title: Performance characteristics of an ion chromatographic method for the quantitation of citrate and phosphate in pharmaceutical solutions.
abstract: The performance of an ion chromatographic method for measuring citrate and phosphate in pharmaceutical solutions is evaluated. Performance characteristics examined include accuracy, precision, specificity, response linearity, robustness, and the ability to meet system suitability criteria. In general, the method is found to be robust within reasonable deviations from its specified operating conditions. Analytical accuracy is typically 100 +/- 3%, and short-term precision is not more than 1.5% relative standard deviation. The instrument response is linear over a range of 50% to 150% of the standard preparation target concentrations (12 mg/L for phosphate and 20 mg/L for citrate), and the results obtained using a single-point standard versus a calibration curve are essentially equivalent. A small analytical bias is observed and ascribed to the relative purity of the differing salts, used as raw materials in tested finished products and as reference standards in the analytical method. The assay is specific in that no phosphate or citrate peaks are observed in a variety of method-related solutions and matrix blanks (with and without autoclaving). The assay with manual preparation of the eluents is sensitive to the composition of the eluent in the sense that the eluent must be effectively degassed and protected from CO(2) ingress during use. In order for the assay to perform effectively, extensive system equilibration and conditioning is required. However, a properly conditioned and equilibrated system can be used to test a number of samples via chromatographic runs that include many (> 50) injections.
authors.affiliation: Technology Resources Division, Baxter Healthcare Corporation, Route 120 and Wilson Road, Round Lake, IL 60073, USA. dennis_jenke@baxter.com
authors.forename: Dennis
authors.initials: D
authors.lastname: Jenke
authors.forename: Salma
authors.initials: S
authors.lastname: Sadain
authors.forename: Karen
authors.initials: K
authors.lastname: Nunez
authors.forename: Frances
authors.initials: F
authors.lastname: Byrne
mesh_terms: D002852:Chromatography, Ion Exchange / Q000379:methods*; D019343:Citric Acid / Q000032:analysis*; D004553:Electric Conductivity; D019999:Pharmaceutical Solutions / Q000737:chemistry*; D010710:Phosphates / Q000032:analysis*; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D012972:Sodium Hydroxide
chemical_list: D019999:Pharmaceutical Solutions; D010710:Phosphates; D019343:Citric Acid; D012972:Sodium Hydroxide