1 Scope
This document is applicable to the determination of polychlorinated dibenzo-p-dioxins
(PCDDs), polychlorinated dibenzofurans (PCDFs), (together termed ‘dioxins’ (PCDD/Fs))
and dioxin-like PCBs and non-dioxin-like PCBs (dl-PCBs and ndl-PCBs) in animal feeding
stuffs. Collaborative studies have been carried out. The method is suitable for the
determination of dioxins, dl-PCBs and ndl-PCBs at the appropriate MRL in compound
feed and ingredients e.g. oil, mineral clay. The method is applicable to samples containing
trace level amounts of one or more dioxins, dioxin-like PCBs and non-dioxin-likePCBs.
The limit of quantification (LOQ) is
-
— 0,05 pg/g (OCDD/F = 0,1 pg/g) for the relevant individual congeners of dioxins/furans,
-
— 0,05 pg/g for non-ortho PCBs,
-
— 10 pg/g for mono-ortho PCBs, and
-
— 100 pg/g for non-dioxin-like-PCBs.
For determination of dioxins and dioxin-like PCBs, the procedure can be used as confirmatory
method as defined by Commission Regulation (EC) No 152/2009 for dioxins and dl-PCB
in feed [1]. Confirmatory methods as described in this standard are high-resolution gas chromatography/high
resolution mass spectrometry (HRGC/HRMS) methods. If only the analysis of non-dioxin-like
PCBs is required, a GC-LRMS method can be used (e.g. EN 15741 [2]) provided that appropriate analytical performance criteria are met in the relevant
range for the matrix of interest.
This document is split into four modules. Each module describes a part of the whole
procedure (see Figure 1 and Figure 2) to be followed:
-
a) Module A: Description of standards which might be used;
-
b) Module B: Description of extraction procedures;
-
c) Module C: Description of clean-up procedures;
-
d) Module D: GC/HRMS determination.
Each module describes a part of the whole method as well as, when applicable, alternatives
which should be equivalent. Each module has to be regarded as an example. Combining
modules and/or alternatives gives a highly flexible, “performance based” procedure.
It is permitted to modify the method if all performance criteria laid down in Commission Regulation (EC) No 152/2009
[1] are met.
Any deviation of the described method, combination of modules needs to be recorded
as part of the QA/QC procedures of accredited laboratories and should be available
on request.
