Document #: QA/SOP/001-A SOP for Analytical Method Validation
Revision No: 00
Issue No:02
For internal use only.
Do not duplicate.
PURPOSE: To provide guidelines for the validation of non-standard or modified methods for
laboratory analysis.
SCOPE: This procedure is applicable to the analysis of samples using methodologies that are not
established by the USP, BP, EP, JP, P or any other Pharmacopoeia.
RESPONSIBILITY:
The !uality "ssurance #anager is responsible for determining the level of validation
re$uired for each analytical method.
Each analyst is responsible for generation of data by the specific instructions of the
!uality "ssurance #anager%!uality &ontrol #anager
The analyst is also responsible for the initial revie' of the data pac(age.
The !uality "ssurance #anager%!uality &ontrol #anager is responsible for secondary
revie' of the data pac(age to assure that the analytical methodology used is validated
by the instruction of this S)P.
PROCEDURE:
Prior to initiating a validation study, the pre-validation activities and subse$uent development
report should be completely covered in the Specific method validation protocol. The method
validation protocol outline is as follo's*
+. TT,E )- #ET.)/
a. "uthor0s 1ame and Title
b. /epartment
c. Signature and /ate
2. "PP3)4",S
a. 1ames and Titles
b. /epartment
c. Signature and /ate
5. S&)PE )- #ET.)/
6rite the ob7ective8 a simple statement of 'hat the protocol 'ill accomplish
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Document #: QA/SOP/001-A SOP for Analytical Method Validation
Revision No: 00
Issue No:02
For internal use only.
Do not duplicate.
9. 4",/"T)1 P"3"#ETE3S
The actual parameters 'ill be comprised from a subset of the belo' list based on the intended
use of the method. Each re$uirement selected for in a given validation protocol should be
follo'ed 'ith detailed strategy 'hich 'ill be used to test for the parameter including the format
of data tables, sampling scheme, sample si:e and formulas for intended calculations.
a. Specificity
b. ,inearity
c. Precision
d. "ccuracy
e. 3uggedness
;. E!UP#E1T
This section should provide all information for the use of the e$uipment or other apparatus
necessary to conduct all aspects of the method.
<. 3E"=E1TS
This section should list all the reagents and their preparation >'here necessary? used to
conduct the method.
@. S"#P,ES
This section should list all the samples, their type, and their preparation >'here necessary?.
>e.g. ra' materials, in-process materials, finished goods or stability samples?
A. P3)&E/U3E
This section should contain all information applicable and relative to the sample, standard and
blan( preparation >eBtraction, dilution etc?, instrument parameters, determination and
calculations
a. Sample preparation
i. EBtraction
ii. /ilution
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Document #: QA/SOP/001-A SOP for Analytical Method Validation
Revision No: 00
Issue No:02
For internal use only.
Do not duplicate.
iii. )ther
b. Standard Preparation
i. EBtraction
ii. /ilution
iii. )ther
c. Blan( Preparation
d. nstrument )perating Parameters
i. nstruments
ii. )perating conditions
+. &olumns
2. Temperature
5. 6avelength
9. Special &alibration
;. )ther
iii. /eterminative step
iv. &alculations >all dilution factors and calculation parameters should be clearly
eBplained?
C. E4",U"T)1 &3TE3"
Specifications or specific values establishing acceptance criteria for each validation parameter
tested for.
+D. 3E-E3E1&ES
4",/"T)1 SU##"3E 3EP)3T
Subse$uent to the eBecution of the protocol, the data must be analy:ed 'ith results, conclusions and
deviations presented in an official validation summary report. The method can be considered valid
provided that all pre-defined acceptance criteria is met and the deviation >if any? do not affect the
scientific interpretation of the data. " statement of the methods validation status should be placed at
the beginning of the final validation summary report, along 'ith signatures, dates and titles of all the
participants and revie'ers.
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