title: Three versus five micrometer chlorinated polysaccharide-based packings in chiral capillary electrochromatography: efficiency and precision evaluation.
abstract: In an earlier part of this study (performance evaluation) it was observed, for home-made capillary electrochromatography (CEC) columns, that smaller particle diameters do not always generate higher efficiencies. This phenomenon was further examined in this study, evaluating Van Deemter curves. Naphthalene and trans-stilbene oxide were analyzed on four 3 µm and four 5 µm chlorinated polysaccharide-based chiral stationary phases (CSPs) applying voltages ranging from 5 to 30 kV. Neither the 3 nor the 5 µm packings generated systematically the highest efficiencies. The varying column efficiencies were optimized by evaluating nine packing procedures for both 3 and 5 µm CSPs. Again it was observed that smaller particle-size packings were not necessarily beneficial for the efficiency of the CEC analysis. This observation was statistically evaluated. A variability study evaluated different precision estimates related to column packing and replicate measurement conditions. The best columns with the highest efficiencies (for chiral separations) and good precision, that is, the lowest RSD values, were generated by the packing procedure in which an MeOH-slurry and a water rinsing step of 8 h were applied.
authors.affiliation: Analytical Chemistry and Pharmaceutical Technology, Center for Pharmaceutical Research, Vrije Universiteit Brussel-VUB, Brussels, Belgium.
authors.forename: Ans
authors.initials: A
authors.lastname: Hendrickx
authors.forename: Katrijn De
authors.initials: KD
authors.lastname: Klerck
authors.forename: Debby
authors.initials: D
authors.lastname: Mangelings
authors.forename: Lies
authors.initials: L
authors.lastname: Clincke
authors.forename: Yvan Vander
authors.initials: YV
authors.lastname: Heyden
mesh_terms: D053801:Capillary Electrochromatography / Q000295:instrumentation* / Q000379:methods; D010316:Particle Size; D011134:Polysaccharides / Q000737:chemistry*; D013267:Stilbenes / Q000302:isolation & purification
chemical_list: D011134:Polysaccharides; D013267:Stilbenes; C025906:stilbene oxide
keywords: 3 vs 5μm packings; chiral electrochromatography; chlorinated polysaccharide-based selectors