Please cite this article as: L. Rubio, S. Sanllorente, L.A. Sarabia, M.C. Ortiz, 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, Chemometrics and Intelligent Laboratory Systems (2014), doi: 10.1016/j.chemolab.2014 This is a PDF file of an unedited manuscript that has been accepted for publication. As a service to our customers we are providing this early version of the manuscript. The manuscript will undergo copyediting, typesetting, and review of the resulting proof before it is published in its final form. Please note that during the production process errors may be discovered which could affect the content, and all legal disclaimers that apply to the journal pertain.
A C C E P T E D M A N U S C R I P T ACCEPTED MANUSCRIPT
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
AbstractIn this work, a headspace solid-phase microextraction and gas chromatography coupled with mass spectrometry (HS-SPME-GC/MS) method for trace determination of primary aromatic amines was developed. The following analytes 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 to extraction the analytes were derivatized in the aqueous solution by diazotation and subsequent iodination. The derivatives were extracted by HS-SPME using a PDMS/DVB fiber and analyzed by CG/MS. A D-optimal design was used to study the parameters affecting the HS-SPME procedure and the derivatization step. Two experimental factors 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 and extraction time was considered in the proposed model. The loadings in the sample mode estimated by a PARAFAC (parallel factor analysis) decomposition for each analyte were the response used in the design because they are proportional to the amount of analyte extracted. The optimum conditions for the best extraction of the analytes were achieved when the reaction time was 20 min, the extraction temperature was 50ºC and the extraction time was 25 min. The interaction was significant.