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Key Documents

G005923

GC Analysis of Polynuclear Aromatic Hydrocarbons (PAHs) in Salmon on SPB®-608 (20 m x 0.18 mm I.D., 0.18 μm) after QuEChERS Cleanup using Supel™ QuE Z-Sep, Fast GC Analysis

suitable for GC, application for SPE

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About This Item

technique(s)

gas chromatography (GC): suitable
solid phase extraction (SPE): suitable

test parameters

sample preparation: Dispersive (QuEChERS)
sample/matrix: raw salmon spiked with PAHs at 100 ng/g
extraction process: add 25 mL acetonitrile and the contents of the Supel™ QuE Non-buffered tube (55294-U); shake for 5 minutes; centrifuge for 5 minutes at 3200 rpm
extraction tube: Supel™ QuE Non-buffered tube, magnesium sulfate/sodium chloride (55294-U)
clean-up tube: Supel™ QuE Z-Sep (500 mg, part no. 55299-U), magnesium sulfate (450 mg, part no. 63135) (55299-U, 63135)
clean-up process: transfer 3 mL of acetonitrile layer, Supel QuE Z-Sep (500 mg) and MgSO4 (450 mg) into an extraction tube; (shake 1 minute; centrifuge for 3 minutes at 3400 rpm; remove 1 mL supernatant for GC-MS analysis)
column: SPB-608, 20 m x 0.18 mm I.D. x 0.18 μm
oven: 60 °C (1 min), 25 °C/min to 275 °C, 10 °C/min to 300 °C (13 min)
inj. temp.: 265 °C
detector: MS, SIM
MSD interface: 300 °C
carrier gas: helium, 1.5 mL/min, constant
injection: 1 μL, splitless (1 min)
liner: 4 mm I.D. FocusLiner™ with taper

suitability

application for SPE

application(s)

food and beverages

General description

Stenerson, K.; Ye, M.; Halpenny, M., New Analytical Tools for the Determination of Persistent Organic Pollutants (POPs) in Fatty Food and Beverage Matrices Using QuEChERS Extraction/Cleanup and Gas Chromatography (GC) Analysis. Pittcon 2013. Sigma-Aldrich/Supelco publication T413034

Application

Extraction solvent: acetonitrile, 25 mL
Clean-up volume: 3 mL
Clearn-up tube: Supel™ QuE Z-Sep (500 mg, part no. 55299-U, magnesium sulfate (450 mg, part no. 63135)

Analysis Note

Sample pretreatment: Place 5 g ground sample into 50 mL centrifuge tube. Spike with 100 ng/g target PAHs and internal standards. Let sit 30 min. Add 5 mL water and homogenize.
This application demonstrates the use of dispersive SPE or QuEChERS for the extraction and cleanup of raw salmon for GC-MS analysis of polynuclear aromatic hydrocarbons (PAHs). Supel™ QuE Z-Sep sorbent was used in the cleanup step and found to reduce background and yield recoveries >80% for a majority of the PAHs tested.

Legal Information

FocusLiner is a trademark of SGE Analytical Science Pty Ltd.
SPB is a registered trademark of Merck KGaA, Darmstadt, Germany
Supel is a trademark of Sigma-Aldrich Co. LLC

Analito

Descripción
    Naphthalene
    2-Methylnaphthalene (β)
    1-Methylnaphthalene
    Biphenyl
    2,6-Dimethylnaphthalene
    Acenaphthylene
    Acenaphthene
    2,3,5-Trimethylnaphthalene
    Fluorene
    Dibenzothiophene
    Phenanthrene
    Anthracene
    1-Methylphenanthrene
    Fluoranthene
    Pyrene
    Retene
    Benzo[b]fluoranthene
    Benzo[k]fluoranthene
    Benzo[j]fluoranthene
    Benzo[e]pyrene
    Benzo[a]pyrene
    Perylene
    Dibenz[a,h]anthracene
    Benzo[ghi]perylene
    Ver todo (24)

SPE tube or plate

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