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Gas chromatography–time-of-flight mass spectrometry for sensitive determination of organic microcontaminants

✍ Scribed by René J. J. Vreuls; Jens Dallüge; Udo A. Th. Brinkman

Publisher
John Wiley and Sons
Year
1999
Tongue
English
Weight
260 KB
Volume
11
Category
Article
ISSN
1040-7685

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✦ Synopsis

In this study the spectrum storage rate, linearity of response, and detection limits of time-of-flight mass spectrometry in combination with capillary Ž . gas chromatography GC᎐TOF-MS were evaluated. TOF-MS was found to be a very powerful technique with limits of detection in the low pg range for Ž . Ž . organophosphorus pesticides OPPs, 1᎐6 pg , triazine herbicides 4᎐60 pg and Ž . polycyclic aromatic hydrocarbons 0.3᎐6 pg . Spectral information of good quality was obtained at spectrum storage rates of up to 500 Hz. For all analyte classes response concentration plots were linear in the range 2 pg᎐1 ng, which is very important in TOF-MS. GC᎐TOF-MS was applied to the determination of the above compound classes in various extracts, which were obtained by means of miniaturized extraction procedures. The analytes were extracted from aqueous Ž . samples surface water, tea and sediment into an organic solvent and 1 L of the extract was injected into the GC system using a split injector. One software tool, automated spectral peak deconvolution, turned out to be very valuable. It enabled calculation of spectra from overlapping peaks even if their retention times differed only three scans. Peaks were reported with their deconvoluted spectrum, the so-called peak true spectrum. In actual practice this means that peaks had to be separated for 0.3 or 0.15 s at a spectrum storage rate of 10 and 20 Hz, respectively. Three extraction procedures combined with GC᎐TOF-MS allowed the analysis of the microcontaminants at 0.1 grL in surface water, at 2 grL in tea, and at Ž . 0.01 mgrkg in sediment with a signal-to-noise ratio SrN of 10. In other words, relevant real-life detection limits can be obtained even under split injection conditions.

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