Abstract
A fast, sensitive, and selective direct injection electrospray tandem mass spectrometry (DI‑ESI‑MS/MS) method that is able to quantify ethyl carbamate in commercial sweetened sugar cane spirit is described. The preparation method uses a modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) with potassium carbonate added to sweetened sugar cane spirit to separate the aqueous phase from the ethanol phase. The aqueous phase contains sucrose that suppresses electrospray ionization. Ethyl carbamate supernatant from the ethanol phase is transferred and enriched with 18-crown-6/trifluoroacetic acid additives. The additives sequester metal cations reducing the ionization of sodium and potassium, favoring the detection of ethyl carbamate as sole protonated cations. The method was successfully applied for the quantification of eleven real samples and certified sugar cane spirit demonstrating its applicability for quality control and regulatory analysis. The method showed reliable analytical parameters compared to conventional gas chromatography mass spectrometry (GC-MS) method commonly used for ethyl carbamate analysis. DI-ESI-MS/MS method requires just a fast step sample clean up and presents consistent values for the limit of detection (LOD 48.0 μg L−1) and limit of quantification (LOQ 160.0 μg L−1). Furthermore, the recoveries obtained were close to 100%, with relative standard deviations below 10% of sample certificates.
Highlights
Cachaça is a type of sugar cane spirit produced in Brazil and recognized as a typical Brazilian alcoholic drink that might be sweetened or not with sucrose
The conventional DI-ESI-MS/MS method developed by Ribeiro et al.[25] of ethyl carbamate determination was not efficient to evaluate sweetened cachaça or sweetened sugar cane spirit, due to the high degree of sugar that reveals a high matrix effect on the electrospray ionization source and the standard addition calibration method make the analyzes laborious and time-consuming
Considering that a variety of alcoholic beverages have sugar as additive and the need to improve the analytical frequency is always required, we developed a modified QuECheRS with an external calibration curve to analyze ethyl carbamate from these beverages.[25,26]
Summary
Cachaça is a type of sugar cane spirit produced in Brazil and recognized as a typical Brazilian alcoholic drink that might be sweetened or not with sucrose. Ethyl carbamate (PubChem CID 5641) is formed in food and beverages by the reaction of ethanol with hydrogen cyanide,[6] and may be formed in the process of producing cachaças and sugar cane spirits.[7,8,9,10] Sugar cane spirits are very popular in Brazil, cachaça, and are part of a typical drink called “caipirinha” (a mixture of cachaça or sugar cane spirit to sugar, lemon and ice). In Brazil, the maximum residue level of ethyl carbamate in (sweetened or not) cachaça and sugar cane spirit is 210 μg L−1, as defined by MAPA, the Brazilian regulation agency for food control.[1]
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