Standard Operating Procedure for Validating Analytical Methods in QA

Department	Tablet
SOP No.	SOP/TAB/204/2025
Supersedes	SOP/TAB/204/2022
Page No.	Page 1 of 7
Issue Date	01/03/2026
Effective Date	06/03/2026
Review Date	01/03/2027

1. Purpose

To define the procedure for validating analytical methods used in quality assurance (QA) during the testing of tablet products. This ensures that analytical methods are accurate, precise, reliable, and suitable for their intended use in quality control.

2. Scope

This SOP applies to all analytical methods used in the testing of raw materials, in-process materials, and finished tablet products in the QA department. It includes the validation of methods for assay, dissolution, content uniformity, and other critical quality attributes.

3. Responsibilities

• Quality Assurance (QA) Manager: Responsible for ensuring that analytical methods are validated in accordance with regulatory requirements and internal standards.
• QC Analyst: Responsible for conducting the method validation tests, recording the results, and reporting findings to the QA team.
• Regulatory Affairs: Ensures that the method validation process complies with applicable regulatory requirements and standards.
• Training Coordinator: Responsible for ensuring that all personnel performing method validation are properly trained and competent.

4. Accountability

The QA Manager is accountable for overseeing the method validation process. The QC Analyst is responsible for conducting the actual validation and documenting the results. The Training Coordinator is responsible for ensuring that all relevant staff are trained on method validation procedures.

5. Procedure

5.1 Method Selection

1. Select the analytical method based on the type of product being tested and the critical quality attributes to be measured. Consider the accuracy, precision, specificity, and robustness of the method.
2. Ensure that the method selected is appropriate for its intended use and that it complies with applicable regulatory guidelines, such as USP, EP, or ICH standards.

5.2 Defining Validation Parameters

1. Identify the validation parameters that need to be evaluated for the method, such as accuracy, precision, specificity, sensitivity, limit of detection, limit of quantitation, and linearity.
2. Ensure that each parameter is tested in accordance with established procedures and regulatory requirements (Annexure-1).

5.3 Conducting Validation Studies

1. Perform the validation studies using representative batches of raw materials, in-process materials, or finished tablets.
2. Ensure that a sufficient number of samples are tested to provide statistically valid results.
3. For each validation parameter, conduct the following tests:
   • Accuracy: Compare the results obtained using the method with known standards or reference methods.
   • Precision: Perform multiple tests to ensure that the method yields consistent results under the same conditions.
   • Specificity: Ensure that the method can accurately measure the desired analyte in the presence of other substances.
   • Linearity: Test the method across a range of concentrations to ensure that the response is linear.
   • Limit of Detection (LOD) and Limit of Quantification (LOQ): Determine the lowest concentration at which the method can reliably detect and quantify the analyte.
4. Document all results in the method validation report (Annexure-2) and ensure that all data is accurately recorded and analyzed.

5.4 Data Analysis

1. Analyze the data collected from the validation studies to determine whether the method meets the predefined acceptance criteria for each parameter.
2. Evaluate the precision, accuracy, and reliability of the method based on the results. If any parameter does not meet the acceptance criteria, further investigation and method optimization are required.

5.5 Reporting of Validation Results

1. Prepare a validation report summarizing the results of the studies, including data analysis, conclusions, and any necessary corrective actions (Annexure-3).
2. Include details of the method, materials tested, testing conditions, and acceptance criteria for each parameter.
3. If the method is validated successfully, recommend its approval for routine use in the QC laboratory.
4. Ensure that the validation report is signed off by the QA Manager and filed as part of the official documentation.

5.6 Revalidation

1. Periodic revalidation may be required for certain methods, especially if there are significant changes in raw materials, equipment, or production processes.
2. Revalidation should be conducted according to the same procedures as the initial validation and include an assessment of whether the method remains suitable for its intended purpose.

5.7 Documentation and Record Keeping

1. Maintain all validation records, including validation study results, raw data, reports, and approval signatures, in a secure and organized manner (Annexure-4).
2. Ensure that all records are available for review during internal audits, regulatory inspections, or quality reviews.
3. Keep the validation documentation for the required retention period as per regulatory guidelines or internal policies.

6. Abbreviations

• SOP: Standard Operating Procedure
• QA: Quality Assurance
• QC: Quality Control
• LOD: Limit of Detection
• LOQ: Limit of Quantification
• RSD: Relative Standard Deviation
• USP: United States Pharmacopeia
• ICH: International Council for Harmonisation

7. Documents

1. Method Validation Report (Annexure-2)
2. Raw Data and Analysis (Annexure-3)
3. Method Validation Protocol (Annexure-1)
4. Validation Records (Annexure-4)

8. References

• 21 CFR Part 211 – Current Good Manufacturing Practice for Finished Pharmaceuticals (US FDA)
• USP <1225> – Validation of Analytical Methods
• ICH Q2(R1) – Validation of Analytical Procedures: Text and Methodology

9. SOP Version

Version: 2.0

10. Approval Section

	Prepared By	Checked By	Approved By
Signature
Date
Name
Designation
Department

11. Annexures

Annexure-1: Method Validation Protocol

Validation Parameter	Acceptance Criteria	Method	Tested By
Accuracy	±2%	Assay Method	John Doe

Annexure-2: Validation Report

Parameter	Test Results	Conclusion	Action Required
Linearity	R² = 0.999	Pass	None

Annexure-3: Raw Data and Analysis

Test	Sample ID	Measured Value	Expected Value	Deviation
Assay	Sample-01	98.5%	99%	0.5%

Annexure-4: Validation Records

Validation ID	Method	Tested By	Completion Date
VAL-001	Assay Method	Jane Smith	01/04/2026

Revision History:

Revision Date	Revision No.	Revision Details	Reason for Revision	Approved By
01/01/2024	1.0	Initial Version	New SOP Creation	QA Head
01/02/2025	2.0	Updated validation parameters	Added new test parameters	QA Head