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Forensic
Applications
Amphetamines, Opiates and Phencyclidine in Oral Fluid
for GC/MS Confirmations
Using 50mg 1mL HyperSep Verify-CX Extraction Column
(Part Number: 60108-741)
Prepare Sample
Add 100 to 500µL of neat sample to a clean test tube
Add internal standard(s) and let sit for 10 minutes at
room temperature
Add 800µL of 100mM phosphate buffer (pH 6.0)
Mix/vortex for 10 seconds
Sample pH should be 6.0±0.5
Adjust pH accordingly with 100mM monobasic or dibasic
sodium phosphate
Condition Verify-CX Extraction Column
200µL of CH
3
OH
200µL of DI H
2
O
200µL of 100mM phosphate buffer (pH 6.0)
Apply Sample
Load sample at 1mL/minute (do not exceed this
flow rate)
Wash Column
500µL of DI H
2
O
500µL of 100mM acetic acid
500µL of CH
3
OH
Dry column (5 minutes at >10"Hg)
Elute Compounds
800µL of CH
2
Cl
2
/IPA/NH
4
OH (70:26:4)
Collect eluate at 1mL/min (do not exceed this rate)
NOTE:
Prepare elution solvent fresh daily; add IPA/NH
4
OH mix,
then add CH
2
Cl
2
(pH 11-12)
Dry Eluate
For amphetamines and PCP, add 100µL of 5% trifluo-
roacetic acid in methanol after 5 minutes of drying
(5 minutes drying removes ammonia, addition of acid
ionizes volatile analytes preventing loss)
Evaporate to full dryness at <40°C under a stream
of nitrogen
Derivatize
For Amphetamines*:
Add 50µL PFPA (PFAA)** then vortex. Overlay with
nitrogen and cap. React for 20 minutes at 70°C.
Evaporate to dryness at <40°C. Reconstitute with
50µL ethyl acetate.
For Opiates*:
Add 200µL of a 1:1 solution of PFPA (PFAA)**
(10 x 1mL ampules, Cat. No. TS-65193)
Vortex then react for 60 minutes at 40°C
Reconstitute with 50µL ethyl acetate
Quantitate
Inject 2µL onto gas chromatograph
* Alternative derivatizations may be used
** Part number TS-65193 (10 x 1mL ampules)
NOTE:
Phencyclidine does not derivatize
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