Optimization of Large-Volume Injection for the Determination of Polychlorinated Biphenyls in Childrenʼs Fast-Food Menus by Low-Resolution Mass Spectrometry

This study includes the determination of five indicator polychlorinated biphenyls (PCBs) (52, 101, 153, 138, and 180), six non-ortho PCBs (35, 80, 81, 77, 126, and 169), and two mono-ortho PCBs (28 and 118) in fast food for children. A freeze-dried sample of 10 g is extracted by using pressurized n-...

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Bibliographic Details
Published in:Journal of agricultural and food chemistry 2008-03, Vol.56 (6), p.1797-1803
Main Authors: Esteve-Turrillas, Francesc A, Caupos, Emilie, Llorca, Isabel, Pastor, Agustín, de la Guardia, Miguel
Format: Article
Language:English
Subjects:
Analytical chemistry
Analytical Methods
Biological and medical sciences
Chemical Sciences
child nutrition
Child, Preschool
children fast-food menu
children's foods
detection limit
extraction
fast foods
Food Analysis - methods
food contamination
Food industries
freeze drying
Fundamental and applied biological sciences. Psychology
gas chromatography
Gas Chromatography-Mass Spectrometry
gel permeation chromatography
Humans
large-volume injection
lipid content
mass spectrometry
Mass Spectrometry - methods
meals (menu)
polychlorinated biphenyls
Polychlorinated Biphenyls - analysis
pretreatment
PVT−CG−MS−MS
Quality Control
quantitative analysis
Reproducibility of Results
solid phase extraction
Tandem Mass Spectrometry
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Summary:This study includes the determination of five indicator polychlorinated biphenyls (PCBs) (52, 101, 153, 138, and 180), six non-ortho PCBs (35, 80, 81, 77, 126, and 169), and two mono-ortho PCBs (28 and 118) in fast food for children. A freeze-dried sample of 10 g is extracted by using pressurized n-hexane in two 5 min cycles at 120 °C and 100 mbar. Fatty extracts were cleaned up by means of acetonitrile/n-hexane partitioning and gel-permeation chromatography. The fractionation of non-ortho, mono-ortho, and indicator PCBs was made on graphitized carbon solid-phase extraction cartridges by using n-hexane, n-hexane/toluene (99:1, v/v), and toluene as elution solvents. Gas chromatography coupled to tandem mass spectrometry and large-volume injections with a programmed-temperature vaporizer (PTV-LV) were used to increase sensitivity and selectivity of the PCB determination. The PTV-LV injection settings, that is, vaporizing temperature, vaporizing time, and purge flow, were optimized by using a central composite design. A 15−40 times increased sensitivity was reached as compared with that obtained with the conventional 1 μL splitless injection. The limits of detection achieved were between 0.3 and 1.2 pg/g, and repeatability data, as relative standard deviation varied, ranged from 2 to 9% for the 0.05 ng/mL PCB level.
ISSN:0021-8561
1520-5118
DOI:10.1021/jf073141u