LC/MS (TOF) Analysis of Illicit Bath Salts in Urine on Ascentis® Express HILIC after Solid Phase Extraction (SPE) using Supel™-Select SCX
Materials
analytical column
SPE tube or plate
accessory
mobile phase component
standard
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
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.
Legal Information
Ascentis is a registered trademark of Merck KGaA, Darmstadt, Germany
Supel is a trademark of Sigma-Aldrich Co. LLC