Accuracy improvement in the determination of palladium in pharmaceuticals by eliminating volatility error when using ICP-MS coupled with direct introduction of sample dissolved in organic solvents

Abstract

A procedure is described for the determination of analytical error caused by volatility of palladium compounds during the analysis of trace levels of palladium in pharmaceutical compounds. It is shown that an analytical error of up to 100% in magnitude is caused by volatility of palladium compounds when the sample, dissolved in organic solvent, is directly nebulized in the spray chamber of the ICP-MS instrument. The proposed procedure is based on the use of thioacetamide to convert the volatile palladium compounds to a non-volatile palladium–thioacetamide complex. It is shown that this procedure ensures complete elimination of volatility error regardless of the chemical nature of volatile palladium compound.