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

Abstract

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.

Optimization of Headspace Solid-phase Microextraction for GC-MS Analysis of Volatile Compounds Produced by Biocontrol Strain <i>Bacillus subtilis</i> CF-3 Using Response Surface Methodology

“…The sample volume reflected only the volume of the LB broth; during the trial, the amount of fermented CF-3 solution added to the flask was 10% of the designated volume of LB broth. LB broth blank samples and two empty headspace vials (one at the beginning and the other at the end of the analysis) were also measured in the same conditions to verify that the fiber was clean before conducting the next measurement (Rubio et al, 2014).…”

Application of Solid-Phase Microextraction Combined with Derivatization for Polar Compound Sampling in Environmental Analysis

“…Diazotation/iodination for aromatic amides: As to the analysis of aromatic amides, the analytes were in vial derivatized by diazotation and subsequent iodination prior to the HS SPME extraction as the following procedure [121,122]. Sample of water was acidified with hydroiodic acid and then mixed with sodium nitrite for a reaction time of 20 min; amidosulfonic acid was added to destroy the surplus of nitrite; and the surplus of iodine was destroyed with the addition of a saturated aqueous solution of sodium as shown in Fig.…”

“…In response to the treatment of massive number of samples, fast and automated analytical methods were recently developed for determination of fenbutatin oxide (FBTO) [131], thiol compounds [171], phenolic compounds [162], PAHs [176], and organometallic compounds [137,160] (Table 7.3). Table 7.3 Application of SPME and derivatization in water analysis [121,122] (continued) GC-MS [148] (continued) (continued) (continued) ECF GC-MS [37] (continued) -Not indicated…”

Usefulness of PARAFAC for the Quantification, Identification, and Description of Analytical Data

“…Applications of PARAFAC and PARAFAC2 to chromatographic analysis (in particular, GC-MS) in this regulated context can be found in Refs. [44,45,46] about pesticides and in the determination of monomers and additives that migrate into food [47,48]; in all these cases, the performance of the analyses is regulated. Usefulness of three-way techniques is shown with other chromatographic techniques too, for example, to determine veterinary residues with HPLC-DAD in Ref.…”