SOP for Analytical Method

Document #: QA/SOP/001-A
Validation
Revision No: 00 For internal use only.
Issue No:02 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, IP or any other Pharmacopoeia.

RESPONSIBILITY:

 The Quality Assurance Manager is responsible for determining the level of validation

required for each analytical method.

 Each analyst is responsible for generation of data by the specific instructions of the

Quality Assurance Manager/Quality Control Manager

 The analyst is also responsible for the initial review of the data package.

 The Quality Assurance Manager/Quality Control Manager is responsible for secondary

review of the data package to assure that the analytical methodology used is validated

by the instruction of this SOP.

PROCEDURE:

Prior to initiating a validation study, the pre-validation activities and subsequent development

report should be completely covered in the Specific method validation protocol. The method

validation protocol outline is as follows:

1. TITLE OF METHOD

a. Author’s Name and Title

b. Department

c. Signature and Date

2. APPROVALS

a. Names and Titles

b. Department

c. Signature and Date

3. SCOPE OF METHOD

Write the objective; a simple statement of what the protocol will accomplish

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 SOP for Analytical Method
Document #: QA/SOP/001-A
Validation
Revision No: 00 For internal use only.
Issue No:02 Do not duplicate.

4. VALIDATION PARAMETERS

The actual parameters will be comprised from a subset of the below list based on the intended

use of the method. Each requirement selected for in a given validation protocol should be

followed with detailed strategy which will be used to test for the parameter including the format

of data tables, sampling scheme, sample size and formulas for intended calculations.

a. Specificity

b. Linearity

c. Precision

d. Accuracy

e. Ruggedness

5. EQUIPMENT

This section should provide all information for the use of the equipment or other apparatus

necessary to conduct all aspects of the method.

6. REAGENTS

This section should list all the reagents and their preparation (where necessary) used to

conduct the method.

7. SAMPLES

This section should list all the samples, their type, and their preparation (where necessary).

(e.g. raw materials, in-process materials, finished goods or stability samples)

8. PROCEDURE

This section should contain all information applicable and relative to the sample, standard and

blank preparation (extraction, dilution etc), instrument parameters, determination and

calculations

a. Sample preparation

i. Extraction

ii. Dilution
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 SOP for Analytical Method
Document #: QA/SOP/001-A
Validation
Revision No: 00 For internal use only.
Issue No:02 Do not duplicate.
iii. Other

b. Standard Preparation

i. Extraction

ii. Dilution

iii. Other

c. Blank Preparation

d. Instrument Operating Parameters

i. Instruments

ii. Operating conditions

1. Columns

2. Temperature

3. Wavelength

4. Special Calibration

5. Other

iii. Determinative step

iv. Calculations (all dilution factors and calculation parameters should be clearly

explained)

9. EVALUATION CRITERIA

Specifications or specific values establishing acceptance criteria for each validation parameter

tested for.

10. REFERENCES

VALIDATION SUMMARY REPORT

Subsequent to the execution of the protocol, the data must be analyzed with 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. A statement of the methods validation status should be placed at

the beginning of the final validation summary report, along with signatures, dates and titles of all the

participants and reviewers.

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