A new LC/MS method has been developed for the simultaneous measurement, in water and wastewater samples, of all species contained in commercial samples of linear type of alcohol ethoxylate (AE) surfactants including fatty alcohols. The method requires derivatization of the terminal hydroxyl of each surfactant species with 2-fluoro-N-methylpyridinium p-toluenesulfonate, which imparts a permanent cationic charge, allowing all species including the fatty alcohols and those with only one ethoxylate to be effectively detected by electrospray MS. Detection limits of typically <10 ppt for each individual species were attained in treated wastewater, in which total AE concentrations (combination of up to 114 individual species) are not expected to exceed 10 ppb. The method was validated for clean water as well as sewage influent and effluent samples.
A method originally developed for the extraction of biomolecules from agarose gel slices has been utilized as a rapid means of isolating biological compounds from gels for subsequent structural characterization by matrix-assisted last desorption-ionization Fourier transform mass spectrometry (MALDI/FTMS). This "freeze-squeeze" extraction method involves pressure extrusion of fluid from frozen gel slices and provides near 50% recovery of analyte in less than 5 min. Experiments were directed at examining the recovery efficiency of the extraction method using 14C-labeled adenosine monophosphate and investigating the effect of high buffer concentrations on the laser desorption mass spectra. When coupled with this extraction technique, MALDI/FTMS can be used to detect and identify biomolecules at the low picomole level in agarose gel slices. The accurate mass measurements and MS/MS capabilities of the FTMS were exploited to provide detailed structural information at the isomeric level for oligonucleotides electrophoresed into agarose gels.
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