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

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)
column temp. 35 C
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)
sample 200 µg/L ea. in acetonitrile
injection 1 µl
detector MS, ESI(+), TIC, m/z 100-1000

Description

Analysis Note 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.
Categories Analytical Chromatography, SPE Applications, Clinical, Forensics and Toxicology, Drugs of abuse, drugs of abuse, Drugs of Abuse
Featured Industry Forensics and Toxicology
Legal Information Ascentis is a registered trademark of Sigma-Aldrich Co. LLC, Supel is a trademark of Sigma-Aldrich Co. LLC
suitability application for HPLC

Materials

     
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