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BS EN 16215:2020

BS EN 16215:2020

$198.66

Animal feeding stuffs: Methods of sampling and analysis. Determination of dioxins and dioxin-like PCBs by GC/HRMS and of indicator PCBs by GC/HRMS

Published By Publication Date Number of Pages
BSI 2020 58
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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:

  1. Module A: Description of standards which might be used;

  2. Module B: Description of extraction procedures;

  3. Module C: Description of clean-up procedures;

  4. 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.

PDF Catalog

PDF Pages PDF Title
2 undefined
8 1 Scope
10 2 Normative references
3 Terms and definitions
11 4 Principle
12 5 Reagents
5.1 General
5.2 Dioxins, furans, non-ortho PCBs, mono-ortho PCBs and non-dioxin-like PCBs and their labelled analogues
6 Apparatus
7 Sampling
13 8 Preparation of test sample
9 Procedure
9.1 General
9.2 Animal feed stuff sample and oil/fat sample
9.2.1 10 g animal feed stuff sample (12 % moisture content)
9.2.2 2,5 g oil/fat sample
10 Extraction
10.1 General
14 10.2 Module BI Extraction using automated Pressurized Fluid Extraction (PFE) system
15 10.3 Module BII: Manual extraction procedure
16 11 Clean-up
11.1 General
18 11.2 Module CI: Automated clean-up
21 11.3 Module CII: Manual sample clean-up, removal of fat and group separation
24 11.4 Additional clean-up-steps for fraction A and fraction B of module CII
26 11.5 Module CIII: Removal of matrix, manual sample clean-up and group separation
31 12 Module D: Gas chromatograph-high resolution mass spectrometer (GC-HRMS)
12.1 General
12.2 Reagents and materials
12.3 Procedure
33 13 Calculation and expression of results
13.1 General
13.2 Calibration by Isotope Dilution
13.3 Linearity
13.4 Calibration criteria
13.5 Identification and confirmation
34 13.6 Calculation
35 13.7 Toxic Equivalent (TEQ) values
38 13.8 Recovery
14 Precision
40 15 Test report
41 Annex A (informative)Description of PTV injection system
A.1 Large volume injection (100 µl) – GC-HRMS Calibration mixtures dioxins and non-ortho PCBs
42 A.2 Sample preparation procedure
A.3 PTV injection conditions using 100 µl injection
43 Annex B (informative)Description of standards and concentration of the standard solutions
B.1 CAS Registry numbers for dioxins, furans, non-ortho PCBs, mono-ortho PCBs and non-dioxin-like PCBs and their labelled analogues
44 B.2 Standard solutions
B.2.1 13C-1,2,3,4-TCDD (50 µg/ml)
B.2.2 13C-1,2,3,6,7,8-HxCDF (50 µg/ml)
B.2.3 37Cl4-2,3,7,8 TCDD (50 µg/ml)
B.2.4 Mixture 13C-PCDD (1 µg/ml)
B.2.5 Mixture 13C-PCDF (1 µg/ml)
B.2.6 Mixture TCDD-HpCDD (5 µg/ml)
B.2.7 Mixture TCDF-HpCDF (5 µg/ml)
B.2.8 OCDD (10 µg/ml)
45 B.2.9 OCDF (50 µg/ml)
B.2.10 OCDF standard (5 µg/ml)
B.2.11 Mixture 13C-non-ortho PCBs (1 µg/ml)
B.2.12 Mixture 13C-mono-ortho PCBs (1 µg/ml)
B.2.13 Mixture 13C-non-dioxin-like PCBs (5 µg/ml)
B.2.14 Mixture non-ortho PCBs (10 µg/ml)
B.2.15 Mixture mono-ortho PCBs (10 µg/ml)
B.2.16 Commercially available mixture non-dioxin-like PCBs (10 µg/ml)
B.2.17 Recovery standard DIOX-RS-100 (100 pg/µl 13C-1,2,3,4-TCDD and 100 pg/µl 13C-1,2,3,6,7,8-HxCDF in toluene)
B.2.18 Recovery standard DIOX-RS-1 (1,0 pg/µl 13C-1,2,3,4-TCDD, 1,0 pg/µl 13C-1,2,3,6,7,8-HxCDF in toluene)
46 B.2.19 Recovery standard TCDD-RS-III (100 pg/µl 13C-1,2,3,4-TCDD in iso-octane)
B.2.20 Recovery standard TCDD-RS-VI (25 pg/µl 13C-1,2,3,4-TCDD in iso-octane)
B.2.21 Clean-up standard CS-50 (50 pg/µl 37Cl4-2,3,7,8-TCDD in toluene)
B.2.22 Clean-up standard CS-1 (1,0 pg/µl 37Cl4-2,3,7,8-TCDD in toluene)
B.2.23 Mixture non-ortho PCBs (NOP-500) (500 pg/µl in toluene)
B.2.24 Mixture PCDD/F and non-ortho PCBs (DIOXNOP) (20 pg/µl in toluene)
B.2.25 Mixture PCDD/F and non-ortho PCBs (DIOXNOP-1) (2,0 pg/µl in toluene)
B.2.26 Mixture mono-ortho PCBs and indicator PCBs (MOPIP-500) (500 pg/µl in iso-octane)
B.2.27 Mixture mono-ortho PCBs and indicator PCBs (MOPIP-25) (25 pg/µl in iso-octane)
47 B.2.28 Mixture mono-ortho PCBs and indicator PCBs (MOPIP-2,5) (2,5 pg/µl in iso-octane)
B.2.29 Mixture mono-ortho PCBs and indicator PCBs (MOPIP-,.25) (0,25 pg/µl in iso-octane)
B.2.30 Mixture 13C-PCDD/F and 13C-non-ortho PCBs (13C-DIOXNOP) (50 pg/µl in toluene)
B.2.31 Mixture 13C-PCDD/F and 13C-non-ortho PCBs (13C-DIOXNOP-2) (0,10 pg/µl in toluene)
B.2.32 Mixture 13C-mono-ortho PCBs and 13C-indicator PCBs (13C-MOPIP-1) (50 pg/µl in iso-octane)
B.2.33 Mixture 13C-mono-ortho PCBs and 13C-indicator PCBs (13C-MOPIP-2) (2,0 pg/µl in iso-octane)
B.3 GC-standard solutions
B.3.1 Standard dioxins and non-ortho PCBs mixtures
48 B.3.2 Preparation mono-ortho PCBs standard mixtures.
50 Annex C (informative)Example of automated procedure
52 Annex D (informative)Mass spectrometer (MS)
56 Annex E (informative)Use of additional clean-up after fractionation using a small multi-layer silica column
E.1 Preparation of the silica mixtures
E.2 Preparation of the small multi-layer column

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BS EN 16215:2020
$198.66