Partial filling micellar electrokinetic chromatography optimization studies of ibuprofen, codeine and degradation products, and coupling to mass spectrometry

Abstract

Studies have been performed to evaluate whether an on-line partial filling-micellar electrokinetic chromatography (PF-MEKC) system could be applied to a recently developed MEKC method for the separation of ibuprofen, codeine and one of the degradation products. Attempts to couple the PF-MEKC system to MS have also been performed. SDS concentration, micellar zone length and concentration of acetonitrile in the buffer were optimized using factorial design. When a small micelle zone was injected directly after the sample introduction, the results improved markedly. The MS parameters have not been optimized, but the studies show promising results for the use of PF-MEKC-mass spectrometry for identification of the degradation products.

Capillary electrophoresis‐mass spectrometry: Recent advances to the analysis of small achiral and chiral solutes

“…The technique of PF-MEKC-MS using a SDS surfactant for separation and detection of ibuprofen, codeine, and degradation products has been described by Stubberud et al [81,82]. In the first publication, the authors used a factorial design to optimize the SDS concentration, micellar zone length, and concentration of ACN [81]. The concentration of SDS and acetonitrile was found to have a significant impact on resolution and peak symmetry of the compounds.…”

Atmospheric Pressure Photoionization for Enhanced Compatibility in On-Line Micellar Electrokinetic Chromatography−Mass Spectrometry

“…The high concentrations of nonvolatile salts and surfactants commonly used in MEKC can seriously suppress analyte ionization, cause intense background signals, and contaminate the ion source. To avoid these problems, for on-line MEKC−MS, most commonly so-called partial-filling techniques are used in which the pseudostationary surfactants are prevented from entering the ion source. − Unfortunately, these approaches often strongly reduce the separation performance and require specific optimization for each analyte. Other MEKC−MS methodologies include reverse-migrating micelles, , high-molecular-mass surfactants, − and volatile surfactants. , However, with these pseudostationary phases, the selectivity and resolution often are inferior to those obtained with conventional surfactants as sodium dodecyl sulfate (SDS).…”

A critical review on the use of modern sophisticated hyphenated tools in the characterization of impurities and degradation products

“…To overcome the difficulty, different approaches used are partial-filling MEKC [200,201], use of reverse-migrating micelles [202], volatile surfactants [203] and high molecular weight PSPs [204]. Accordingly, a partial-filling MEKC-MS method was deployed for the separation of ibuprofen, codeine and their IMPs [200,201]. Directly coupled MEKC-MS was also evaluated for impurity profiling of galantamine and ipratropium [205].…”