Automated pre-column derivatization with 9-xanthydrol for the determination of ethyl carbamate in food matrices by high performance liquid chromatography with fluorimetric detection
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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.
KeywordsEthyl carbamate 9-xanthydrol High performance liquid chromatography Fluorimetric detection Wine Tequila Soy sauce
The financial support from National Council of Science and Technology, Mexico (CONACYT, Project 253879), and from University of Guanajuato (Grant 051/2018), is gratefully acknowledged.
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