121
Forensic
Applications
Tetrahydrocannabinol (THC) in Oral Fluid for GC/MS Confirmation
Using 200mg 10mL HyperSep Verify-CX Extraction Column
(Part Number: 60108-742)
Prepare Sample
To 1mL of oral fluid add 50ng/mL internal standard
(THCA D9-TMS) and let sit for 10 minutes at room
temperature
Vortex for 10 seconds
Add 0.5mL of glacial acetic acid and vortex for 10 seconds
Condition Verify-CX Extraction Column
3mL of CH
3
OH then aspirate
3mL of DI H
2
O then aspirate
1mL of 0.1N HCl then aspirate
Apply Sample
Load sample at 1mL/minute (do not exceed this flow rate)
Wash Column
2mL of DI H
2
O
2mL of 0.1N HCl/acetonitrile (70:30)
Dry column (5 minutes at >10"Hg)
200µL of hexane
Elute THC
2mL of hexane/ethyl acetate (50:50)
Collect eluate at 1mL/min (do not exceed this rate)
Dry Eluate
Evaporate to full dryness at <40°C under a stream
of nitrogen
Derivatize
Add 50µL of MSTFA***
Vortex for 10 seconds then heat for 20 minutes at 60°C
Vortex for 10 seconds while hot
Reconstitute in 50µL of ethyl acetate
Quantitate
Inject 2µL onto gas chromatograph
Monitor the following ions:
Compound
Primary Ion** Secondary
Tertiary
THCA-TMS
371
386
387
THCA D9-TMS*
380
479
* Suggested internal standard
** Quantitation ion
*** Part number TS-48910 (10 x 1mL ampule)
Recommended GC Columns
Part Number
TRACE TR-DoA5 Column, 15m x 0.25mm x 0.25µm
26AF130P
TRACE TR-DoA35 Column, 15m x 0.20mm x 0.33µm
26AC497P
Source
Janet Putnam, Assistant Laboratory Director/RP Advanced Toxicology Network, Memphis, TN
Tear Gas, Extraction of Chloroacetophenone (CS),
O-chlorobenzylidenemalononitrile (CN) and
Trans-8-methyl-N-vanillyl-6-nonenamide (OC) from Cloth for GC/MS
Using 200mg 10mL HyperSep Verify-CX Extraction Column
(Part Number: 60108-742)
Prepare Sample
If suspected tear gas is on clothing, cut out a portion of
the sprayed area and a negative control sample.
Extract each of these samples into hexane. For canisters
of suspected tear gas, spray onto a Kimwipe
®
or
equivalent product and extract the sprayed area and a
negative control into hexane.
Condition Verify-CX Extraction Column
3mL of CH
3
OH
3mL of DI H
2
O
1mL of 100mM phosphate buffer (pH 6.0)
NOTE:
Aspirate at <3"Hg to prevent sorbent drying
Apply Sample
Load sample at 1mL/minute
Wash Column
3mL of DI H
2
O
3mL of hexane
Dry column (5 minutes at >10"Hg)
Elute Analytes
1mL of CH
3
OH
Dry Eluate
Evaporate to full dryness at <40°C under a stream of
nitrogen
Reconstitute
Add 200µL of CH
3
OH
Mix/vortex then transfer to a GC/MS vial and cap
Quantitate
Inject 1 to 2µL onto gas chromatograph