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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

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technique(s)

HPLC: suitable

test parameters

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

suitability

application for HPLC

application(s)

forensics and toxicology

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

Analyte

Description
    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®
    See All (9)

SPE tube or plate

Product No.
Description
Pricing

accessory

Product No.
Description
Pricing

analytical column

Product No.
Description
Pricing

mobile phase component

Product No.
Description
Pricing

standard

Product No.
Description
Pricing

B-045

Butylone hydrochloride solution, 1.0 mg/mL in methanol (as free base), ampule of 1 mL, certified reference material, Cerilliant®

B-047

Buphedrone hydrochloride solution, 1.0 mg/mL in methanol (as free base), ampule of 1 mL, certified reference material, Cerilliant®

E-071

Ethylone hydrochloride, 1.0 mg/mL in methanol (as free base), ampule of 1 mL, certified reference material, Cerilliant®

F-015

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

F-016

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

M-138

Mephedrone hydrochloride solution, 1.0 mg/mL in methanol (as free base), ampule of 1 mL, certified reference material, Cerilliant®

M-140

Methylone hydrochloride, 1.0 mg/mL in methanol (as free base), ampule of 1 mL, certified reference material, Cerilliant®

M-146

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

M-147

Methedrone hydrochloride solution, 1.0 mg/mL in methanol (as free base), ampule of 1 mL, certified reference material, Cerilliant®

Certificates of Analysis (COA)

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