G005796

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

Propriétés

• Technique(s): HPLC: suitable
• Paramètres du test: 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
• Adéquation: application for HPLC
• Application(s): forensics and toxicology

Description

Remarque sur l'analyse

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.

Informations légales

Ascentis is a registered trademark of Merck KGaA, Darmstadt, Germany

Supel is a trademark of Sigma-Aldrich Co. LLC

Analyte

3,4-Methylenedioxypyrovalerone HCl (MDPV) 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^®
3-Fluoromethcathinone hydrochloride solution, 1.0 mg/mL in methanol (as free base), ampule of 1 mL, certified reference material, Cerilliant^®
Butylone 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^®
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^®
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