Validation

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The Commission Decision 2002/657/EC Performance
criteria by Dr. Michael Scheutwinkel
International Federation forConsulting GmbH IFC
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Content of Annex of CD 2002/657/EC
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1 Definitions 2 Performance
criteria and other requirements for
analytical methods 2.1 General criteria to
be fulfilled by any technique,
procedure, etc. 2.2 Criteria for screening
methods 2.3 Criteria for confirmatory
methods (organics) 2.4 Criteria for
confirmatory methods (elements) 3
Recommended valdidation procedures -
classical validation - alternative
validations, e.g. InterVal
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Performance criteria according to CD 2002/657/EC
2.1 General requirements
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Sample handling
Test performance
Maximum chance for the detection of the analyte
Recovery with each batch of samples
Specifity
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Commission Decision 2002/657/EC
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Performance criteria according to CD 2002/657/EC
2.2 Screening methods
In case of a suspected non-compliant result, a
confirmation is obligatory.
False compliant rate lt 5 (ß-error)
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Suitable confirmatory methods according to CD
2002/657/EC, here only extract
Table 1
Measuring technique Substances Annex I 96/23/EEC Limitations
LC or GC with MS Groups A and B Only if following either an on-line or off- line chromatographic separation Only if full scan technique are used or using at least 3 (group B) or 4 (group A) identification points for techniques that do not record the full mass spectra
LC-full-scan DAD Group B Specific requirements for absorption in UV spectrometry have to be met
Others -----
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Table 9
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Commission Decision 2002/657/EC
Table 10
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Performance criteria according to CD 2002/657/EC
2.3 Confirmatory methods for analysis of
organics, common requirements
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1
Use of internal standard or confirmation by
co-chromatogaphy
No discrimination in cases that two compounds
give same response, only chromatographic
analysis without spectrometric detection is not
appropriate.
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Use of CRM or fortification of material
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Performance criteria according to CD 2002/657/EC
2.3 Confirmatory methods for analysis of
organics, specific requirements
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2
Minimum trueness (Table 2)
Reproducibility CV() (Table 3)
CV interlaboratory coefficient of variation
in
MRL existing? CV 50 of limit
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Commission Decision 2002/657/EC
Table 3
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Commission Decision 2002/657/EC
Table 2
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Commission Decision 2002/657/EC
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Performance criteria according to CD 2002/657/EC
Confirmatory methods for analysis of
organics, performance criteria for MS
Chromatographic separation
MS detection
Usually full scan, lt 10 deviation from
reference MS
SIM S/N ratio gt 31
Full scan SIM see table 4
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2.3 Confirmatory methods for organics,
performance criteria
LC with different detection techniques
Chromatography coupled to infrared detection
GC-ECD
2-D TLC coupled to full-scan UV/VIS
spectrometric detection
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Commission Decision 2002/657/EC
Table 5
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Commission Decision 2002/657/EC
Table 6
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Performance criteria according to CD 2002/657/EC
Table 4
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Commission Decision 2002/657/EC
Table 6
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2.4 Confirmatory methods for elements, see also
table 7
Differential pulse anodic strippingvoltametry
Trueness of quantitative tests
AAS
ICP-AES
ICP-MS
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Table 7
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Table 8