LC/MS Analysis of Fluoroamphetamine Drugs of Abuse in Urine on Ascentis® Express HILIC after SPE using Supel™-Select SCX

Materials
related product
4-Fluoroamphetamine hydrochloride solution
1.0 mg/mL in methanol (as free base), ampule of 1 mL, certified reference material, Cerilliant®(±)-2-Fluoroamphetamine hydrochloride solution
1.0 mg/mL in methanol (as free base), ampule of 1 mL, certified reference material, Cerilliant®CONDITIONS
sample preparation
SPE (Solid Phase Extraction)
sample/matrix
urine, 1 mL
SPE tube/cartridge
Supel-Select SCX SPE 96-well Plate, 30 mg/well (575664-U)
condition
1 mL methanol, then 1 mL 0.1% formic acid in water
washing
2 x 1 mL 10% methanol in water, 2 x 1 mL 1% formic acid in methanol
elution
2 mL 5% ammonium hydroxide in acetonitrile
eluate post-treatment
evaporate to 500 μL with nitrogen at room temperature, reconstitute in 250 μL acetonitrile
column
Ascentis Express HILIC, 10 cm x 2.1 mm I.D., 2.7 μm particles (53939-U)
mobile phase
5 mM ammonium formate in acetonitrile:water (90:10, v/v)
flow rate
0.4 mL/min
pressure
1570 psi (108 bar)
column temp.
35 °C
detector
TOF/MS
injection
2 μL
Description
Analysis Note
The fluoroamphetamines (FA) are a group of "designer" stimulant drugs in the amphetamine family. Four members of the FA family are shown here isolated from urine using Supel-Select SCX SPE and separated in under 3 minutes on an Ascentis Express HILIC column. Cerilliant CRMs were used to ensure reliable MS identification and quantification.
Legal Information
Ascentis is a registered trademark of Merck KGaA, Darmstadt, Germany, Supel is a trademark of Sigma-Aldrich Co. LLC