Article ID | Journal | Published Year | Pages | File Type |
---|---|---|---|---|
1192134 | International Journal of Mass Spectrometry | 2014 | 5 Pages |
•A convenient detection method for trace palladium by DART-MS was developed and the distinct palladium isotopic pattern was used for palladium detection.•Fast detection of 18 s per sample was achieved which makes the method possible for high throughput analysis.•Limit of detection at 120 ppb was achieved with a chelating agent 4-methyl-piperazine-1-carbodithioate.•Good intensity was obtained with both volatile (methanol or acetonitrile) and nonvolatile solvents (DMSO or DMF).•Semi-quantitation of palladium content was achieved for samples from compound collections in early drug discovery.
A detection method for palladium by direct analysis in real time (DART-MS) was developed. The method was used for the detection and semi-quantification of palladium in compound samples for which palladium was used during synthesis from compound collections in early drug discovery. The samples containing palladium were mixed with the chelating agent 4-methyl-piperazine-1-carbodithioate and a palladium chelating complex was subsequently formed and detected by DART-MS. The distinct isotopic pattern of palladium was observed and used for its qualitative identification. Semi-quantification was performed based on the peak areas of the extracted ion currents for the four most abundant isotope peaks at m/z 456, 457, 459 and 461. The limit of detection for this method was observed to be 1.2 μM (120 ppb). With DART ionization, rapid analysis of 18 s per sample was achieved with low carryover. Different solvents and chelating agents were also tested for this analysis, and satisfactory signal intensity was obtained using both volatile and nonvolatile solvents.
Graphical abstractFigure optionsDownload full-size imageDownload high-quality image (87 K)Download as PowerPoint slide