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
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