Simultaneous Determination of Dysprosium and Iron in Urine by Capillary Zone Electrophoresis Coupled to Cloud Point Extraction

C. ORTEGA, S. CERUTTI, R.A. OLSINA, L.D. MARTINEZ, M.F. SILVA

JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS

Elsevier

Año: 2004 vol. 36 p. 721 - 727

0731-7085

Automated preconcentration strategies are needed when analyzing metals in real samples by capillary electrophoresis (CE) with UV detection. The on-line incorporation of cloud point extraction (CPE) to flow injection analysis (FIA) associated with CE for simultaneouslydetermining dysprosium and iron at ppb levels in urine is presented and evaluated for the first time. The preconcentration step is mediated by micelles of the non-ionic surfactant polyethyleneglycol-mono-p-nonylphenylether (PONPE 7.5) with 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol. The micellar system containing the complex was loaded into the FIA manifold at a flow rate of 8ml min−1, and the surfactant rich-phase was retained in a microcolumn packed with cotton, at pH 9.2. The surfactant-rich phase was eluted with 50 ul acetonitrile directly into the CE sample vial, allowing to reach an enrichment factor of 200-fold for a 10ml sample urine. The type and composition of the background electrolytes (BGE) were investigated with respect to separation selectivity, reproducibility and stability. A BGE of 20mMsodium tetraborate buffer containing 13% acetonitrile, pH 9.0 was found to be optimal for the separation of metal chelates. Detection was performed at 585 nm. An enhancement factor of 200 was obtained for the preconcentration of 10 ml of sample solution. The detection limitsfor the preconcentration of 10 ml of urine were 0.20 ug l−1 for Dy, and. 0.48 ug l−1 for Fe. The calibration graphs using the preconcentration system were linear with a correlation coefficient of 0.9989 (Dy) and 0.9976 (Fe) at levels near the detection limits up to at least 500 ug l−1. Themethod was successfully applied to the determination of dysprosium and iron in urine for monitoring the elimination of dysprosium-based pharmaceuticals