Analiza LC/MS nielegalnej fenetyloaminy i katynonu "soli do kąpieli" w osoczu w Ascentis® Express HILIC po ekstrakcji za pomocą końcówek SPME LC
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®Methedrone hydrochloride solution
1.0 mg/mL in methanol (as free base), ampule of 1 mL, certified reference material, Cerilliant®kolumna analityczna
składnik fazy ruchomej
wyposażenie dodatkowe
CONDITIONS
sample/matrix
Rat plasma was adjusted to pH 3.0 with phosphoric acid and spiked at 50 ng/mL with selected Bath Salt compounds. (A 750 μL aliquot of the spiked plasma was placed into each well of a 1.0 mL 96 well collection plate.)
SPME fiber
SPME LC tip, mixed-mode (57234-U)
extraction
SPME LC fibers were preconditioned in 50:50 methanol:water and placed into sample wells. Extraction was performed for 15 minutes on an IKA VORTEX MS3 shaker at 500 rpm.
desorption process
SPME LC Tip fibers were then desorbed in 100 μL of 0.5% ammonium hydroxide in methanol for 60 minutes at 500 rpm vortex.
desorption process
Desorbed samples were evaporated and reconstituted in 40 μL of acetonitrile and injected directly into the LC/MS system.
column
Ascentis Express HILIC, 10 cm x 2.1 mm I.D., 2.7 μm particles (53939-U)
mobile phase
5 mM ammonium formate (98:2 acetonitrile:water)
flow rate
0.6 mL/min
pressure
1842 psi (127 bar)
column temp.
35 °C
detector
ESI(+), 100-1000 m/z
injection
1 μL
Opis
Komentarz do analizy
Mikroekstrakcja do fazy stałej (SPME) została wykorzystana w tym zastosowaniu do ekstrakcji "soli kąpielowych" fenetyloaminy i katynonu ze wzbogaconego osocza. Po elucji z włókna SPME, związki zostały rozdzielone na kolumnie Ascentis Express HILIC i wykryte przy użyciu detekcji MS ESI(+). Rozpuszczalniki LC-MS o bardzo wysokiej czystości zostały użyte w celu zapewnienia niskich zakłóceń tła i niskiej zawartości cząstek stałych w celu zapewnienia niezawodnej i bezawaryjnej pracy. CRM Cerilliant zapewniły niezawodną identyfikację i kwantyfikację.
Informacje prawne
Ascentis is a registered trademark of Merck KGaA, Darmstadt, Germany