115
Quetiapine in Urine, Blood, Plasma/Serum and Tissue
for LC/PDA 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 urine, blood, plasma/serum, or 1g (1:4) of
tissue homogenate
Add 2mL of 100mM phosphate buffer (pH 6.0)
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 phosphate buffer
3mL of 100mM acetic acid
3mL of CH
3
OH
Dry column (5 minutes at >10"Hg)
3mL of hexane
Dry column (5 minutes at >10"Hg)
Elute Quetiapine
3mL of ethyl acetate/acetonitrile/ammonia (78:20:2, v/v/v)
Collect eluate at 1 to 2mL/min
NOTE:
Prepare elution solvent fresh daily
Evaporate
Evaporate eluates gently under a stream of nitrogen
at <40°C
Reconstitute
Reconstitute sample in 100µL of 0.1% trifluoroacetic
acid (aq)
Analysis
Inject 50µL of sample onto LC/MS/MS system
Monitor the following ions:
Compound
Quetiapine
Quinidine*
* Suggested internal standard
Flow rate: 1mL/min
Column temperature: ambient
Mobile phase: acetonitrile:0.1% trifluoroacetic acid (25:75)
Detector: diode array (250nm)
Recommended HPLC Column
Part Number
Hypersil GOLD 3µm, 150 x 4.6mm
25003-154630
Forensic
Applications