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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

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

Materials

SPE tube or plate

Product No.
Description
Pricing

55248-U

Supel™ QuE

Empty Centrifuge Tube with Lid, centrifuge tube volume 50 mL, pk of 50, suitable for EN 15662:2008 per BS

55294-U

Supel™ QuE

Non-Buffered Tube 1, pk of 50

55299-U

Supel™ QuE

Z-Sep+ Bulk, pkg of 20 g

CONDITIONS

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

Description

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

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HPLC ColumnsGC Columns & AccessoriesTLC Plates & AdsorbentsSolid Phase Microextraction (SPME)Solid Phase Extraction & QuEChERS

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