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112
Propoxyphene in Urine, Blood, Plasma/Serum and Tissue
for GC or GC/MS Confirmations
Using 200mg 10mL HyperSep Verify-CX Extraction Column
(Part Number: 60108-742)
Prepare Sample
To 1mL of 100mM phosphate buffer (pH 6.0) add
internal standard*
Add 1mL of blood, plasma/serum, 2mL of urine or 1g
(1:4) of tissue homogenate
Mix/vortex
Sample pH should be 6.0±0.5
Adjust pH accordingly with 100mM monobasic or dibasic
sodium phosphate
Centrifuge as appropriate
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)
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
3mL of 100mM acetic acid
3mL of CH
3
OH
Dry column (5 minutes at >10"Hg)
Elute Propoxyphene
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
Evaporate to dryness at <40°C
Reconstitute with 100µL ethyl acetate
Quantitate
Inject 1 to 2µL onto gas chromatograph
For mass spectrometry, monitor the following ions:
Compound
Primary Ion** Secondary
Tertiary Other
D
5
-propoxyphene*
63
120
213 255,270
Propoxyphene
58
115
208 250,265
* Suggested internal standard
** Quantitation ion
NOTE: To improve the analysis for Norpropoxyphene, the primary metabolite of
Dextropropoxyphene, add 1 drop of 35% sodium hydroxide solution to the urine sample
and, then after mixing, bring the pH to 6 for SPE extraction (this step converts the
Norpropoxyphene to Norpropoxyphene amide, a more stable compound)
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
Forensic
Applications