Power-Prep Automated Extraction and Clean-up System for

Dioxins are located in fat. ✓ Norm PCDD/Fs = 5 pg I-TEQ/g fat. ✓ Norm PCBs = 200 ng/g fat. PCDD/Fs and PCBs in Foodstuff. DIOXIN SYMPOSIUM BREMEN ...
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Power-PrepTM Automated Extraction and Clean-up System for PCDDs, PCDFs and PCBs Jef Focant and Hamid Shirkhan FMS Inc. Dioxin Lab. BELGIUM

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Dioxins Analysis ! Extraction (Soxhlet, L-L, Micro-waves, SFE, ASE, SPE, …) ! Clean-up (Liquid chromatography) ! Analysis (GC/MS, bio-assays, …) DIOXIN SYMPOSIUM BREMEN

Power-prep System ! Automated sample prep. System ! PC controlled valves and pump ! Modular system (1 to 20 samples in

)

! Stalling et al. paper based (Si, Al, C) ! Disposable columns (1-25g packing) DIOXIN SYMPOSIUM BREMEN

Valves Driver Pump and Pressure

Power supply

Controller

Valves

DIOXIN SYMPOSIUM BREMEN

Gauge 1. 2. 3. 4. 5.

Pump 1

2

M3 M2

1

2

Silica

M3

Hexane 2% DCM 50% DCM EtAc/Benz Toluene

1 2 3 4 5

Sample

Carbon

M6 1

M4

M6

1

2

2

1

M7 M5

2

2

1

M7 M5 2

2

1

1

M4

2

2

1

Alumina

1

1. 2. 3. 4. 5.

PCDD/Fs PCB Fraction 1 Fraction 2 Fraction 3

M8 Organic waste

Multi-Matrix System ! Biological (Patterson Jr., CDC) ! Environmental (Rivera, Spain) ! Food (De Pauw, Belgium)

DIOXIN SYMPOSIUM BREMEN

PCDD/Fs and PCBs in Foodstuff ! 95% of intake is via food ! Dioxins are located in fat ! Norm PCDD/Fs = 5 pg I-TEQ/g fat ! Norm PCBs = 200 ng/g fat DIOXIN SYMPOSIUM BREMEN

Solid Samples (Meat, fish, dairy fat, eggs, …)

DIOXIN SYMPOSIUM BREMEN

Lipids Isolation ! Sample Homogenisation (liquid N2) ! Freeze-drying (overnight) ! Grinding ! ASE extraction (overnight) ! Lipids determination and spiking DIOXIN SYMPOSIUM BREMEN

Background Levels Matrix

Levels pg I-TEQ/g fat

Pork Horse Beef Poultry Eggs (yolk)

0.1 – 0.3 4.5 – 14 0.8 – 1.5 0.5 – 1.0 1.5 – 7.0 DIOXIN SYMPOSIUM BREMEN

Required Amount of Fat Very low level of contamination (≤ 0.1 ppt)

+

LOQ (GC/IDHRMS) ≈ 0.1 ppt and recoveries