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International Federation forConsulting GmbH IFC

TheTheCommission Decision Commission Decision

2002/657/EC2002/657/ECPerformance criteriaPerformance criteria

by

Dr. Michael Scheutwinkel

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Content of Annex of CD 2002/657/EC

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 requirements2.1 General requirements

Sample handlingSample handling Test performanceTest performance

SpecifitySpecifity

Recovery with each batch of samples

Recovery with each batch of samples

Maximum chance for the detection

of the analyte

Maximum chance for the detection

of the analyte

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Performance criteria according to CD 2002/657/EC

2.2 Screening methods2.2 Screening methods

False compliant rate < 5 % (β-error)

False compliant rate < 5 % (β-error)

In case of a suspected non-compliant result,

a confirmation is obligatory.

In case of a suspected non-compliant result,

a confirmation is obligatory.

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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 -----

Suitable confirmatory methods according to

CD 2002/657/EC, here only extract

Table 1

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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

2.3 Confirmatory methods for analysis of organics, common requirements

No discrimination in cases that two compounds give same response,

only chromatographic analysis without spectrometric

detection is not appropriate.

No discrimination in cases that two compounds give same response,

only chromatographic analysis without spectrometric

detection is not appropriate.

Use of internal standard

or confirmation by co-chromatogaphy

Use of internal standard

or confirmation by co-chromatogaphy

Use of CRMor fortification of

material

Use of CRMor 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

2.3 Confirmatory methods for analysis of organics, specific requirements

Minimum trueness(Table 2)

Minimum trueness(Table 2)

Reproducibility CV(%)(Table 3)

Reproducibility CV(%)(Table 3)

CV = interlaboratory coefficient

of variation in %

CV = interlaboratory coefficient

of variation in %MRL existing?

CV = 50% of limitMRL existing?

CV = 50% of limit

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Table 2

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Performance criteria according to CD 2002/657/EC

Confirmatory methods for analysis of organics,performance criteria for MS

Confirmatory methods for analysis of organics,performance criteria for MS

Chromatographicseparation

Chromatographicseparation

MS detectionMS detection

Usually full scan,< 10% deviation

from reference MS

Usually full scan,< 10% deviation

from reference MS

Full scan + SIM see table 4

Full scan + SIM see table 4

SIM S/N ratio > 3:1

SIM S/N ratio > 3:1

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LC with differentdetection techniques

LC with differentdetection techniques

2-D TLC coupled to full-scan UV/VIS

spectrometricdetection

2-D TLC coupled to full-scan UV/VIS

spectrometricdetection

Chromatography coupled to

infrared detection

Chromatography coupled to

infrared detection

2.3 Confirmatory methods for organics, performance criteria2.3 Confirmatory methods for organics, performance criteria

GC-ECDGC-ECD

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Table 5

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Commission Decision 2002/657/EC Table 6

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Table 4

Performance criteria according to CD 2002/657/EC

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Commission Decision 2002/657/EC Table 6

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Differential pulse anodicstrippingvoltametry

Differential pulse anodicstrippingvoltametry

ICP-AESICP-AES

Trueness of quantitative tests

Trueness of quantitative tests

2.4 Confirmatory methods for elements, see also table 7

2.4 Confirmatory methods for elements, see also table 7

AASAAS

ICP-MSICP-MS

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Table 8