Rapid and sensitive determination of acrylamide in drinking water by planar chromatography and fluorescence detection after derivatization with dansulfinic acid

被引:44
作者
Alpmann, Alexander [1 ]
Morlock, Gertrud [1 ]
机构
[1] Univ Hohenheim, Inst Food Chem, D-70599 Stuttgart, Germany
关键词
acrylamide; derivatization; drinking water; HPTLC-FLD;
D O I
10.1002/jssc.200700391
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
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 mu g/L. LOD was calculated to be 0.02 5 mu g/L and experimentally proved for spiked samples at levels down to 0.05 mu g/L (S/N = 6) which was suited for monitoring the EU limit value of 0.1 mu g/L in drinking water (0.5 mu g/L demanded by World Health Organization (WBO)/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 mu g/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.
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页码:71 / 77
页数:7
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