Rapid and sensitive determination of acrylamide in drinking water by planar chromatography and fluorescence detection after derivatization with dansulfinic acid. Alpmann, A. & Morlock, G. Journal of Separation Science, 31(1):71–77, 2008. Paper abstract bibtex On the basis of a novel derivatization, a new planar chromatographic method has been developed for the determination of acrylamide (AA) in drinking water at the ultra-trace level. After SPE, the water extracts were oversprayed on a high-performance thin-layer chromatography (HPTLC) silica gel plate with the derivatization agent dansulfinic acid and derivatized in situ. Chromatography was performed with ethyl acetate and the fluorescent product was quantified at 366/\textgreater400 nm. Verification was based on HPTLC-ESI/MS, HPTLC-direct analysis in real-time (DART)-TOF/MS and NMR. The routine HPTLC-fluorescence detection (FLD) method was validated for spiked drinking water. The regression analysis was linear (r \textgreater0.9918) in the range of 0.1-0.4 mug/L. LOD was calculated to be 0.025 mug/L and experimentally proved for spiked samples at levels down to 0.05 mug/L (S/N = 6) which was suited for monitoring the EU limit value of 0.1 mug/L in drinking water (0.5 mug/L demanded by World Health Organization (WHO)/US Environmental Protection Agency (EPA)). Within-run precision and the mean between-run precision (RSD, n = 3, three concentration levels each) were evaluated to be 4.8 and 11.0%, respectively. The mean recovery (0.1, 0.2, and 0.3 mug/L) was 96% corrected by the internal standard. The method, in comparison with HPLC-MS/MS showed comparable results and demonstrated the accuracy of the method.
@article{alpmann_rapid_2008,
title = {Rapid and sensitive determination of acrylamide in drinking water by planar chromatography and fluorescence detection after derivatization with dansulfinic acid},
volume = {31},
issn = {1615-9314},
url = {http://dx.doi.org/10.1002/jssc.200700391},
abstract = {On the basis of a novel derivatization, a new planar chromatographic method has been developed for the determination of acrylamide (AA) in drinking water at the ultra-trace level. After SPE, the water extracts were oversprayed on a high-performance thin-layer chromatography (HPTLC) silica gel plate with the derivatization agent dansulfinic acid and derivatized in situ. Chromatography was performed with ethyl acetate and the fluorescent product was quantified at 366/{\textgreater}400 nm. Verification was based on HPTLC-ESI/MS, HPTLC-direct analysis in real-time (DART)-TOF/MS and NMR. The routine HPTLC-fluorescence detection (FLD) method was validated for spiked drinking water. The regression analysis was linear (r {\textgreater}0.9918) in the range of 0.1-0.4 mug/L. LOD was calculated to be 0.025 mug/L and experimentally proved for spiked samples at levels down to 0.05 mug/L (S/N = 6) which was suited for monitoring the EU limit value of 0.1 mug/L in drinking water (0.5 mug/L demanded by World Health Organization (WHO)/US Environmental Protection Agency (EPA)). Within-run precision and the mean between-run precision (RSD, n = 3, three concentration levels each) were evaluated to be 4.8 and 11.0\%, respectively. The mean recovery (0.1, 0.2, and 0.3 mug/L) was 96\% corrected by the internal standard. The method, in comparison with HPLC-MS/MS showed comparable results and demonstrated the accuracy of the method.},
number = {1},
journal = {Journal of Separation Science},
author = {Alpmann, Alexander and Morlock, Gertrud},
year = {2008},
keywords = {AccuTOF},
pages = {71--77},
}
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Chromatography was performed with ethyl acetate and the fluorescent product was quantified at 366/\\textgreater400 nm. Verification was based on HPTLC-ESI/MS, HPTLC-direct analysis in real-time (DART)-TOF/MS and NMR. The routine HPTLC-fluorescence detection (FLD) method was validated for spiked drinking water. The regression analysis was linear (r \\textgreater0.9918) in the range of 0.1-0.4 mug/L. LOD was calculated to be 0.025 mug/L and experimentally proved for spiked samples at levels down to 0.05 mug/L (S/N = 6) which was suited for monitoring the EU limit value of 0.1 mug/L in drinking water (0.5 mug/L demanded by World Health Organization (WHO)/US Environmental Protection Agency (EPA)). Within-run precision and the mean between-run precision (RSD, n = 3, three concentration levels each) were evaluated to be 4.8 and 11.0%, respectively. The mean recovery (0.1, 0.2, and 0.3 mug/L) was 96% corrected by the internal standard. 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After SPE, the water extracts were oversprayed on a high-performance thin-layer chromatography (HPTLC) silica gel plate with the derivatization agent dansulfinic acid and derivatized in situ. Chromatography was performed with ethyl acetate and the fluorescent product was quantified at 366/{\\textgreater}400 nm. Verification was based on HPTLC-ESI/MS, HPTLC-direct analysis in real-time (DART)-TOF/MS and NMR. The routine HPTLC-fluorescence detection (FLD) method was validated for spiked drinking water. The regression analysis was linear (r {\\textgreater}0.9918) in the range of 0.1-0.4 mug/L. LOD was calculated to be 0.025 mug/L and experimentally proved for spiked samples at levels down to 0.05 mug/L (S/N = 6) which was suited for monitoring the EU limit value of 0.1 mug/L in drinking water (0.5 mug/L demanded by World Health Organization (WHO)/US Environmental Protection Agency (EPA)). 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