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Commission Regulation (EC) No 152/2009 of 27 January 2009 laying down the methods of sampling and analysis for the official control of feed (Text with EEA relevance)
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The requirements set out in this Chapter shall be applied where feed is analysed for the official control of the levels of non-dioxin-like PCBs and as regards sample preparation and analytical requirements for other regulatory purposes, which includes the controls performed by the feed business operator to ensure compliance with the provisions of Regulation (EC) No 183/2005.
Gas chromatography/Electron Capture Detection (GC-ECD), GC-LRMS, GC-MS/MS, GC-HRMS or equivalent methods.
Monitoring of at least the following number of molecular ions or characteristic ions from the molecular cluster:
two specific ions for HRMS;
three specific ions for LRMS;
two specific precursor ions, each with one specific corresponding transition product ion for for MS-MS.
Maximum permitted tolerances for abundance ratios for selected mass fragments:
Relative deviation of abundance ratio of selected mass fragments from theoretical abundance or calibration standard for target ion (most abundant ion monitored) and qualifier ion(s): ± 15 %
Results exceeding the maximum level shall be confirmed with two GC columns with stationary phases of different polarity.
The performance of the method shall be validated in the range of the maximum level (0,5 to 2 times the maximum level) with an acceptable coefficient of variation for repeated analysis (see requirements for intermediate precision in point (9).
The sum of the LOQs(2) of non-dioxin-like PCBs shall not be higher than one-third of the maximum level(3).
Regular blank controls, analysis of spiked samples, quality control samples, participation in inter-laboratory studies on relevant matrices.
Addition to products (before extraction and clean-up process).
results shall be corrected for recoveries of internal standards;
recoveries of isotope-labelled internal standards shall be between 60 and 120 %;
lower or higher recoveries for individual congeners with a contribution to the sum of non-dioxin-like PCBs below 10 % are acceptable.
recovery of internal standard(s) shall be controlled for every sample;
recoveries of internal standard(s) shall be between 60 and 120 %;
results shall be corrected for recoveries of internal standards.
In accordance with the provisions of [F2Regulation (EU) 2017/625], laboratories shall be accredited by a recognised body operating in accordance with ISO Guide 58 to ensure that they are applying analytical quality assurance. Laboratories shall be accredited following the EN ISO/IEC 17025 standard. In addition, the principles as described in Technical Guidelines for the estimation of measurement uncertainty and limits of quantification for PCB analysis shall be followed when applicable(4).
Textual Amendments
F2Words in Annex 5 Pt. B Ch. 3 point 8 substituted (31.12.2022) by The Food and Feed (Miscellaneous Amendments) Regulations 2022 (S.I. 2022/1351), regs. 1(1), 16(6)(c)(i)
a Use of all six 13 C-labelled analogues as internal standards required. | ||
Isotope dilution mass spectrometry a | Other techniques | |
---|---|---|
Trueness | – 20 to + 20 % | – 30 to + 30 % |
Intermediate precision (RSD %) | ≤ 15 % | ≤ 20 % |
Difference between upper and lower-bound calculation | ≤ 20 % | ≤ 20 % |
Textual Amendments
F3Words in Annex 5 Pt. B Ch. 3 point 10.5 substituted (31.12.2022) by The Food and Feed (Miscellaneous Amendments) Regulations 2022 (S.I. 2022/1351), regs. 1(1), 16(6)(c)(ii)
Textual Amendments
[F1Congeners often found to co-elute are for example PCB 28/31, PCB 52/69 and PCB 138/163/164. For GC-MS also possible interferences from fragments of higher chlorinated congeners shall be considered.]
[F1The principles as described in the ‘ Guidance Document on the Estimation of LOD and LOQ for Measurements in the Field of Contaminants in Feed and Food ’ (http://ec.europa.eu/food/safety/animal-feed_en) shall be followed when applicable.]
[F1It is highly recommendable to have a lower contribution of the reagent blank level to the level of a contaminant in a sample. It is in the responsibility of the laboratory to control the variation of blank levels, in particular, if the blank levels are subtracted.]
[F1Current requirements are based on the TEFs published in: M. Van den Berg et al, Toxicol Sci 93(2), 223–241 (2006).]
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