GC Analysis of Fipronil in Eggs on the SLB®PAHms Column after QuEChERS Extraction and Cleanup Using ZSep+

GC Analysis of Fipronil in Eggs on the SLB®PAHms Column after QuEChERS Extraction and Cleanup Using ZSep+

Conditions

sample/matrix Homogenized eggs spiked with fipronil at 5 ng/g
extraction tube Supel QuE nonbuffered extraction tube #1 (55294U)
extraction process 10 g of sample + 10 mL of acetonitrile in 50 mL extraction tube. Shake for 10 min at 2250 rpm on shaker. (Add contents of extraction tube and shake for 1 min. Centrifuge at 5000 rpm for 5 min. Remove supernatant for cleanup.)
cleanup tube 55408U, 55486U
cleanup process Add 1 mL of extract to 2 mL cleanup tube or 8 mL of extract to 12 mL cleanup tube. Shake for 1 min. (Centrifuge at 5000 rpm for 3 min. Remove supernatant for GC/MS/MS analysis)
column SLB®PAHms Capillary GC Column, 30m L× 0.25 mm I.D., df 0.25 μm (28340U)
oven 50 °C (2 min), 15 °C/min to 340 °C (10 min)
inj. temp. 250 °C

Description

Analysis Note The maximum residue limit designated by the EU for fipronil in eggs is 5 ng/g. Analysis to this level can be achieved using the “Quick, Easy, Effective, Rugged and Safe” approach (QuEChERS) for extraction and cleanup. In this application, QuEChERS extraction and cleanup followed by GC/MS/MS analysis were used for the determination of fipronil in egg samples spiked at 5 ng/g. Eggs have a relatively high fat content (approx. 10%), of which some will coextract during the QuEChERS procedure. ZSep +, a silica sorbent functionalized with zirconia and C18, can be used to reduce fatty matrix. Using ZSep+, recovery of fipronil after cleanup averaged 94% from egg samples spiked at 5 ng/g.
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Materials

     
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