The utility of silica hydride-based stationary phases for dual-mode ultra high performance liquid chromatography separation of synthetic cathinone positional isomers

J Sep Sci. 2020 Sep;43(17):3449-3457. doi: 10.1002/jssc.202000599. Epub 2020 Jul 28.

Abstract

Emerging drugs usually mimic the effects of traditional drugs, but are not always controlled due to the chemically altered structures. Positional isomers of emerging drugs are difficult to analyze because they challenge the separation and detection techniques commonly employed by forensic laboratories. The utility of silica hydride stationary phases for the ultra-high performance liquid chromatography separation of synthetic cathinone positional isomers was studied in this manuscript. SiH phases are operable under both reversed phase and aqueous normal phase chromatographic conditions without the need to change solvent reservoirs. The separation of eight positional isomers of the synthetic cathinone, pentedrone, was investigated using five silica hydride phases, and compared to a classical dual column reversed phase, hydrophilic interaction chromatography system, and to a bimodal pentaflurophenyl column. Significant selectivity differences were observed using either a combination of a classical reversed phase C18 and NP Silica columns or the various bimodal columns. The silica hydride silica-C column, which contains no derivatized ligands attached to the silica hydride backbone, not only gave the most orthogonal separation of the bimodal columns, but provided a unique separation of all eight positional isomers (resolution ≥ 1) using the combination of reverse phase and aqueous normal phase chromatographic conditions.

Keywords: bimodal separations; emerging drugs; positional isomers; silica hydride stationary phases.

MeSH terms

  • Alkaloids / chemistry
  • Alkaloids / isolation & purification*
  • Chromatography, High Pressure Liquid
  • Hydrophobic and Hydrophilic Interactions
  • Molecular Structure
  • Psychotropic Drugs / chemistry
  • Psychotropic Drugs / isolation & purification*
  • Silicates / chemistry*
  • Stereoisomerism

Substances

  • Alkaloids
  • Psychotropic Drugs
  • Silicates
  • silica hydride
  • cathinone