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/>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 >0.9918) in the range of 0.1–0.4 μg/L. LOD was calculated to be 0.025 μg/L and experimentally proved for spiked samples at levels down to 0.05 μg/L (S/N = 6) which was suited for monitoring the EU limit value of 0.1 μg/L in drinking water (0.5 μg/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 μg/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.