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Presentation on theme: "DiscovIR-GC™."— Presentation transcript:

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


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


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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