Analiza LC/MS (TOF) nielegalnych soli do kąpieli w moczu na urządzeniu 2445 Express HILIC po ekstrakcji do fazy stałej (SPE) przy użyciu 5225-Select SCX
Materiały
Standardowe
Butylone hydrochloride solution
1.0 mg/mL in methanol (as free base), ampule of 1 mL, certified reference material, Cerilliant®Buphedrone hydrochloride solution
1.0 mg/mL in methanol (as free base), ampule of 1 mL, certified reference material, Cerilliant®Etylon
1.0 mg/mL in methanol (as free base), ampule of 1 mL, certified reference material, Cerilliant®4-Fluoromethcathinone hydrochloride solution
1.0 mg/mL in methanol (as free base), ampule of 1 mL, certified reference material, Cerilliant®3-Fluoromethcathinone hydrochloride solution
1.0 mg/mL in methanol (as free base), ampule of 1 mL, certified reference material, Cerilliant®Mephedrone hydrochloride solution
1.0 mg/mL in methanol (as free base), ampule of 1 mL, certified reference material, Cerilliant®Methylone hydrochloride
1.0 mg/mL in methanol (as free base), ampule of 1 mL, certified reference material, Cerilliant®3,4-Methylenedioxypyrovalerone HCl (MDPV) solution
1.0 mg/mL in methanol (as free base), ampule of 1 mL, certified reference material, Cerilliant®Methedrone hydrochloride solution
1.0 mg/mL in methanol (as free base), ampule of 1 mL, certified reference material, Cerilliant®kolumna analityczna
probówka lub płytka SPE
składnik fazy ruchomej
CONDITIONS
sample/matrix
urine samples spiked at 100 ng/mL with each target analyte (To ensure full ionization of the analytes, spiked samples were treated with formic acid to a final concentration of 0.1% formic acid.)
SPE tube/cartridge
Supel-Select SCX, 30 mg/1 mL (54240-U)
condition
1 mL 1% formic acid acetonitrile then 1 mL water
sample addition
1 mL spiked water blank or urine
washing
1 mL water, 1 mL 1% formic acid acetonitrile, 1 mL water
elution
2 mL 10% ammonium hydroxide in acetonitrile
eluate post-treatment
thoroughly mix via vortex agitation, evaporate 1 mL aliquot to dryness, reconstitute in 100 μL water:methanol
column
Ascentis Express HILIC, 10 cm x 2.1 mm I.D., 2.7 μm particles (53939-U)
mobile phase
(A) 5 mM ammonium formate acetonitrile; (B) 5 mM ammonium formate water; (98:2, A:B); premixed
flow rate
0.6 mL/min
pressure
1842 psi (127 bar)
column temp.
35 °C
detector
MS, ESI(+), TIC, m/z 100-1000
injection
1 μL
sample
200 μg/L ea. in acetonitrile
Opis
Komentarz do analizy
Sole do kąpieli to psychoaktywne dopalacze z rodziny fenetyloamin i katynonów. Przedstawiono tutaj szybką, czułą analizę LC/TOF-MS dziewięciu soli do kąpieli wyekstrahowanych z ludzkiego moczu przy użyciu polimerowej SPE na Supel-Select SCX i rozdzielonych na kolumnie Ascentis Express HILIC. Brak zakłócających pików na chromatogramie świadczy o skuteczności oczyszczania próbki. Aby zapewnić niezawodną identyfikację i kwantyfikację MS, zastosowano CRM Cerilliant.
Informacje prawne
Ascentis is a registered trademark of Merck KGaA, Darmstadt, Germany
Supel is a trademark of Sigma-Aldrich Co. LLC