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1. A Novel Cleanup Procedure for Determining Mono- to Deca-BDE in Lipophilic Matrices Shelepchikov AA1,2, Ovcharenko VV1, Brodsky ES2, Kozhushkevich AI1, Komarov AA1, Kalantaenko AM1, Turbabina KA1 1 The All-Russian State Center for Quality and Standardization of Veterinary Drugs and Feed (VGNKI) 2Severtsov Institute of Ecology and Evolution, Russian Academy of Sciences (IPEE RAS), Moscow, Russia Introduction: • More than 20 years of active PBDEs analysis • Generally accepted methods are still lacking • Limited laboratories detect heavy-PBDEs • Very few can analyze Mono- and DiBDEs BACK NEXT

2. The USEPA 1614 Method has no recoveries criteria for mono- and di-BDEs. The Method E3481 of Ontario Ministry of the Environment and Climate Change allows for the determination of tri- to deca-BDE using the Power‑Prep™ by FMS Other published methods known to us are not used for routine analysis of fat samples or do not contain enough information for reproducing The purpose of this work was to develop a viable method for determining mono- to decabromobiphenyl ethers in fat-containing food and feedstuff matrices On a FMS TotalPowerPrep™ we completely lost MoBDE and have obtained 44-77% recovery for medium brominated BDE (*), with more then 20 pg BDE-47 at blank(**) (*) fish meal sample, procedure proposed by official FMS representatives (**)columns PBDE-HCDS-ACD-TFC, PBDEE-ABN-STD, PBDEA-BAS-011, PBDEC-CCE-034, solvent blank ~1pg A Novel Cleanup Procedure for Determining Mono- to Deca-BDE in Lipophilic Matrices BACK Shelepchikov AA, Ovcharenko VV, Brodsky ES, Kozhushkevich AI, Komarov AA, et al NEXT

3. We didn’t trytoimproveEPA, FMS etc. methods and developed a novel one fromscratch ~ 0.5 g fat in 5-7 ml hexane Fat removing column ~14-15mm ID glass column Na2SO4 ~ 2g K2SiO3 ~ 4g Na2SO4 ~ 1g Florisil ~ 5g K2SiO3 ~ 4g Na2SO4 ~ 1g H2SO4 /SiO2 ~ 1g Alumina column ~ 9mm ID glass column 4 g neutral aluminum oxide (activated at 400°C overnight), condition with 15 ml hexane Concentrate to ~2 ml (optional) Flow Wash by 15 ml hexane (waste) Elution by 50 ml hexane Elution by 20 ml diethyl ether : hexane (1:4 v:v) heavy PBDE low PBDE Concentration to ~10 μl and GC-MS analysis That’s all you need for clean-up 25-30 m SGE HT-8 or “5% Phenyl” column 10-15 m DB-5ht column A Novel Cleanup Procedure for Determining Mono- to Deca-BDE in Lipophilic Matrices NEXT Shelepchikov AA, Ovcharenko VV, Brodsky ES, Kozhushkevich AI, Komarov AA, et al BACK

4. PBDE concentrations and recoveries in fish oil sample A Novel Cleanup Procedure for Determining Mono- to Deca-BDE in Lipophilic Matrices BACK NEXT Shelepchikov AA, Ovcharenko VV, Brodsky ES, Kozhushkevich AI, Komarov AA, et al

5. All PBDEs congeners from mono- to deca- • Low blank level (<1 pg for most abundant congeners) • Easy to use • Stable and high recovery (at least 80%) • Low solvent consumption (110 ml per sample) • Halogen FREE • No Fake Management Systems and others expensive lab techniques METHOD BENEFITS A Novel Cleanup Procedure for Determining Mono- to Deca-BDE in Lipophilic Matrices Shelepchikov AA, Ovcharenko VV, Brodsky ES, Kozhushkevich AI, Komarov AA, et al BACK NEXT

6. A Novel Cleanup Procedure for Determining Mono- to Deca-BDE in Lipophilic Matrices Shelepchikov AA, Ovcharenko VV, Brodsky ES, Kozhushkevich AI, Komarov AA, Kalantaenko AM, Turbabina KA any questions dioxin@mail.ru Acknowledgements: We would like to thank the Biosystems Safety Center of Moscow State University for technical support. References: 1. Berton P, Lana NB, Ríos JM, García-Reyes JF and Altamirano JC (2016) Analytica Chimica Acta, 905 24-41. 2. Lacorte S and Ikonomou, MG (2009) Chemosphere74 412-420. 3. Shin J, Boo H, Bang E, Gorinstein S and Seo J (2012) European Food Research and Technology 235 295-301. 4. Blanco SL and Vieites JM Analytica Chimica Acta (2010) 672 137-146. Thank you for your attention! BACK NEXT