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LC/MS (TOF) Analysis of Illicit Bath Salts in Urine on Ascentis® Express HILIC after Solid Phase Extraction (SPE) using Supel-Select SCX

LC/MS (TOF) Analysis of Illicit Bath Salts in Urine on Ascentis® Express HILIC after Solid Phase Extraction (SPE) using Supel™-Select SCX application for HPLC

Materiali

Accessorio

N° Catalogo
Descrizione
Determinazione del prezzo

Collettore del vuoto Visiprep SPE

DL (Disposable Liner), 12-port model

Collettore del vuoto Visiprep SPE

DL (Disposable Liner), 24-port model

Colonna analitica

N° Catalogo
Descrizione
Determinazione del prezzo

Ascentis® Express HILIC HPLC Column

2.7 μm particle size, L × I.D. 10 cm × 2.1 mm

Colonnina o piastra per SPE

N° Catalogo
Descrizione
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Supel-Select SCX SPE Tube

bed wt. 30 mg, volume 1 mL, pk of 100

Componente della fase mobile

N° Catalogo
Descrizione
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Formato di ammonio

eluent additive for LC-MS, LiChropur, ≥99.0%

Standard

N° Catalogo
Descrizione
Determinazione del prezzo

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®

Ethylone hydrochloride

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®

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

Descrizione

Risultati analitici

Bath salts are psychoactive designer drugs of the phenethylamine and cathinone families. Shown here is the rapid, sensitive LC/TOF-MS analysis of nine bath salts extracted from human urine using polymeric SPE on Supel-Select SCX and separated on an Ascentis Express HILIC column. Notice the lack of interfering peaks in the chromatogram demonstrating the effectiveness of the sample cleanup. Cerilliant CRMs were used to ensure reliable MS identification and quantification.

Note legali

Ascentis is a registered trademark of Merck KGaA, Darmstadt, Germany
Supel is a trademark of Sigma-Aldrich Co. LLC