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.com
Volume 5, Issue 3 (Suppl)
Mod Chem Appl, an open access journal
ISSN: 2329-6798
Global Chemistry 2017
September 04-06, 2017
September 04-06, 2017 | London, UK
5
th
Global Chemistry Congress
Optimization of automated pressurized liquid extraction and cleanup of PBDE in animal feed
Aleksandr Kozhushkevich, A A Komarov, V V Ovcharenko, A A Shelepchikov, A V Sorokin
and
A M Kalantaenko
VGNKI Institute, Russia
Introduction:
Polybrominated diphenyl ethers (PBDEs) are massively used as flame retardants. They are chemically and
biologically persistent, lipophilic, and able to bio-accumulate in fatty tissues and biomagnify throughout food chains. Similarly
to dioxins, PBDEs may be transferred from animal feed to lipid-containing food such as milk and eggs. Therefore, there is a need
for developing efficient methods of PBDE determination in animal feed matrices. With animal feed matrices, an automated
Power Prep system (FMS Inc., USA) has previously been used for PBDE clean-up following manual column extraction and
shaking with concentrated sulfuric acid. Our goal was to optimize PBDE extraction and clean-up from a typical feed matrix
(fish meal) using a more advanced Total-Rapid-Prep system (FMS, USA) which includes a pressurized liquid extraction
module (PLE), multi-column sample cleanup module (Power-Prep) and evaporation/solvent exchange module (SuperVap).
Materials & Method:
About 10 g of feed were mixed with diatomaceous earth, and then spiked with 100 µl mixtures of mass-
labeled PBDE congeners and 100 µl mass-labeled PBDE internal standard solutions to monitor recoveries. Extraction was
performed on PLE with n-hexane at 1200C and 15 MPa (two static cycles of 20 min each, the purge time 120 s). The extracts
were evaporated on SuperVap to 10 ml and subjected to automated cleanup on silica and alumina columns. Elution parameters
were optimized (Fig. 1). Elution by 40 ml 20% DCM/Hex followed by 120 ml 50% DCM/Hex gave the best recovery values for
all congeners including di-brominated BDE-15 (Fig. 2). The purified extracts were concentrated on SuperVap and analysed on
a TSQ 8000 Evo GC-MS/MS (Thermo, USA).
Results & Discussion:
Compared to the semi-automated method, we obtained better recoveries for di- to tetra-brominated
congeners (Fig. 2) in a fully automated setup which saves time and solvents.
Biography
Aleksandr Kozhushkevich is a Senior Scientist at All-Russian State Center for Quality and Standardization of Veterinary Drugs and Feed (VGNKI), Department of
POPs Control in Feedstock and Feeds. He has many years of experience in the analysis of persistent organic pollutants in food and feed.
kazhuha@gmail.comAleksandr Kozhushkevich et al., Mod Chem Appl 2017, 5:3(Suppl)
DOI: 10.4172/2329-6798-C1-006