Abstract
In this work, derivatization of ethyl carbamate (EC) with 9-xanthydrol prior to liquid chromatography with fluorimetric detection (HPLC-FLD) was revisited, focusing on refining the reaction conditions and on automation. Perchloric acid was used for sample acidification and a sequence of operations was defined to perform the reaction in the autosampler needle. Chromatographic separation together with automated pre-column derivatization accounted for 18.5 min analytical run. FLD photomultiplier gain was changed in the elution region of analyte to enhance sensitivity. The instrumental detection limit (DL) was 0.52 μg L−1; after suitable sample pretreatment, the proposed procedure was applied for EC determination in liquors, red wines and soy sauces (method DLs: 0.59; 0.96; 0.65 μg L−1, respectively). Recoveries obtained after standard addition were in the range 101–103%, 71–79% and 89–93%, respectively. Standard addition method was used for EC quantification in several samples; the concentrations ranged from not detected up to 40.7 μg L−1 in liquors, 25.9 μg L−1 in wines and 7.18 μg L−1 in soy sauces.
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