Open AccessDetermination of Ethyl Carbamate in Commercial Sweetened Sugar Cane Spirit by ESI-MS/MS Using Modified QuEChERS and 18-Crown-6/Trifluoroacetic Acid Spiking Additives
Author(s) -
Angélica Priscila Parussolo Tonin,
Camila B. Poliseli,
Nayane B. M. Sinosaki,
Fernanda Martínez,
Oscar de Oliveira Santos,
Cláudio Alvarenga de Oliveira,
Valquíria Silva,
Jesuí Vergílio Visentainer,
Eduardo C. Meurer
Publication year - 2022
Publication title -
journal of the brazilian chemical society
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.337
H-Index - 70
eISSN - 1678-4790
pISSN - 0103-5053
DOI - 10.21577/0103-5053.20220001
Subject(s) - chemistry , trifluoroacetic acid , chromatography , quechers , electrospray ionization , detection limit , mass spectrometry , ethyl carbamate , pesticide residue , pesticide , agronomy , biology , food science , wine
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.