EN 15741:2009 – Foderstoffer – Bestemmelse af OC-pesticider og PCB ved GC/MS
1 Scope
This European Standard specifies a gas chromatographic/mass spectrometric method for the determination of organochlorine pesticides (OC’s) and polychlorinated biphenyls (PCBs) in animal feeding stuffs and oil.
The method is applicable to animal feeding stuffs with a water content up to about 20 wt% and oil/fatty samples containing residues of one or more of the following OC’s and PCBs and some of their isomers and degradation products:
Aldrin;
Dieldrin;
Chlordane (= sum of Chlordane isomers and Oxychlordane);
DDT (= sum of isomers op’-DDT, pp’-DDT, pp’-TDE (pp’-DDD), and pp’-DDE);
Endosulfan (sum of α-/β-isomers and Endosulfan-sulphate);
Endrin;
Heptachlor (= sum of Heptachlor and β-Heptachlorepoxide);
Hexachlorobenzene (HCB);
Hexachlorocyclohexane isomers α-HCH (α-BHC), β-HCH (β-BHC), γ-HCH (γ-BHC or lindane);
PCB 28, 52, 101, 138, 153 and 180 (“Indicator PCBs”) and PCB 198, 209.
The method is not yet applicable to Chlorocamphene (Toxaphene), a complex mixture of polychlorinated camphenes. Chlorocamphene has a very distinctive chromatographic profile and is easily recognisable by GC/ECD. Positive identification of the toxaphene isomers can be performed by negative chemical ionisation mass spectrometry (NCI-MS), electron impact tandem mass spectrometry (EI-MSxMS) or electron impact high resolution mass spectrometry (EI-HRMS) [1], which is not within the scope of this method.
The limit of quantification for the mentioned organochlorine pesticides and PCBs is 5 ng/g in general.
However, 10 ng/g applies for Heptachlor Aldrin, Endrin, Dieldrin, and Endosulfan (α-, β- and sulphate).
Individual laboratories are responsible to ensure that the equipment they used will achieve these limits of quantifications.
2 Normative references
The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.
ISO 6498, Animal feeding stuffs – Preparation of test samples
3 Terms and definitions
For the purpose of this document, the following terms and definitions apply.
3.1
limit of detection
smallest measured content, from which it is possible to deduce the presence of the analyte with reasonable statistical certainty
NOTE The limit of detection is numerically equal to three times the standard deviation of the mean of blank determinations (n>10).
3.2
limit of quantification
lowest content of the analyte which can be measured with reasonable statistical certainty
NOTE If both accuracy and precision are constant over a concentration range around the limit of detection, then the limit of quantification is numerically equal to 6 times the standard deviation of the mean of blank determinations (n>10).
3.3
feed Additives
substances are feed additives when they comply with the definition of feed additives given in the Regulation 1831/2003
EN 15741:2009 – Foderstoffer – Bestemmelse af OC-pesticider og PCB ved GC/MS