title: Evaluation of 1.5 microM reversed phase nonporous silica in packed capillary electrochromatography and application in pharmaceutical analysis.
abstract: Reversed-phase nonporous silica (RP-NPS) of 1.5 microm dp is employed to demonstrate rapid and efficient separations in packed capillary electrochromatography (CEC). Two methods for packing capillaries and two techniques to manufacture frits used to hold the packing in place are evaluated for their effect upon separation performance using polyaromatic hydrocarbons (PAHs) and polar neutral pharmaceutical compounds. Attention is given to conditioning of the packed capillaries for high efficiency separations without necessity for sodium dodecyl sulfate (SDS). Separation conditions for the nonporous materials were modified from those previously determined on porous reversed-phase silica. Feasibility for method development and validation of a parent pharmaceutical compound and related impurities in the range of 0.1-120% of a 5 mg/mL concentration was assessed and reported. An approach to improving detection sensitivity through use of large-bore capillaries is briefly discussed.
authors.affiliation: Department of Pharmaceutical Chemistry and the Center for Bioanalytical Research, University of Kansas, Lawrence 66047, USA.
authors.forename: P D
authors.initials: PD
authors.lastname: Angus
authors.forename: C W
authors.initials: CW
authors.lastname: Demarest
authors.forename: T
authors.initials: T
authors.lastname: Catalano
authors.forename: J F
authors.initials: JF
authors.lastname: Stobaugh
mesh_terms: D000873:Anthracenes / Q000302:isolation & purification; D001713:Biphenyl Compounds / Q000302:isolation & purification; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D019075:Electrophoresis, Capillary / Q000379:methods*; D005069:Evaluation Studies as Topic; D005240:Feasibility Studies; D005449:Fluorenes / Q000302:isolation & purification; D008280:Magnetics; D009281:Naphthalenes / Q000302:isolation & purification; D011312:Pressure; D012680:Sensitivity and Specificity; D012822:Silicon Dioxide; D013890:Thiourea / Q000302:isolation & purification
chemical_list: D000873:Anthracenes; D001713:Biphenyl Compounds; D005449:Fluorenes; D009281:Naphthalenes; D012822:Silicon Dioxide; D013890:Thiourea; C031721:naphthalene; C010574:biphenyl; C007738:fluoranthene; C041509:fluorene; C034020:anthracene