The Epidemic is coming (Tucson News KOLD/KMSB)
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2 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. 3 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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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 5
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
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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 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 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 napthyl isomer AM napthyl isomer JWH-018 adamantyl JWH napthyl isomer JWH-250 JWH-098 RCS-4 C4 homolog AM-694 JWH-201 JWH-210 JWH-203 AM iodo isomer JWH-302
15 DiscovIR-GC The Solution for Designer Drugs Step #1 Separation by Gas Chromatography GC typical Step #2 Controlled Deposition - unique solid phase deposition. Step #3 Chemical Identification - using FTIR specificity (positional and stereoisomers)
16
17 How does it work?
18 GC-IR System optics 18
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 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 Cryogenic LN2 IR Detector Interferometer PCB Sample deposit ZnSe window M C T ABB Bomem Vacuum chamber 21 Precision Vacuum Backplate Optical path
22 Heated Transfer line
23 GC-IR/MS
24 24 Loading the sample disk
25 Sample collection mechanism DiscovIR VACUUM CHAMBER, (10-4 torr) Resistive Heaters +/-5 o C Disc auto load/unload 25 4 inch diameter ZnSe disc, washable & reusable Holds 50 hours of chromatography in spiral track Auto location, Checks for sample, Post dep. analysis
26 Data Acquisition and Instrument Control software based on Thermo GRAMS 26
27 Chromatogram Trace Spectrum Trace Spectrum Trace 27
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 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
35
36 Methamphetamine via Shake and Bake method: Analysis of a field sample by GC-IR Methamphetamine Pseudoephedrine 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
40
41 Emerging Threat 2C-Phenethylamines
42
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 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)
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
60
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