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Method Validation and Verification
Method Validation and Verification
verification
W. W. Wong
Senior Accreditation Officer
HKAS
29 July 2009
What is it?
When is it required?
Why is it necessary?
What are required?
How much is adequate?
How should it be done?
Any questions on the questions?
2
Samples
Proficiency testing
Reference materials
Validated methods
Method Verification
ISO/IEC 17025 cl. 5.4.2
The laboratory shall confirm that it can
properly operate standard methods before
introducing the tests or calibrations. If the
standard method changes, the confirmation
shall be repeated.
Laboratory
requirement
Verification
(Secondary
validation)
Validation
Validation
(Primary validation)7
Method verification
Released early 2008
http://www.aoac.org/al
acc_guide_2008.pdf
Method Verification
10
Method Verification
Standard methods shall be verified for:
1. the equipment
2. the required
reagents
reference
materials/standard,
11
Method Verification
To demonstrate you can repeat the method
performance, including:
Detection limits
Precision
Bias
12
Method Verification
Method detection limit
Method Verification
Method detection limit
Factors to consider:
How many matrices are needed?
How are the values obtained compared with
those of the standard method?
14
0%
10
0%
Method Verification
%F
AT
IN
TE
RO
%P
0%
0%
10
100%
0%
%CARBOHYDRATES
15
J. AOAC, 83 (2), 413 (2000)
The Referee, AOAC Intl, July 1993
Method Verification
Method detection limit
How many food matrices are needed?
Less than validation
Professional judgment needed on the possible
matrix effects on the detection limits
Most difficult food matrices
How far can the light shine?
16
Method Verification
Method detection limit
How are the values obtained compared with those
of the standard method?
RSD not significantly different from std
method and
Mean recovery within acceptable limits
17
Method Verification
Precision
18
Method Verification
Precision
- comparison of precision of the two methods
2
r
2
r
S B
F=
S A
where S r2 B =
repeatability
std
dev
of
lab
2
r
19
Method Verification
Precision
- comparison of precision obtained against the
required value
The precision of the measurement process is assessed
by comparing the within-laboratory std dev under
repeatable conditions with the required value of the
within-lab std dev
20
Method Verification
Precision
- Compute
= { sw/wo}2
2
c
distribution at degrees of
freedom (n-1) divided by the degree of freedom (n-1)
21
Method Verification
Precision
- Decision
2
2
c table : No evidence that the
process is not as precise as required.
22
Method Verification
Bias
23
Method Verification
Bias
Method Verification
Bias
2
2
2
Given sR = sL + sr
2
2
2
2
sD = sR - sr + sw /n
Hence,
< 2 (sR2 - sr2 + sw2/n)
25
Method Verification
Bias
Method Verification
Bias
Thank you
28