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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