Determination of aromatic amines at trace levels by derivatization with heptafluorobutyric anhydride and gas chromatography-electron-capture negative-ion chemical ionization mass spectrometry

Longo, Marco; Cavallaro, A.

doi:10.1016/s0021-9673(96)00548-1

Cited by 51 publications

(23 citation statements)

References 16 publications

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“…These methods include ion-pair extraction with bis-2-ethylhexylphosphate (BEHPA), derivatization of compounds with isobutyl chloroformate (IBCF) and their GC/MS analysis. Longo and Cavallaro developed a method for the determination of aromatic amines at trace levels by derivatization with heptafluorobutyric anhydride and gas chromatography electroncapture negative-ion chemical ionization mass spectrometry [31].Brede et al developed a GC/MS method for the determination of primary aromatic amines in water samples, using solid-phase analytical derivatization (SPAD) for the sample preparation [32]. However, the GC/MS technique requires a preconcentration step to obtain good sensitivity.…”

Section: Accepted M Manuscriptmentioning

confidence: 99%

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

Rubio

Sanllorente

Sarabia

et al. 2014

Chemometrics and Intelligent Laboratory Systems

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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.

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Section: Accepted M Manuscriptmentioning

confidence: 99%

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

Rubio

Sanllorente

Sarabia

et al. 2014

Chemometrics and Intelligent Laboratory Systems

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“…This was followed by perfluorobutyrylation (Section III.B.1) and end analysis by GC-MS (Section IV.A) 110 . A 125-fold rise in concentration was achieved in a method for determination of aromatic amines and nitroarene metabolites in acid hydrolyzed urine.…”

Section: Liquid-liquid Extractionmentioning

confidence: 99%

“…A study was carried out on 73 primary and secondary aromatic amines, including some nitro and chloro derivatives, by which a 100 µL solution of the amine in isooctane was treated with an equal volume of heptafluorobutyric anhydride, at 60 • C for 30 min, followed by elimination of excess reagent and acid byproduct with 2 mL of phosphate buffer at pH 8, LLE with three 1 mL aliquots of CH 2 Cl 2 , drying and evaporation of the unified extract to 0.5 mL. End analysis was by GC with electron-capture negative-ion chemical ionization (EC-NICI) MS detection (Section IV.A) 110 .…”

Section: In-line Preconcentrationmentioning

confidence: 99%

Analytical Aspects of Aromatic Amines

Zabicky

2009

Patai's Chemistry of Functional Groups

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“…Methods for preconcentration and detection of aromatic amines in environmental samples were mainly based on liquid-liquid extraction (LLE) [7], solid-phase extraction (SPE) [8] and liquid-liquid-liquid-phase microextraction (LLLME) [9] followed by high performance liquid chromatography (HPLC) with ultraviolet-visible or fluorescence detector, as well as solidphase microextraction (SPME) [10,1] and dispersive liquid-liquid microextraction (DLLME) with simultaneous derivatization followed by gas chromatography/mass spectrometry (GC-MS) [11].…”

Section: Introductionmentioning

confidence: 99%

Simultaneous conduction of two- and three-phase hollow-fiber-based liquid-phase microextraction for the determination of aromatic amines in environmental water samples

Tao

Liu

Wang

et al. 2009

Journal of Chromatography A

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Determination of aromatic amines at trace levels by derivatization with heptafluorobutyric anhydride and gas chromatography-electron-capture negative-ion chemical ionization mass spectrometry

Cited by 51 publications

References 16 publications

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

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

Analytical Aspects of Aromatic Amines

Simultaneous conduction of two- and three-phase hollow-fiber-based liquid-phase microextraction for the determination of aromatic amines in environmental water samples

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