. Diastereomers in Meth Synthesis
Ephedrine
Pseudoephedrine

38. Pseudoephedrine IR Spectrum Direct Deposition VS. Solid Phase Reference
Comparable To Solid phase/condensed phase IR spectra run with:
- ATR
- KBR pellet
- Nujol Mull

39. FTIR Specificity: Pseudoephedrine hit list  

41. Emerging Threat 2C-Phenethylamines

43. Bath salt sample Analysis         

44. 4-fluoromethcathinone overlaid with 3-fluoromethcathinone

45. Solid Phase Mid-IR Spectrum of Mephedrone

46. Solid Phase Mid-IR Spectrum of Lidocaine

47. Solid Phase Mid-IR Spectrum of MDPV

48. Presence of one Cannabinoids: JWH-018

49. Advantage of Solid Phase DD GC-IR

50. 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

51. JWH-073 and JWH-015 isomers MW 327.4

52. JWH-073 overlaid with JWH-015 isomer

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

54. Tryptamines

55. 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)

56. Exhibit containing BZP, TFMPP, MDMA and Caffeine

57. Clandestine Tablet: Containing BZP, TFMPP, MDMA and Caffeine

58. 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

59. 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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