660 likes | 989 Views
DiscovIR-GC ™. 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
E N D
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.
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
DiscovIR-GC Positional Isomers JWH-250 JWH-302 JWH-201
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-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 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)
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 PCB Interferometer ABB Bomem MCT Sample deposit ZnSe window Vacuum chamber Precision Vacuum Backplate Optical path
DiscovIR VACUUM CHAMBER, (10-4 torr) Sample collection mechanism Resistive Heaters +/-5oC Disc auto load/unload 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™
Chromatogram Trace Spectrum Trace Spectrum 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)
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
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 SpectrumDirect Deposition VS. Solid Phase Reference Comparable To Solid phase/condensed phase IR spectra run with: - ATR - KBR pellet - Nujol Mull
Bath salt sample Analysis
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