GC Analysis of Amphetamines in Urine on a 100% Methyl Column after SPME using 100 μm PDMS Fiber

sample/matrix

1 mL urine + 0.7g potassium carbonate in 20 mL headspace vial, equilibrated at 80°C, 30 min

SPME fiber

polydimethylsiloxane, 100 μm (57300-U)

derivatization

methyl bis-trifluoroacetamide (headspace, 0.5 min, ambient)

extraction

headspace, 3-5 min, 80 °C

desorption process

1 min, 270 °C

column

100% methyl polysiloxane, 12.5 m × 0.2 mm I.D., 0.33 μm (Supelco equivalent, Equity-1, 28041-U)

oven

60 °C (1 min) to 140 °C (4 min) at 30 °C/min, then to 276 °C at 20 °C/min, 4 min

inj. temp.

splitless (closed 1 min), 270 °C

detector

MS, full scan