MALDI-TOF MS stability study of model poly( p-phenylene terephthalamide)s

Gies, Anthony P.; Schotman, Anton; Hercules, David M.
February 2010
Analytical & Bioanalytical Chemistry;Feb2010, Vol. 396 Issue 4, p1481
Academic Journal
In the present study, we address the possibility of matrix-assisted laser desorption/ionization (MALDI)–time-of-flight MS analysis-induced chain fragmentation in poly( p-phenylene terephthalamide) (PPD-T) by considering two possible sources: (1) grinding-induced fragmentation resulting from the evaporation–grinding MALDI sample preparation method (E-G method) and (2) in-source/metastable fragmentation induced by the MALDI laser. An analysis of variance (ANOVA) statistical study found, with a high probability, that obtaining MALDI spectra with the effective laser area as large as possible (the “fanned-out” setting) did not cause any chain fragmentation due to the E-G MALDI sample preparation method, even when three additional grinding steps were used. However, the effect of laser fluence was less clear. A significant effect of laser fluence was observed for lower mass oligomers (<1,400 Da), but there was essentially no effect for higher mass species up to our limit of ANOVA measurement (∼2,300 Da). Plausible explanations are presented to explain these observations. The most likely scenario is that “unexpected” end-group modifications occur during PPD-T synthesis, producing small quantities of low mass species, which are amplified by the MALDI-EG extraction procedure. [Figure not available: see fulltext.]


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