Abstract
An all-glass miniaturized light-phase rotary perforator for the enrichment of polar compounds has been modified/miniaturized and applied. Its application is demonstrated here for the analysis of nitrophenols and dinitrophenols from low-concentration/low-volume samples. For the method development of high-performance liquid chromatography–mass spectrometry (MS) four eluents were tested: (1) water–methanol, (2) acetic acid–methanol, (3) trifluoroacetic acid–methanol and (4) water–acetonitrile. The last eluent mentioned was used for the subsequent investigation of samples from field experiments. Detection limits varied between 1 ng and 50 pg. The relative standard deviation in repeated measurements was below 15%, corresponding to a good reproducibility. Recoveries ranged between 31 and 100%, showing a significant dependence on the extraction time and the final volume of the sample after evaporation. Quantification was carried out by using deuterated 4-nitrophenol and 2,4-dinitrophenol as standards and applying previously determined response factors. Structure determination of further substances under atmospheric pressure chemical ionization was performed by a first screening with a source collision-induced dissociation, followed by the definite analysis by MSn. The first results are shown for cloud water, fog water and rainwater samples from different locations.
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Acknowledgements
The authors wish to thank H. Macholeth for the miniaturizing and modification to an all-glass LPRP, H. Bachmann for the processing of the enrichment of the cloud water samples and last, but not least, O. Klemm and T. Wrzesinsky (Bayreuther Institut für Terrestrische Ökosystemforschung, BITÖK, of the University of Bayreuth) as well as K. Bower (University of Manchester) for providing water samples from Waldstein and Holme Moss, respectively.
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Hofmann, D., Hartmann, F. & Herrmann, H. Analysis of nitrophenols in cloud water with a miniaturized light-phase rotary perforator and HPLC-MS. Anal Bioanal Chem 391, 161–169 (2008). https://doi.org/10.1007/s00216-008-1939-6
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DOI: https://doi.org/10.1007/s00216-008-1939-6