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Paroxetine in Urine, Blood and Plasma/Serum
for LC/MS/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 standards*
Add 1mL of urine, blood or plasma/serum
Add 2mL of 100mM phosphate buffer (pH 6.0)
Vortex and centrifuge as appropriate
Condition Verify-CX Extraction Column
3mL of CH
3
OH then aspirate
3mL of DI H
2
O then aspirate
3mL 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 Paroxetine
3mL of ethyl acetate/acetonitrile/ammonium hydroxide
(78:20:2, v/v/v)
Collect eluate at 1 to 2mL/minute
Evaporate
Evaporate to dryness at <40°C
Reconstitute
100µL of CH
3
OH
Analysis
Inject 5µL of sample onto LC/MS/MS system
Monitor the following ions:
Compound
MRM Transition
Paroxetine
330.0/190.1
Paroxetine-D6*
336.0/76.1
* Suggested internal standard
Mobile phase:
Time (min)
% Acetonitrile
% 0.1% Formic Acid
0
10
90
15
50
50
16
10
90
20
10
90
Flow rate: 0.35mL/min
Column temperature: ambient
Recommended HPLC Column
Part Number
Hypersil GOLD Phenyl 3µm, 150 x 2.1mm
25903-152130
110
Forensic
Applications
Phencyclidine in Urine
Using 30mg 3mL HyperSep Retain-CX Extraction Column
(Part Number: 60107-302)
Sample Preparation
1mL of urine
Add internal standard* and 1mL 100mM phosphate
buffer (pH 6.0)
Mix/vortex
Condition HyperSep Retain-CX Extraction Column
Load at a rate of 1 to 2mL/min
Wash Column
1 x 1mL DI H
2
O
1 x 1mL 100mM acetic acid
1 x 1mL CH
3
OH
Dry column (3 mins at >10"Hg)
Elute
2 x 0.5mL CH
2
Cl
2
/IPA/NH
4
OH (78/20/2)
Collect eluate at 1 to 2mL/min
Add 1 drop 1% HCl in CH
3
OH to eluate before evaporating
Evaporate to dryness at <40°C
Reconstitute with 100µL ethyl acetate
Analysis
Inject 1 to 2µL onto GC/MS
For mass spectrometry monitor the following ions:
Compound
Target (Quantitation) Ion
Qualifier Ions
Phencyclidine
200
91, 242
Phencyclidine-D5*
205
96, 247
* Suggested internal standard: Phencyclidine-D5
Recommended GC Column
Part Number
TraceGOLD TG-5SilMS 30m x 0.25m x 0.25µm
26096-1420