GC Analysis of PCBs in Cod Liver Oil (Spiked) on SLB®-5ms after SPE using Supelclean™ EZ-POP NP and Supelclean LC-Si

GC Analysis of PCBs in Cod Liver Oil (Spiked) on SLB®-5ms after SPE using Supelclean™ EZ-POP NP and Supelclean LC-Si

Conditions

sample preparation SPE (Solid Phase Extraction)
sample/matrix cod liver oil spiked with PCBs (at 10 ng/g)
SPE tube/cartridge Supelclean™ EZ-POP NP, 12 mL, Pk 20 (54341-U)
SPE tube/cartridge Supelclean™ LC-Si, 100 mg/1 mL (504041)
condition 10 mL acetone, 10 min dry at 20" mercury
condition 4 mL acetone, 10 min dry at 20" mercury, then 4 mL hexane
sample addition 0.5 g sample, weighed directly on cartridge
sample addition 1 mL of resulting extract from above
elution 15 mL acetonitrile
elution 5 mL hexane
eluate post-treatment evaporate to 1 mL at 40 ºC under nitrogen
eluate post-treatment back extract acetonitrile eluent with 2 x 10 mL portions of hexane, evaporate hexane extract to approximately 1 mL at 40 ºC under nitrogen
column SLB-5ms 20m x 0.18mm, 0.18 µm (28564-U)
oven 75 °C (1 min), 12 °C/min to 340 °C (20 min)
carrier gas hydrogen, 1.2 mL/min
injection 1 µL, splitless (0.75 min)
liner 4 mm I.D., split/splitless type, wool packed single taper FocusLiner™ design
inj. temp. 250 °C
detector muECD, 340 °C

Description

Analysis Note PCBs are lipophilic and they have a tendency to bioaccuµlate and, through bioaccuµlation, may pose a risk to humans. When PCB-containing substances are cleaned or dumped into rivers or oceans, PCBs may find their way into aquatic lifeforms such as fish. Fish oil, which is high in levels of the beneficial fatty acids EPA and DHA, is a popular nutritional supplement. Due to the health risk of exposure to PCBs, fish oil is often analyzed for the presence of these compounds to ensure its safety. In this application, a new extraction/cleanup method was developed for PCBs from pure cod liver oil (which was spiked with PCBs) using the EZ-POP NP SPE cartridge.
Categories Analytical Chromatography, SPE Applications, GC Applications, Dioxins, PCBs, PBDEs, Dioxins/PCBs/PBDEs
Featured Industry Food and Beverages
Legal Information Supelclean is a trademark of Sigma-Aldrich Co. LLC, FocusLiner is a trademark of SGE Analytical Science Pty Ltd., SLB is a registered trademark of Sigma-Aldrich Co. LLC
suitability application for GC, application for SPE

Materials

     
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