Analysis of nitrophenols in cloud water with a miniaturized light-phase rotary perforator and HPLC-MS.

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 MS( n ). The first results are shown for cloud water, fog water and rainwater samples from different locations.