title: Determination of pharmaceutically related compounds by suppressed ion chromatography: I. Effects of organic solvent on suppressor performance.
abstract: This overall study aims to investigate gradient elution ion-exchange chromatography of pharmaceutically relevant compounds using universal nebulisation detectors, such as evaporative light scattering detection (ELSD). Addition of organic solvents to the eluent is necessary to minimise hydrophobic adsorption on the polymeric stationary phase and improve solubility of analytes. It is also necessary to de-salt the eluent prior to detection, and in this work, ion chromatography suppressors were used for this step. Such suppressors have been designed for aqueous eluents, so the purpose of the present study was to investigate the effects of methanol and acetonitrile on suppressor performance. Chemical and electrolytic suppressors were evaluated for baseline drift, noise and efficiency of suppression using aqueous/organic eluents containing up to 40% (v/v) methanol or acetonitrile. Chemical suppression of aqueous/organic eluents showed minimal noise levels, uniform low baseline and low gradient drift. Electrolytic suppression gave good performance, but with higher baseline conductivity levels and baseline drift than chemical suppression. The elevated baseline was found not to be caused by incomplete suppression of the eluent, but was attributed to chemical reactions involving the organic solvents and facilitated by high electric currents and heat generation. It was demonstrated that suppressed ion-exchange separation using a complex KOH elution profile could be coupled with ELSD, with the suppressor effectively de-salting the eluent, producing a stable baseline. Finally, complementary separation selectivity was demonstrated using a set of pharmaceutically related organic acids separated by reversed-phase and ion-exchange methods.
authors: Pfizer Analytical Research Centre, Australian Centre for Research On Separation Science, School of Chemistry, University of Tasmania, Hobart, Australia.
authors: Naama
authors: N
authors: Karu
authors: Greg W
authors: GW
authors: Dicinoski
authors: Melissa
authors: M
authors: Hanna-Brown
authors: Paul R
authors: PR
authors: Haddad
mesh_terms: D000097:Acetonitriles; D002852:Chromatography, Ion Exchange / Q000295:instrumentation / Q000379:methods*; D056148:Chromatography, Reverse-Phase; D004867:Equipment Design; D006878:Hydroxides; D008027:Light; D016014:Linear Models; D000432:Methanol; D009930:Organic Chemicals / Q000737:chemistry*; D004364:Pharmaceutical Preparations / Q000032:analysis / Q000737:chemistry*; D017680:Potassium Compounds; D012542:Scattering, Radiation; D012997:Solvents / Q000737:chemistry
chemical_list: D000097:Acetonitriles; D006878:Hydroxides; D009930:Organic Chemicals; D004364:Pharmaceutical Preparations; D017680:Potassium Compounds; D012997:Solvents; C029943:potassium hydroxide; D000432:Methanol; C032159:acetonitrile