title: Microextraction by packed sorbent and salting-out-assisted liquid-liquid extraction for the determination of aromatic amines formed from azo dyes in textiles.
abstract: EU legislation prohibits the use of certain azo dyes which, on reduction, form any of 22 aromatic amines listed in Regulation (EC) 1907/2006 at concentrations above the threshold limit of 30 mg Kg(-1). Two different extraction techniques for the determination of aromatic amines formed from azo dyes in textiles in combination with gas chromatography-mass spectrometry (GC-MS) are described. The first one is based on microextraction by packed sorbent (MEPS) and the other approach involves salting-out-assisted liquid-liquid extraction (SALLE). The influence of several parameters on the efficiency of the extraction using MEPS (sorbent material, sample volume, elution solvent, elution volume and washing steps, among others) and SALLE (extraction volume and amount of salt) were investigated. In addition, chromatographic separation was optimized and quadrupole mass spectrometry was evaluated using the synchronous SIM/scan data acquisition mode. The repeatability (n=8, S/N=3) of the methods, calculated as the relative standard deviation (RSD) was below 15 and 11% for all compounds when MEPS and SALLE were used, respectively. Standard additions procedure was used to quantify the aromatic amines in the textil samples. The detection limits in the samples for both methods were lower than the maximum value allowed by legislation. The results obtained in the analysis of textiles revealed the presence of o-anisidine, p-chloroaniline, 4-chloro-o-toluidine, 2-naphthylamine and 3,3'-dimethoxybenzidine in some of them.
authors.affiliation: Departamento de Química Analítica, Nutrición y Bromatología, Facultad de Ciencias Químicas, Universidad de Salamanca, 37008 Salamanca, Spain.
authors.forename: Miguel del Nogal
authors.initials: Mdel N
authors.lastname: Sánchez
authors.affiliation: Departamento de Química Analítica, Nutrición y Bromatología, Facultad de Ciencias Químicas, Universidad de Salamanca, 37008 Salamanca, Spain.
authors.forename: Patricia Martín
authors.initials: PM
authors.lastname: Santos
authors.affiliation: Departamento de Química Analítica, Nutrición y Bromatología, Facultad de Ciencias Químicas, Universidad de Salamanca, 37008 Salamanca, Spain.
authors.forename: Cristina Pérez
authors.initials: CP
authors.lastname: Sappó
authors.affiliation: Departamento de Química Analítica, Nutrición y Bromatología, Facultad de Ciencias Químicas, Universidad de Salamanca, 37008 Salamanca, Spain. Electronic address: jlpp@usal.es.
authors.forename: José Luis Pérez
authors.initials: JL
authors.lastname: Pavón
authors.affiliation: Departamento de Química Analítica, Nutrición y Bromatología, Facultad de Ciencias Químicas, Universidad de Salamanca, 37008 Salamanca, Spain.
authors.forename: Bernardo Moreno
authors.initials: BM
authors.lastname: Cordero
keywords: Aromatic amines; Mass spectrometry; Microextraction by packed sorbent; Salting-out-assisted liquid–liquid extraction