Abstract
Various mass spectrometric techniques, such as gas chromatography (GC)–mass spectrometry (MS) after derivatization, liquid chromatography–electrospray ionization (LC–ESI) MS and ESI-time of flight (TOF)-MS have been applied to the determination of, in general substituted, polar organic sulfonates. Methods were developed for the rapid quantification of such industrial chemicals in wastewater effluents and surface water, as required following spills leading to unusually high emissions into the river Rhine, Germany. Using these methods, the tonnage of methylsulfamido-antipyrin, an intermediate of the pain reliever metamizole synthesis, and 3-nitro-benzenesulfonate could be directly calculated without time-consuming enrichment or clean-up procedures. Thereby a significant increase in sensitivity was achieved by switching a cation suppressor between LC and MS. But still, the evaluation and identification of more complex chemical structures of formerly unknown substituted and halogenated by-products of 2-chlorotoluene methylsulfon-synthesis in wastewater was only possible through the combined interpretation of the GC– and LC–ESI mass spectra and with the additional information obtained from application of ESI-TOF-MS to the samples.
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