title: Improved sample preparation for GC-MS-SIM analysis of ethyl carbamate in wine.
abstract: An improved sample preparation procedure for analysis of carcinogenic ethyl carbamate (EC) in wine by GC-MS-SIM is proposed. Differences over AOAC reference procedure were: (1) use of EC-d5 as internal standard instead of less similar propyl carbamate; (2) extraction by diethyl ether instead of more toxic dichloromethane, and (3) concentration by vacuum automated parallel evaporation instead of more time and work consuming rotary evaporation. Mean recovery was 104.4%, intraday precision was 6.7% (3.4 μg L(-)(1)) and 1.7% (88.5 μg L(-)(1)), regression coefficient was 0.999 in the linear working range of 3-89 μg L(-)(1), and limits of detection and quantification were 0.4 and 1.2 μg L(-)(1). Applicability was demonstrated by analysis (in triplicate) of 5 wine samples. EC concentration ranged from 5.2 ± 0.2 to 29.4 ± 1.5 μg L(-)(1). The analytical method is selective, accurate, repeatable, linear, and has similar method performance as the reference method along with the several mentioned advantages.
authors: Universidade Federal Rural de Pernambuco, Departamento de Tecnologia Rural, CEP 52.171-900, Recife, PE, Brazil. Electronic address: ian@dtr.ufrpe.br.
authors: Ian C C
authors: IC
authors: Nóbrega
authors: Embrapa Uva e Vinho/Semiárido, BR 428, km 152, CEP 56.302-970, Petrolina, PE, Brazil.
authors: Giuliano E
authors: GE
authors: Pereira
authors: Laboratório de Agrotóxicos e Contaminantes em Alimentos e Bebidas Alcoólicas (LabTox), Instituto de Tecnologia de Pernambuco (ITEP), CEP 50.740-540, Recife, PE, Brazil.
authors: Marileide
authors: M
authors: Silva
authors: Universidade Federal Rural de Pernambuco, Departamento de Tecnologia Rural, CEP 52.171-900, Recife, PE, Brazil.
authors: Elainy V S
authors: EV
authors: Pereira
authors: Laboratório de Agrotóxicos e Contaminantes em Alimentos e Bebidas Alcoólicas (LabTox), Instituto de Tecnologia de Pernambuco (ITEP), CEP 50.740-540, Recife, PE, Brazil.
authors: Marcelo M
authors: MM
authors: Medeiros
authors: Laboratório de Agrotóxicos e Contaminantes em Alimentos e Bebidas Alcoólicas (LabTox), Instituto de Tecnologia de Pernambuco (ITEP), CEP 50.740-540, Recife, PE, Brazil.
authors: Danuza L
authors: DL
authors: Telles
authors: Laboratório de Agrotóxicos e Contaminantes em Alimentos e Bebidas Alcoólicas (LabTox), Instituto de Tecnologia de Pernambuco (ITEP), CEP 50.740-540, Recife, PE, Brazil.
authors: Eden C
authors: EC
authors: Albuquerque
authors: Embrapa Uva e Vinho/Semiárido, BR 428, km 152, CEP 56.302-970, Petrolina, PE, Brazil.
authors: Juliane B
authors: JB
authors: Oliveira
authors: Chemisches und Veterinäruntersuchungsamt (CVUA) Karlsruhe, Weissenburger Strasse 3, 76187 Karlsruhe, Germany.
authors: Dirk W
authors: DW
authors: Lachenmeier
mesh_terms: D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D014520:Urethane / Q000032:analysis*; D014920:Wine / Q000032:analysis*
chemical_list: D014520:Urethane
keywords: Automated parallel evaporation; Diethyl ether extraction; Ethyl carbamate; GC–MS–SIM; Validation; Wine