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Evolution in the Sample Preparation for the Measurement of POPs in Biological Matrices. J.-F. Focant. MS Laboratory Organic and Biological Anal. Chem. Human Exposure?. Non-occupational exposure (adults) > 90\% due to food Invasive unpopular human biomonitoring

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slide1
Evolution in the Sample Preparation for the Measurement of POPs in Biological Matrices

J.-F. Focant

MS Laboratory

Organic and Biological Anal. Chem.

slide2
Human Exposure?
  • Non-occupational exposure (adults)
  • > 90% due to food
  • Invasive unpopular human biomonitoring
        • analyses of foodstuffs (feed, …)
  • Analyticaly challenging…
slide3
A ‘Good’ Kick…

Coût : 400 106 € (0.21% PIB)

1 gouvernement

Time axis

Focant and De Pauw, Les Dioxines. La Recherche323 (1999) 84.

Cost : 1 government and 1-2 billions €…

7 106 chickens & 50,000 pigs slaughtered

slide4
EU Commission Strategy (food-feed)
  • Maximum levels set as ALARA
  • MRL strategy(SANCO/11248/2011 & 11515/2011)
  • Uniform sampling and analysis criteria
  • Comprehensive & reliable data

Robust tools needed…

slide5
Analytical Criteria
  • Commission Regulation 1883/2006
  • Commission Regulation 152/2009
  • EPA1613B
  • prEN16215 (feed)
      • PBMS (different modules)
      • Module B: Extraction
      • Module C: Clean-up

Manual

or

automated

slide6
Today’s Capacity
  • D+1 Fat matrices (regular input)
  • D+3 Feed matrices (regular input)
  • D+5 All matrices (irregular input)
slide9
Parallel PLE

Extraction,

solventreduction and exchange

slide10
Automated PLE

70-85 min.

+ 5-25 min wash time = 75-110 min cycle time

slide12
Traceability of Events

P(psi)

T(C)

1800

150

1500

125

Heat & Pressurize Cool & Depressurize

0

0

27 37 45

Time

(min.)

Pressure: Chan. 1

Chan. 2

Chan. 3

Temperature: Chan. 1

Chan. 2

Chan. 3

slide15
Online Solvent Reduction
  • 6 lines system
  • N2 flow
  • T prog.
  • No water bath
  • Solvent exchange
  • Dustfilter in
slide16
PLE Properties
  • Stand-alone automated parallel system
  • Up to 6 samples at a time (modular)
  • 1.8h / 6 samples (cycle time)
  • Wide bore plumbing (no pump cavitation)
  • PLE is an ‘old’ and proven concept
  • Robust and versatile (various cell sizes)
  • Easily usable under QA/QC requirements
  • Good throughput / cost effectiveness ratio
slide19
1) Hexane 90ml

2) 50:50 100ml

Waste

3) Hexane 10ml

PCBs

Waste

4) Toluene

Extract in hexane (20 ml)

Silica

Alumina

PCDD/Fs & NO-PCBs

Carbon

slide20
Automated Clean-up

75 min.

+ 15 min wash time = 90 min cycle time

slide23
Previous generation

Current generation

slide24
Previous

generation

Current

generation

Previous

generation

Current

generation

slide25
Tracability by Lot #
  • Good stability
  • Good lot-to-lot reproducibility
  • ‘PCB-free’ , ‘PBDE-free’ columns…
slide26
Natural Spray Dried Milk

Experiment

CR values

10.5±2.4

26.2±0.4

4.8±0.4

BCR-607 (n=3)

(PCDD/Fs + cPCBs in ppt, other PCBs in ppb)

RSDs < 20% Recovery rates inside EU Directive range

slide27
QC Serum Samples

(n=4)

(PCDD/Fs + cPCBs in ppt, other PCBs in ppb)

RSDs < 10% Recovery rates in the high 60% range

slide28
Online Solvent Reduction
  • 100 mL Hx/DCM to 500 µL
  • 80 mL toluene to 500 µL
  • Nitrogen flow
  • 30°C, heating metal block
slide30
Sample Clean-up Properties
  • Stand-alone automated parallel system
  • Up to 6 samples at a time (modular)
  • 1.5h / 6 samples (cycle time)
  • Disposable Si, Al, and C
  • 20 year old concept, many revisions since then
  • Robust and versatile (various column sizes)
  • Easily usable under QA/QC requirements
  • Good throughput / cost effectiveness ratio
slide32
The Integrated Approach

13C spiking

Solvent exchange

Lipid

Determination

Keeper

Several fractions

PTV-LVI

PLE

Keep it open

SR-1

Clean-up & Fractionation

SR-2

GC-MS

slide33
Time Scale
  • Condition the clean-up system
  • Fill PLE cell
  • Heat and presurize
  • Cool, nitrogen purge to evaporator
  • Reduce volume (on the go)
  • Load on silica
  • Elute silica with hexane
  • Elute alumina with 50:50 (PCBs)
  • Back-elute carbon with toluene (D/Fs)

25 min

25 min

per cycle

30 min

40

min

Total time : 2 to 3h per sets of 6 samples in parallel

slide34
Same-Day Testing Capability
  • Sample preparation for PLE 0.5 h
  • Parallel PLE (2 cycles) 1.5 h
  • First solvent reduction 0.5 h
  • Parallel Clean-up and fractionation 2 h
  • Second solvent reduction 1.5 h
  • Std addition and transfer to GC 0.1 h
  • PTVLVI-GC-IDHRMS 1 h
  • QA/QC check and reporting 0.5 h
  • TOTAL ~ 8 h
slide35
The missing link (2009)...

PLE-Vap-PrepLC-GCxGC-PTVLVI-IDEIHRMS

slide36
The missing link (2012)...

Std addition & injection on

TriPlusTM Autosampler

slide37
What Next for Tomorrow ?
  • Dioxin testing is getting faster and more reliable
  • Confirmatory approach status changed…
  • Confirmatory not too far from screening…
  • EU strategy to be revisited ?
  • Focus on ‘better’ use of CALUX
slide38
Not to Forget…
  • Dioxin testing remains a task for chemists…
  • Keeping blank levels under control is crucial…
  • ‘Simplifying’ the MS side is one thing, keep
  • performing state-of-the-art sample preparation is
  • another one…
  • Fast and reliable does not mean trivial…
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