title: Evaluation of a hydrophilic interaction liquid chromatography design space for sugars and sugar alcohols.
abstract: Based on a column-screening exercise, a column ranking system was developed for sample mixtures containing any combination of 26 sugar and sugar alcohol analytes using 16 polar stationary phases in the HILIC mode with acetonitrile/water or acetone/water mobile phases. Each analyte was evaluated on the HILIC columns with gradient elution and the subsequent chromatography data was compiled into a statistical software package where any subset of the analytes can be selected and the columns are then ranked by the greatest separation. Since these analytes lack chromophores, aerosol-based detectors, including an evaporative light scattering detector (ELSD) and a charged aerosol detector (CAD) were employed for qualitative and quantitative detection. Example qualitative applications are provided to illustrate the practicality and efficiency of this HILIC column ranking. Furthermore, the design-space approach was used as a starting point for a quantitative method for the trace analysis of glucose in trehalose samples in a complex matrix. Knowledge gained from evaluating the design-space led to rapid development of a capable method as demonstrated through validation of the following parameters: specificity, accuracy, precision, linearity, limit of quantitation, limit of detection, and range.
authors.affiliation: Small Molecule Design and Development, Lilly Research Laboratories, Eli Lilly and Company, Indianapolis, IN, 46285, USA. Electronic address: hetrickem@lilly.com.
authors.forename: Evan M
authors.initials: EM
authors.lastname: Hetrick
authors.affiliation: Discovery and Development Statistics, Lilly Research Laboratories, Eli Lilly and Company, Indianapolis, IN, 46285, USA.
authors.forename: Timothy T
authors.initials: TT
authors.lastname: Kramer
authors.affiliation: Small Molecule Design and Development, Lilly Research Laboratories, Eli Lilly and Company, Indianapolis, IN, 46285, USA.
authors.forename: Donald S
authors.initials: DS
authors.lastname: Risley
mesh_terms: D000465:Algorithms; D002241:Carbohydrates / Q000032:analysis* / Q000302:isolation & purification; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D057927:Hydrophobic and Hydrophilic Interactions; D012997:Solvents / Q000737:chemistry; D013402:Sugar Alcohols / Q000032:analysis* / Q000302:isolation & purification
chemical_list: D002241:Carbohydrates; D012997:Solvents; D013402:Sugar Alcohols
keywords: CAD; Carbohydrate; ELSD; HILIC; Sugar; Sugar alcohols