Transcript Validation - Instituto Nacional de Metrologia

The
Commission Decision
2002/657/EC
Performance criteria
by
Dr. Michael Scheutwinkel
International Federation for
Consulting GmbH IFC
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Content of Annex of CD 2002/657/EC
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Definitions
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Performance criteria and other requirements for
analytical methods
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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)
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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
2
1
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
False compliant rate
< 5 % (β-error)
In case of a suspected
non-compliant result,
a confirmation is
obligatory.
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Suitable confirmatory methods according to
Table 1
CD 2002/657/EC, here only extract
Substances
Annex I
96/23/EEC
Limitations
LC or GC
with MS
Groups A
and B
- Only if following either an on-line or offline 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
Measuring
technique
Others
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Commission Decision 2002/657/EC
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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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
internal standard
or confirmation by
co-chromatogaphy
3
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,
< 10% deviation
from reference MS
Full scan + SIM
see table 4
SIM
S/N ratio > 3:1
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Commission Decision 2002/657/EC
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Commission Decision 2002/657/EC
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2.3 Confirmatory methods for
organics, performance criteria
Chromatography
coupled to
infrared detection
LC with different
detection techniques
GC-ECD
2-D TLC coupled
to full-scan UV/VIS
spectrometric
detection
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Commission Decision 2002/657/EC
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Commission Decision 2002/657/EC
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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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Commission Decision 2002/657/EC
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Commission Decision 2002/657/EC
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2.4 Confirmatory methods for elements,
see also table 7
Trueness of
quantitative tests
Differential pulse anodic
strippingvoltametry
AAS
ICP-AES
ICP-MS
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Table 7
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Commission Decision 2002/657/EC
Table 8
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