RT info:eu-repo/semantics/article
T1 Optimization of a headspace solid-phase microextraction and gas chromatography/mass spectrometry procedure for the determination of aromatic amines in water and in polyamide spoons
A1 Rubio Martínez, Laura
A1 Sanllorente Méndez, Silvia
A1 Sarabia Peinador, Luis Antonio
A1 Ortiz Fernández, Mª Cruz
K1 Primary aromatic amines
K1 HS-SPME-GC/MS
K1 Derivatization
K1 D-optimal design
K1 PARAFAC
K1 Migration test
K1 Química analítica
K1 Chemistry, Analytic
AB In this work, a headspace solid-phase microextraction and gas chromatography coupledwith mass spectrometry(HS-SPME-GC/MS) method for trace determination of primary aromatic amines was developed. The followinganalytes were investigated: aniline (A), 4,4′-diaminodiphenylmethane (4,4′-MDA) and 2,4-diaminotoluene(2,4-TDA) using 3-chloro-4-fluoroaniline (3C4FA) and 2-aminobiphenyl (2ABP) as internal standards. Prior toextraction the analytes were derivatized in the aqueous solution by diazotation and subsequent iodination.The derivativeswere extracted byHS-SPME using a PDMS/DVB fiber and analyzed by GC/MS. A D-optimal designwas used to study the parameters affecting the HS-SPME procedure and the derivatization step. Two experimentalfactors at two levels and one factor at three levels were considered: (i) reaction time, (ii) extraction temperature,and (iii) extraction time in the headspace. The interaction between the extraction temperature andextraction time was considered in the proposed model. The loadings in the sample mode estimated by aPARAFAC (parallel factor analysis) decomposition for each analyte were the response used in the design becausethey are proportional to the amount of analyte extracted. The optimum conditions for the best extraction of theanalytes were achieved when the reaction time was 20 min, the extraction temperature was 50 °C and theextraction time was 25 min. The interaction was significant.A calibration based on a PARAFAC decomposition provided the following values of decision limit (CCα): 1.07 μgL−1for A, 1.23 μg L−1 for 2,4-TDA and 0.83 μg L−1 for 4,4′-MDA for a probability of false positive fixed at 5%. Also, theaccuracy (trueness and precision) of the procedurewas assessed. Furthermore, all the analyteswere unequivocallyidentified.Finally, the method was applied to spiked water samples and polyamide cooking utensils (spoons). 3% (w/v)acetic acid in aqueous solution was used as food simulant for testing migration from polyamide kitchenware.Detectable levels of 4,4′-diaminodiphenylmethane and aniline were found in food simulant from some of theinvestigated cooking utensils.
PB Elsevier
SN 0169-7439
YR 2014
FD 2014-04
LK http://hdl.handle.net/10259/4251
UL http://hdl.handle.net/10259/4251
LA eng
NO Ministerio de Economía y Competitividad (CTQ2011-26022) and Juntade Castilla y León (BU108A11-2)
DS Repositorio Institucional de la Universidad de Burgos
RD 26-abr-2024