LC/MS Analysis of Illicit Phenethylamine and Cathinone"Bath Salts" in Plasma on Ascentis® Express HILIC after Extraction using SPME LC Tips

LC/MS Analysis of Illicit Phenethylamine and Cathinone

Conditions

sample/matrix Rat plasma was adjusted to pH 3.0 with phosphoric acid and spiked at 50 ng/mL with selected Bath Salt compounds. (A 750 µL aliquot of the spiked plasma was placed into each well of a 1.0 mL 96 well collection plate.)
desorption process Desorbed samples were evaporated and reconstituted in 40 µL of acetonitrile and injected directly into the LC/MS system.
desorption process SPME LC Tip fibers were then desorbed in 100 µL of 0.5% ammonium hydroxide in methanol for 60 minutes at 500 rpm vortex.
extraction SPME LC fibers were preconditioned in 50:50 methanol:water and placed into sample wells. Extraction was performed for 15 minutes on an IKA VORTEX MS3 shaker at 500 rpm.
SPME fiber SPME LC tip, mixed-mode (57234-U)
column Ascentis Express HILIC, 10 cm x 2.1 mm I.D., 2.7 µm particles (53939-U)
column temp. 35 °C
mobile phase 5 mM ammonium formate (98:2 acetonitrile:water)
flow rate 0.6 mL/min
pressure 1842 psi (127 bar)
injection 1 µL
detector ESI(+), 100-1000 m/z

Description

Analysis Note Solid phase microextraction (SPME) was used in this application to extract phenethylamine and cathinone "bath salts" from spiked plasma. After elution from the SPME fiber, the compounds were separated on an Ascentis Express HILIC column and detected using MS ESI(+) detection. Ultra high purity LC-MS solvents were used to supply low background interference and low particulate contaminants for robust, trouble-free operation. Cerilliant CRMs provided reliable identification and quantification.
Categories Analytical Chromatography, Drugs of Abuse
Featured Industry Forensics and Toxicology
Legal Information Ascentis is a registered trademark of Sigma-Aldrich Co. LLC
suitability application for LC-MS, application for SPME

Materials

     
Related Links