N. Ostah

Electrospray Mass Spectrometry: An Alternative Method for the Identification of Organotin Compounds

The limitations of conventional gas chromatography-mass spectrometry (GC-MS) analyses for alkyl- and aryl-tin compounds are discussed, particularly the excessive fragmentation from electron impact (EI) ionization. Negative EI methods exhibit low ionization capabilities and are restricted to compounds with an electronegative centre, and are thus not suitable for general routine analysis. Liquid chromatography-MS (LC-MS) interfaces offer potential advantages in terms of reduced sample work-up since no derivatization is required. Electrospray techniques give reproducible mass spectra for each compound studied under fixed instrumental parameters. Changes in the cone/repeller voltages can radically alter the observed mass spectra. High-mass species were observed for each compound studied and tentative structures for these species are proposed.

Investigation of amine and polyol functionality in extracts of polyurethane wound management dressings using MALDI-MS

Polyurethane (PU) foams used in wound management are produced by a reaction between aromatic diisocyanates and polyether polyols. There is concern that residues of these starting materials, which may contain aromatic amine functionality, may leach from the finished polymer during in vivo applications. Furthermore, oligomers and additives may be leached from the PU system after the polymerization process is complete. Finished polymers have, therefore, been extracted with a range of solvents, such as water, diethyl ether and dilute HCl. The extracts were subjected to MALDI-MS (matrix-assisted laser desorption ionization mass spectrometry) analysis in an attempt to determine the amine and polyol functionality. Direct MALDI-MS analysis of the wound dressing extracts indicated the presence of components based on the polyols [corrected] used in the formulation of the foam. The spacing between the peaks identified the base monomer used in the polyol. MALDI-MS analysis of the fluorescamine derivatives of model amine compounds has demonstrated the anticipated increase in mass (278 for monoamines and 278 and 556 for diamines). Similar results were obtained from the derivatization of model polyols with phenyl isocyanate, where the mass shift (n x 119) was a direct measure of the number of active hydroxyl groups. Fluorescamine labelling of PU foams shows the colour change which could be [corrected] indicative of the presence of an amine, but the subsequent MALDI-MS analysis was unable to demonstrate the anticipated increase in mass.

The MS-MS Determination of the Fragmentation Pathways of Some Substituted 1,2,3-Benzotriazin-4-ones with Possible Applications in Metabolic Studies

1,2,3‐Benzotriazin‐4‐one derivatives are extensively used as herbicides, insecticides and nematicides. Incorporation of these compounds into the human food chain is a cause for concern, since their toxicity to man is well documented.