LC/MS Analysis of Methamphetamine Enantiomers on Astec® CHIROBIOTIC® V2 in Urine after SPE using Supel™-Select SCX
Materialien
Analytische Säule
SPE-Röhrchen oder -Platte
Standard
(±)-Methamphetamin -Lösung
1.0 mg/mL in methanol, ampule of 1 mL, certified reference material, Cerilliant®CONDITIONS
sample preparation
SPE (Solid Phase Microextraction)
sample/matrix
1 mL of synthetic urine spiked with 25 ng/mL
SPE well plate
Supel-Select SCX SPE 96-well Plate, 30 mg/well (575664-U)
extraction process
acidified to 3-4 pH with formic acid
condition
1 mL 1% formic acid in acetonitrile, then 1 mL water
sample
1.0 mL urine
washing
2 mL water, then 1 mL 25% methanol
elution
1 mL 10% ammonium hydroxide in acetonitrile
eluate post-treatment
evaporate to dryness under nitrogen at 40 °C, reconstitute in 1 mL mobile phase
column
Astec CHIROBIOTIC V2, 15 cm x 4.6 mm I.D., 5 μm particles (15023AST)
mobile phase
[A] methanol; [B] water; [C] acetic acid; [D] ammonium hydroxide; (95:5:0.1:0.02, A:B:C:D)
flow rate
1.0 mL/min
pressure
1221 psi (84 bar)
column temp.
20 °C
detector
MS, ESI(+),SIR m/z 150.1
injection
2 μL
Beschreibung
Sonstige Hinweise
sample pretreatment: acidified to 3-4 pH with formic acid
Rechtliche Hinweise
Astec is a registered trademark of Merck KGaA, Darmstadt, Germany
CHIROBIOTIC is a registered trademark of Sigma-Aldrich Co. LLC
Supel is a trademark of Sigma-Aldrich Co. LLC