Commission Regulation (EC) No 152/2009Show full title

[F1 CHAPTER III U.K. Sample preparation and requirements for methods of analysis used in official control of the levels of non-dioxin-like PCBs (PCB # 28, 52, 101, 138, 153, 180)

1. Applicable detection methods U.K.

Gas chromatography/Electron capture detection (GC/ECD), GC/LRMS, GC/MS-MS, GC/HRMS or equivalent methods.

2. Identification and confirmation of analytes of interest U.K.

2.1. Relative retention time in relation to internal standards or reference standards (acceptable deviation of +/– 0,25 %). U.K.

2.2. Gas chromatographic separation of all six indicator PCBs (PCB 28, PCB 52, PCB 101, PCB 138, PCB 153 and PCB 180) from interfering substances, especially co-eluting PCBs, in particular if levels of samples are in the range of legal limits and non-compliance is to be confirmed. U.K.

Note: Congeners 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. U.K.

2.3. Requirements for GC/MS techniques U.K.

Monitoring of at least:

(a)

two specific ions for HRMS;

(b)

two specific ions of m/z > 200 or three specific ions of m/z > 100 for LRMS;

(c)

1 precursor and 2 product ions 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):

a Sufficient number of mass fragments with relative intensity > 10 % available, therefore not recommendable to use qualifier ion(s) with a relative intensity of less than 10 % compared to the target ion.
Relative intensity of qualifier ion(s) compared to target ion	GC-EI-MS (relative deviation)	GC-CI-MS, GC-MS n (relative deviation)
> 50 %	± 10 %	± 20 %
> 20 % to 50 %	± 15 %	± 25 %
> 10 % to 20 %	± 20 %	± 30 %
≤ 10 %	± 50 % a	± 50 % a

2.4. Requirements for GC/ECD techniques U.K.

Results exceeding the tolerance shall be confirmed with two GC columns with stationary phases of different polarity.

3. Demonstration of performance of method U.K.

The performance of the method shall be validated in the range of the level of interest (0,5 to 2 times the level of interest) with an acceptable coefficient of variation for repeated analysis (see requirements for intermediate precision in point 8).

4. Limit of quantification U.K.

The blank values shall not be higher than 30 % of the level of contamination corresponding to the maximum level (1) .

5. Quality control U.K.

Regular blank controls, analysis of spiked samples, quality control samples, participation in inter-laboratory studies on relevant matrices.

6. Control of recoveries U.K.

6.1. Suitable internal standards with physico-chemical properties comparable to analytes of interest shall be used. U.K.

6.2. Addition of internal standards: U.K.

Addition to products (before extraction and clean-up process).

6.3. Requirements for methods using all six isotope-labelled indicator PCB congeners: U.K.

(a)

results shall be corrected for recoveries of internal standards;

(b)

recoveries of isotope-labelled internal standards shall be between 50 and 120 %;

(c)

lower or higher recoveries for individual congeners with a contribution to the sum of the six indicator PCBs below 10 % are acceptable.

6.4. Requirements for methods using not all six isotope-labelled internal standards or other internal standards: U.K.

(a)

recovery of internal standard(s) shall be controlled for every sample;

(b)

recoveries of internal standard(s) shall be between 60 and 120 %;

(c)

results shall be corrected for recoveries of internal standards.

6.5. The recoveries of unlabelled congeners shall be checked by spiked samples or quality control samples with concentrations in the range of the level of interest. Recoveries for these congeners shall be considered acceptable, if they are between 70 and 120 %. U.K.

7. Requirements for laboratories U.K.

In accordance with the provisions of Regulation (EC) No 882/2004, 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.

8. Performance characteristics: criteria for the sum of the six indicator PCBs at the level of interest U.K.

Trueness	– 30 to + 30 %
Intermediate precision (RSD%)	≤ 20 %
Difference between upper- and lower-bound calculation	≤ 20 %

9. Reporting of the results U.K.

9.1. In so far as the used analytical procedure makes it possible, the analytical results shall contain the levels of the individual PCB congeners and be reported as lower-bound, upper-bound and medium-bound in order to include a maximum of information in the reporting of the results and thereby enabling the interpretation of the results according to specific requirements. U.K.

9.2. The report shall include the method used for extraction of PCBs and lipids. U.K.

9.3. The recoveries of the individual internal standards shall be made available in case the recoveries are outside the range referred to in point 6, in case the maximum level is exceeded and in other cases upon request. U.K.

9.4. As the uncertainty of measurement is to be taken into account when deciding about the compliance of a sample, this parameter shall also be made available. Thus, analytical results shall be reported as x +/- U whereby x is the analytical result and U is the expanded measurement uncertainty using a coverage factor of 2 which gives a level of confidence of approximately 95 %. U.K.

9.5. If the uncertainty of measurement is taken into account by applying CCα (as described in point 2.1 of Chapter I), this parameter shall be reported. U.K.

9.6. The results shall be expressed in the same units and with at least the same number of significant figures as the maximum levels laid down in Directive 2002/32/EC.] U.K.

Textual Amendments

F1 Substituted by Commission Regulation (EU) No 278/2012 of 28 March 2012 amending Regulation (EC) No 152/2009 as regards the determination of the levels of dioxins and polychlorinated biphenyls (Text with EEA relevance).

(1)

[F1 It 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.]

Textual Amendments

F1 Substituted by Commission Regulation (EU) No 278/2012 of 28 March 2012 amending Regulation (EC) No 152/2009 as regards the determination of the levels of dioxins and polychlorinated biphenyls (Text with EEA relevance).