Benzodiazepines(with extra internal standards) by MSD on a ZB-Drug1

GC Conditions

Column

Zebron ZB-Drug-1, GC Cap. Column 10 m x 0.18 mm x 0.18 µm, Ea

Part No

7CD-G023-08

Phase Name

ZB-Drug-1

Injection

Split 10:1 @ 260°C

Carrier Gas

Constant Flow Helium, 0.7 mL/min

Detection

Mass Selective (MSD) @ (320°C)

Detection Info

Sample Notes

Analytes are 4µg/mL derivatized with MTBSTFA Sim ions: (Quant ion*) D5-Nordiazepam (*332,334): Nordiazepam (*327,328,383): D5-Oxazepam (*462,519): Oxazepam (*457,513,459): D5-Temazepam (*362,288,390): Temazepam (*357,359,385): Lorazepam-d4 (*495,517) Lorazepam (*491,513,493): Clonazepam-d4 (*376,330): Clonazepam (*372,374,326):Diazepam-d5 (*261,287): Diazepam (*256,283,221): Alprazolam-d5 (*284,313): Alprazolam (*279,308,204): D5-a-Hydroxyalprazolam (*386,388): a-Hydroxyalprazolam (*381,383,384)

Sample Preparation Details

Condition 1

3 mL Methanol at 1 mL/min

Condition 2

3 mL Water at 1 mL/min

Condition 3

1 mL 100mM phosphate buffer (pH 6.0) at 1 mL/min

Load

Load 2.00 mL Sample diluted in Urine

Wash 1

2 mL Water at 1 mL/min

Wash 2

2 mL 20% acetonitrile in 100mM phosphate buffer (pH 6.0) at 1 mL/min

Dry

Dry column(5 minutes at > 10 in Hg) add 2mL of hexane and aspirate

Elution 1

5 mL Ethyl acetate at 1 mL/min

Evaporation

Evaporate to dryness

Reconstitute

50 µL Pyridine/MTBSTFA