4.Method of analysis to be used by the laboratory and laboratory control requirements
4.1.Definitions
A number of the most commonly used definitions that the laboratory will be required to use are given below:
r
=
Repeatability, the value below which the absolute difference between two single test results obtained under repeatability conditions (i.e., same sample, same operator, same apparatus, same laboratory, and short interval of time) may be expected to lie within a specific probability (typically 95 %) and hence
.
sr
=
Standard deviation, calculated from results generated under repeatability conditions.
RSDr
=
Relative standard deviation, calculated from results generated under repeatability conditions
.
R
=
Reproducibility, the value below which the absolute difference between single test results obtained under reproducibility conditions (i.e., on identical material obtained by operators in different laboratories, using the standardised test method), may be expected to lie within a certain probability (typically 95 %);
.
sR
=
Standard deviation, calculated from results under reproducibility conditions.
RSDR
=
Relative standard deviation calculated from results generated under reproducibility conditions
, where
is the average of results over all laboratories and samples.
HORRATr
=
the observed RSDr divided by the RSDr value estimated from the Horwitz equation (1) using the assumption r = 0.66R.
HORRATR
=
the observed RSDR value divided by the RSDR value calculated from the Horwitz equation.
U
=
the expanded uncertainty, using a coverage factor of 2 which gives a level of confidence of approximately 95 %.
4.2.General requirements
Methods of analysis used for food control purposes must comply with points 1 and 2 of the Annex to Council Directive 85/591/EEC.
4.3.Specific requirements
Where no specific methods for the determination of benzo(a)pyrene in food are prescribed at Community level, laboratories may select any validated method provided the selected method meets the performance criteria indicated in the Table. The validation should ideally include a certified reference material.
TABLE
Performance criteria for methods of analysis for benzo(a)pyrene
Parameter | Value/comment |
---|
Applicability | Food specified in Regulation (EC) No …/2005 |
Detection limit | No more than 0,3 μg/kg |
Limit of quantification | No more than 0,9 μg/kg |
Precision | HORRATr or HORRATR values of less than 1.5 in the validation collaborative trial |
Recovery | 50 %-120 % |
Specificity | Free from matrix or spectral interferences, verification of positive detection |
4.3.1.Performance Criteria — Uncertainty Function Approach
However, an uncertainty approach may also be used to assess the suitability of the method of analysis to be used by the laboratory. The laboratory may use a method which will produce results within a maximum standard uncertainty. The maximum standard uncertainty can be calculated using the following formula:
where:
Uf
is the maximum standard uncertainty
LOD
is the limit of detection of the method
C
is the concentration of interest
If an analytical method provides results with uncertainty measurements less than the maximum standard uncertainty the method will be equally suitable to one which meets the performance characteristics given in the Table.
4.4.Recovery calculation and reporting of results
The analytical result is to be reported corrected or uncorrected for recovery. The manner of reporting and the level of recovery must be reported. The analytical result corrected for recovery is used for checking compliance (see Annex I, point 5).
The analyst should note the ‘European Commission Report on the relationship between analytical results, the measurement of uncertainty, recovery factors and the provisions in EU food legislation’ (2).
The analytical result has to be reported as x +/– U whereby x is the analytical result and U is the measurement uncertainty.
4.5.Laboratory quality standards
Laboratories must comply with Directive 93/99/EEC.
4.6.Other considerations for the analysis
Proficiency testing
Participation in appropriate proficiency testing schemes which comply with the ‘International Harmonised Protocol for the Proficiency Testing of (Chemical) Analytical Laboratories’ (3) developed under the auspices of IUPAC/ISO/AOAC.
Internal quality control
Laboratories should be able to demonstrate that they have internal quality control procedures in place. Examples of these are the ‘ISO/AOAC/IUPAC Guidelines on Internal Quality Control in Analytical Chemistry Laboratories’ (4).