title: Direct analysis of palladium in active pharmaceutical ingredients by anodic stripping voltammetry.
abstract: Anodic stripping voltammetry, a classical electroanalytical method has been optimized to analyze trace Pd(II) in active pharmaceutical ingredient matrices. The electroanalytical approach with an unmodified glassy carbon electrode was performed in both aqueous and 95% DMSO/5% water (95/5 DMSO/H2O) solutions, without pretreatment such as acid digestion or dry ashing to remove the organics. Limits of detection (LODs) in the presence of caffeine and ketoprofen were determined to be 11 and 9.6 μg g(-1), with a relative standard deviation (RSD) of 5.7% and 2.3%, respectively. This method is simple, highly reproducible, sensitive, and robust. The instrumentation has the potential to be portable and the obviation of sample pretreatment makes it an ideal approach for determining lost catalytic metals in pharmaceutical-related industries. Furthermore, the simultaneous detection of Pd(II) with Cd(II) and Pb(II) in the low μg L(-1) range indicates that this system is capable of simultaneous multi-analyte analysis in a variety of matrices.
authors.affiliation: Department of Chemistry, University of Tennessee, Knoxville, TN 37996, USA.
authors.forename: Samuel M
authors.initials: SM
authors.lastname: Rosolina
authors.affiliation: Department of Chemistry, University of Tennessee, Knoxville, TN 37996, USA.
authors.forename: James Q
authors.initials: JQ
authors.lastname: Chambers
authors.affiliation: Department of Chemistry, University of Tennessee, Knoxville, TN 37996, USA. Electronic address: xue@utk.edu.
authors.forename: Zi-Ling
authors.initials: ZL
authors.lastname: Xue
mesh_terms: D055664:Electrochemical Techniques / Q000379:methods*; D004566:Electrodes; D010165:Palladium / Q000032:analysis*; D004364:Pharmaceutical Preparations / Q000737:chemistry*
chemical_list: D004364:Pharmaceutical Preparations; D010165:Palladium
keywords: Active pharmaceutical ingredients; Anodic stripping voltammetry; Palladium; Unmodified glassy carbon electrode