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119
Forensic
Applications
Sympathomimetic Amines in Urine, Blood, Plasma/Serum and
Tissue for GC or GC/MS Confirmations
Alternative Drying Procedure – Form TMS Derivative
Using 200mg 10mL HyperSep Verify-CX Extraction Column
(Part Number: 60108-742)
Prepare Sample
To 2mL of urine add internal standard(s)* and 1mL of
100mM phosphate buffer (pH 6.0)
Mix/vortex
Sample pH should be 6.0±0.5
Adjust pH accordingly with 100mM monobasic or dibasic
sodium phosphate
Condition Verify-CX Extraction Column
3mL of CH
3
OH then aspirate
3mL of DI H
2
O then aspirate
1mL of 100mM phosphate buffer (pH 6.0) then aspirate
NOTE:
Aspirate at <3"Hg to prevent sorbent drying
Apply Sample
Load sample at 1 to 2mL/minute
Wash Column
3mL of DI H
2
O
1mL of 100mM acetic acid
3mL of CH
3
OH
Dry column (5 minutes at >10"Hg)
Elute SMA
3mL of CH
2
Cl
2
/IPA/NH
4
OH (78:20:2)
Collect eluate at 1 to 2mL/min
NOTE:
Prepare elution solvent fresh daily; add IPA/NH
4
OH mix,
then add CH
2
Cl
2
(pH 11-12)
Concentrate Eluate
Add 30µL silylation grade DMF to eluate
Evaporate to 30µL at <40°C
Alternate Drying Procedure – Form TMS Derivative
Add 50µL BSTFA (with 1% TMCS)**** and
50µL of ethyl acetate
React for 45 minutes at 70°C
Quantitate
Inject 1 to 2µL onto gas chromatograph
For mass spectrometry, monitor the following ions:
Analyte (TMS)
Primary Ion** Secondary Tertiary
D
5
-amphetamine*
120
197
92
D
6
-amphetamine*
120
198
93
D
10
-amphetamine*
120
202
97
D
11
-amphetamine*
120
203
98
Amphetamine
116
192
91
D
5
-methamphetamine*
134
211
92
D
8
-methamphetamine*
137
214
92
D
9
-methamphetamine*
137
215
93
Methamphetamine
130
206
91
Pseudoephedrine
130
147
294
Ephedrine
130
147
294
Methylenedioxyamphetamine 116
236
135
Methylenedioxymethamphetamine 130
250
131
Para-Methoxamphetamine
116
222
121
* Suggested internal standards for GC/MS
** Quantitation ion
*** Part number TS-20672 (50mL vial)
**** Part number TS-38831 (10 x 1mL ampules)
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