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Merck
CN

G006323

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

application for SPE, suitable for GC

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technique(s)

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

test parameters

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)
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 ºC 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 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)
inj. temp.: 250 °C
detector: μECD, 340 °C
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

suitability

application for SPE

application(s)

food and beverages

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 cod liver oil (which was spiked with PCBs) using the EZ-POP NP SPE cartridge.

Legal Information

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

Analyte

Description
    2,4,4′,-Trichlorobiphenyl (No. 28)
    2,2′,5,5′-Tetrachlorobiphenyl (No. 52)
    2,2′,4,5,5′-Pentachlorobiphenyl (No. 101)
    3,4,4′,5-Tetrachlorobiphenyl (No.81)
    3,3′,4,4′-Tetrachlorobiphenyl (No. 77)
    2′,3,4,4′,5-Pentachlorobiphenyl (No. 123)
    2,3′,4,4′,5-Pentachlorobiphenyl (No. 118)
    2,3,4,4′,5-Pentachlorobiphenyl (No. 114)
    2,2′,4,4′,5,5′-Hexachlorobiphenyl (No. 153)
    2,3,3′,4,4′-Pentachlorobiphenyl (No. 105)
    2,2′,3,4,4′,5′-Hexachlorobiphenyl (No. 138)
    3,3′,4,4′,5-Pentachlorobiphenyl (No. 126)
    2,3′,4,4′,5,5′-Hexachlorobiphenyl (No. 167)
    2,3,3′,4,4′,5-Hexachlorobiphenyl (No. 156)
    2,3,3′,4,4′,5′-Hexachlorobiphenyl (No. 157)
    2,2′,3,4,4′,5,5′-Heptachlorobipheny (No. 180)
    3,3′,4,4′,5,5′-Hexachlorobiphenyl (No. 169)
    2,3,3′,4,4′,5,5′-Heptachlorobiphenyl (No. 189)
    2,2′,3,3′,4,4′,5′5′,6,6′-Decachlorobiphenyl (No. 209)
    See All (19)

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