SOP for Validation of Mixing Processes – V 2.0

Procedure for Validation of Mixing Processes

Department	Quality Assurance (QA)/Production/Research & Development (R&D)
SOP No.	SOP/Ointment/111
Supersedes	V 1.0
Page No.	Page X of Y
Issue Date	[Insert Issue Date]
Effective Date	[Insert Effective Date]
Review Date	[Insert Review Date]

1. Purpose

The purpose of this Standard Operating Procedure (SOP) is to define the systematic approach for the validation of mixing processes used in ointment manufacturing. This ensures that mixing parameters are optimized, reproducible, and meet product quality specifications.

2. Scope

This SOP applies to all personnel in the Quality Assurance (QA), Production, and Research & Development (R&D) departments involved in the validation of mixing processes for ointment manufacturing.

3. Responsibilities

Production Supervisor: Oversees mixing process and ensures adherence to validation protocol.
QA Officer: Verifies validation process compliance and reviews test results.
R&D Scientist: Defines critical mixing parameters and ensures process optimization.
Validation Team: Conducts validation trials and compiles data.
QA Manager: Approves validation protocol and final validation report.

4. Accountability

The QA and Production Managers are accountable for ensuring the mixing process validation is performed according to regulatory guidelines and GMP requirements.

5. Procedure

5.1 Validation Planning

Prepare a Mixing Process Validation Protocol outlining:
- Objective and scope of validation
- Batch size and equipment used
- Mixing speed, duration, and temperature control
- Acceptance criteria for homogeneity, viscosity, and pH
Define sampling points for evaluation of process parameters.
Ensure

that mixing equipment is calibrated and operational before validation.

5.2 Execution of Validation Batches

Conduct at least three consecutive mixing validation batches to confirm process consistency.
Ensure each batch follows the same mixing procedure, including:
- Loading sequence of raw materials
- Mixing time and speed
- Temperature monitoring
- Homogenization process
Collect in-process samples at predefined intervals.

5.3 Testing and Evaluation of Validation Data

Test each sample for critical quality attributes, including:
- Homogeneity (assay and active ingredient distribution)
- Viscosity (Brookfield or Rheometer test)
- pH stability
- Microbial contamination
- Phase separation
Compile data and compare against predefined acceptance criteria.

5.4 Process Optimization

If deviations are observed, adjust mixing parameters accordingly.
Perform additional validation trials if required.
Document all process optimizations in the Validation Report.

5.5 Approval and Finalization

QA must review and approve the Mixing Validation Report.
Ensure that final parameters are incorporated into the Master Batch Record (MBR).
Maintain validation records for regulatory audits.

6. Abbreviations

GMP – Good Manufacturing Practices
QA – Quality Assurance
MBR – Master Batch Record
R&D – Research & Development

7. Documents

Mixing Validation Protocol (Annexure-1)
Mixing Validation Report (Annexure-2)

8. References

ICH Q8 – Pharmaceutical Development
WHO GMP Guidelines for Process Validation

9. SOP Version

Version 2.0

10. Approval Section

	Prepared By	Checked By	Approved By
Signature
Date
Name
Designation
Department

11. Annexures

Annexure-1: Mixing Validation Protocol

Validation Parameter	Specification	Acceptance Criteria
Mixing Speed	500-1000 rpm	±10% Variation
Mixing Time	30-60 minutes	No phase separation
Temperature	40°C ± 2°C	Stable viscosity

Annexure-2: Mixing Validation Report

Batch Number	Mixing Speed	Time	Homogeneity	Viscosity	Final Approval
OINT-1101	800 rpm	45 min	Compliant	Pass	QA Manager
OINT-1102	750 rpm	50 min	Compliant	Pass	QA Manager

12. Revision History:

Revision Date	Revision No.	Details of Revision	Reason for Revision	Approved By
01/01/2024	1.0	Initial Version	New SOP	QA Head
01/02/2025	2.0	Updated SOP Format	Standardization of Document	QA Head