Please use this identifier to cite or link to this item: http://hdl.handle.net/10316/27137
Title: Rapid and sensitive methodology for determination of ethyl carbamate in fortified wines using microextraction by packed sorbent and gas chromatography with mass spectrometric detection
Authors: Leça, João M. 
Pereira, Vanda 
Pereira, Ana C. 
Marques, José C. 
Keywords: Ethyl carbamate; Wines; Microextraction by packed sorbent; Gas chromatography–mass spectrometric detection
Issue Date: 6-Feb-2014
Publisher: Elsevier
Citation: LEÇA, João M. [et al.] - Rapid and sensitive methodology for determination of ethyl carbamate in fortified wines using microextraction by packed sorbent and gas chromatography with mass spectrometric detection. "Analytica Chimica Acta". ISSN 0003-2670. Vol. 811 (2014) p. 29-35
Serial title, monograph or event: Analytica Chimica Acta
Volume: 811
Abstract: This work presents a new methodology to quantify ethyl carbamate (EC) in fortified wines. The presented approach combines the microextraction by packed sorbent (MEPS), using a hand-held automated analytical syringe, with one-dimensional gas chromatography coupled with mass spectrometry detection (GC–MS). The performance of different MEPS sorbent materials was tested, namely SIL, C2, C8, C18, and M1. Also, several extraction solvents and the matrix effect were evaluated. Experimental data showed that C8 and dichloromethane were the best sorbent/solvent pair to extract EC. Concerning solvent and sample volumes optimization used in MEPS extraction an experimental design (DoE) was carried out. The best extraction yield was achieved passing 300 μL of sample and 100 μL of dichloromethane. The method validation was performed using a matrix-matched calibration using both sweet and dry fortified wines, to minimize the matrix effect. The proposed methodology presented good linearity (R2 = 0.9999) and high sensitivity, with quite low limits of detection (LOD) and quantification (LOQ), 1.5 μg L−1 and 4.5 μg L−1, respectively. The recoveries varied between 97% and 106%, while the method precision (repeatability and reproducibility) was lower than 7%. The applicability of the methodology was confirmed through the analysis of 16 fortified wines, with values ranging between 7.3 and 206 μg L−1. All chromatograms showed good peak resolution, confirming its selectivity. The developed MEPS/GC–MS methodology arises as an important tool to quantify EC in fortified wines, combining efficiency and effectiveness, with simpler, faster and affordable analytical procedures that provide great sensitivity without using sophisticated and expensive equipment.
URI: http://hdl.handle.net/10316/27137
ISSN: 0003-2670
DOI: 10.1016/j.aca.2013.12.018
Rights: openAccess
Appears in Collections:I&D CIEPQPF - Artigos em Revistas Internacionais
FCTUC Eng.Química - Artigos em Revistas Internacionais

Files in This Item:
File Description SizeFormat
Rapid and sensitive methodology for determination of ethyl carbamate in fortified wines.pdf421.95 kBAdobe PDFView/Open
Show full item record

SCOPUSTM   
Citations

26
checked on Feb 18, 2020

WEB OF SCIENCETM
Citations 5

29
checked on Jul 2, 2021

Page view(s)

244
checked on Jul 21, 2021

Download(s) 10

1,419
checked on Jul 21, 2021

Google ScholarTM

Check

Altmetric

Altmetric


Items in DSpace are protected by copyright, with all rights reserved, unless otherwise indicated.