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

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

The contribution of planar chromatography to food analysis

“…Despite some percent less precision than HPLC, HPTLC is, nevertheless, regarded as an appropriate method for, for example, analysis of biogenic amines in fish and fish products [51], benzo[a]pyrene (BaP) in 200 different food items [52], mycotoxins in a variety of samples [25], or Sudan red in different foods [11][12][13]. Similar results are also obtained by use of HPTLC-FLD and HPLC-MS-MS for analysis of acrylamide in water at ultra-trace levels [44]. For example in residue analysis of glyphosate and AMPA in water, an interlaboratory trial for HPLC-MS also showed that HPTLC-FLD gave results which correlated quite well (r 2 = 0.986) with the true value [53].…”

“…For active ingredients in energy drinks the repeatability in the matrix was up to 1.5% [46,47]; for ITX at trace levels in milk, yoghurt, and fat it was up to 6.4% [45]. Repeatability for HAA was up to 4.4% [43] and for acrylamide in water at ultra-trace levels, including derivatization, was 4.6% [44]. All these values are, surely, appropriate in food analysis.…”

“…But the situation changes if it is proved that the separating power (selectivity) is sufficient for the purpose given or the results obtained are comparable with those from methods of higher reputation [44]. Plate numbers and heights (HETP) depend on the chromatographic system selected, making it difficult to present representative figures.…”

Radiation Processing for Sprout Inhibition of Stored Potatoes and Mitigation of Acrylamide in Fries and Chips

“…Therefore, some non-MS methods such as LC-UV (Paleologos and Kontominas, 2005) and LC-diode array detection (DAD) with the detectors set at 210 and 225, pulsed electrochemical detection and GC-ECD (electron capture) have been developed and optimized (Casella et al, 2006). Thinlayer chromatography (TLC) with fluorescence detection after derivatization with dansulfinic acid has also been proposed (Alpmann and Morlock 2008). Besides, MS/ MS, proton transfer reaction mass spectrometry (PTR-MS), pyrolysis (Py) -GC-MS and FT-IR spectrometry have also been considered to be very useful techniques for monitoring real time changes in acrylamide content.…”

Correct assignment of lipophilic dye mixtures? A case study for high-performance thin-layer chromatography–mass spectrometry and performance data for the TLC–MS Interface

“…For the modified ChromeXtract coupled to electrospray ionization (ESI)-MS, repeatabilities (%RSD) of selected ion monitoring (SIM) signal intensities were proven to be, for example, 12.5% for harmane [14], 6.7% for isopropylthioxanthone [15] and 8.7% for 3-dansylpropanamide [10,16]. The functional correlation of the analytical response showed a determination coefficient (r 2 ) of 0.9915 for harmane [14] and a correlation coefficient (r) of 0.9983 for isopropylthioxanthone [15].…”