GC Analysis of PCBs in Cod Liver Oil (Unspiked) on SLB®-5ms after SPE using Supelclean™ EZ-POP NP and Supelclean LC-Si
CONDITIONS
sample preparation
Solid Phase Extraction
sample/matrix
cod liver oil
SPE tube/cartridge
Supelclean™ EZ-POP NP, 12 mL, pack of 20 (54341-U)
condition
10 mL acetone, 10 min dry at 20" mercury
sample addition
0.5 g sample, weighed directly on cartridge
elution
15 mL acetonitrile
eluate post-treatment
back extract acetonitrile eluent with 2 x 10 mL portions of hexane, evaporate hexane extract to approximately 1 mL at 40 °C under nitrogen
SPE tube/cartridge
Supelclean™ LC-Si, 100 mg/1 mL (504041)
condition
4 mL acetone, 10 min dry at 20" mercury, then 4 mL hexane
sample addition
1 mL of resulting extract from above
elution
5 mL hexane
eluate post-treatment
evaporate to 1 mL at 40 °C under nitrogen
column
SLB-5ms, 20 m x 0.18 mm I.D., 0.18 μm (28564-U)
oven
75 °C (1 min), 12 °C/min to 340 °C (20 min)
inj. temp.
250 °C
detector
μECD, 340 °C
carrier gas
hydrogen, 1.2 mL/min
injection
1 μL splitless (0.75 min)
Description
Analysis Note
PCBs are lipophilic and they have a tendency to bioaccumulate and, through bioaccumulation, 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 fish oil using the EZ-POP NP SPE cartridge.
Legal Information
SLB is a registered trademark of Merck KGaA, Darmstadt, Germany
Supelclean is a trademark of Sigma-Aldrich Co. LLC