Rapid and Cost-Effective Determination of Acrylamide in Coffee by Planar Chromatography and Fluorescence Detection After Derivatization with Dansulfinic Acid

Abstract

A new method has been developed for the determination of acrylamide in ground coffee by planar chromatography using prechromatographic in situ derivatization with dansulfinic acid. After pressurized fluid extraction of acrylamide from the coffee samples, the extracts were passed through activated carbon and concentrated. These extracts were applied onto a silica gel 60 HPTLC plate and oversprayed with dansulfinic acid. By heating the plate, acrylamide was derivatized into the fluorescent product dansylpropanamide. The chromatographic separation with ethyl acetatetert.-butyl methyl ether (8 + 2, v/v) mobile phase was followed by densitometric quantification at 254/>400 nm using a 4 point calibration via the standard addition method over the whole system for which acrylamide was added at different concentrations at the beginning of the extraction process. The method was validated for commercial coffee. The linearity over the whole procedure showed determination coefficients between 0.9995 and 0.9825 (n = 6). Limit of quantitation at a signal-to-noise ratio of 10 was determined to be 48 g/kg. The within-run precision (relative standard deviation, n = 6) of the chromatographic method was 3. Commercial coffee samples analyzed showed acrylamide contents between 52 and 191 g/kg, which was in correlation with amounts reported in previous publications.

Ultra trace level determinations of acrylamide in surface and drinking water by GC-MS after derivatization with xanthydrol

“…A wide range of analytical techniques has been developed to detect AA at trace levels in foods and water samples. Most of these procedures are based on determining AA by electrochemical methods , electrophoresis , chemiluminescence , HPLC , high‐performance TLC (HPTLC) , LC–MS , ion‐exclusion chromatography coupled to MS , GC , and GC–MS . Most of these methods were developed for the analysis of food or coffee, but several methods were oriented toward water .…”

“…In particular, the derivative is thermally labile and another hydrolysis reaction is needed to create the mono‐brominated derivative. In the addition to this bromination method, derivatization with 2‐mercaptobenzoic acid and dansulfinic acid has been used for the determination of AA. Polar reagents have been optimized for HPLC , HPTLC , or LC–MS detection and are not optimal for GC–MS detection.…”