Procedure for Validation of Filling Processes

Department	Quality Assurance (QA)/Production/Research & Development (R&D)
SOP No.	SOP/Ointment/113
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 establish a systematic process for the validation of filling processes in ointment manufacturing. This ensures that the filling operation maintains consistency, accuracy, and compliance with regulatory standards.

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 the filling process for ointment manufacturing.

3. Responsibilities

• Production Supervisor: Oversees the filling process and ensures adherence to validation protocols.
• QA Officer: Ensures compliance with GMP and regulatory guidelines.
• R&D Scientist: Determines critical filling parameters for validation.
• Validation Team: Conducts validation trials and compiles data.
• QA Manager: Approves the filling validation protocol and final validation report.

4. Accountability

The QA and Production Managers are accountable for ensuring compliance with regulatory requirements and the accuracy of the filling process validation.

5. Procedure

5.1 Validation Planning

• Develop a Filling Process Validation Protocol outlining:
  • Objective and scope of validation
  • Batch size and equipment specifications
  • Filling accuracy, speed, and volume
  • Acceptance criteria for weight variation, tube sealing integrity, and homogeneity
• Identify sampling points for in-process quality control checks.
• Ensure filling equipment is calibrated and in optimal condition before validation.

5.2 Execution of Validation Batches

• Conduct a minimum of three consecutive validation batches to confirm process consistency.
• Ensure each batch follows the same filling procedure, including:
  • Filling volume and weight control
  • Tube or container positioning
  • Speed and accuracy of dispensing
  • Sealing method and integrity testing
• Collect in-process samples at predefined intervals.

5.3 Testing and Evaluation of Validation Data

• Test each sample for critical quality attributes, including:
  • Fill weight variation
  • Container sealing integrity
  • Uniformity of the filled product
  • Microbial contamination checks
  • Final product appearance
• Compile all data and compare results with predefined acceptance criteria.

5.4 Process Optimization

• If deviations occur, adjust filling parameters accordingly.
• Conduct additional validation trials if necessary.
• Document all process optimizations in the Validation Report.

5.5 Approval and Finalization

• QA must review and approve the Filling Validation Report.
• Ensure validated parameters are incorporated into the Master Batch Record (MBR).
• Maintain validation records for regulatory audits and inspections.

6. Abbreviations

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

7. Documents

• Filling Validation Protocol (Annexure-1)
• Filling Validation Report (Annexure-2)

8. References

• ICH Q8 – Pharmaceutical Development
• WHO GMP Guidelines for Process Validation
• US FDA Guidance on 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: Filling Validation Protocol

Validation Parameter	Specification	Acceptance Criteria
Filling Volume	30-100g	±5% Variation
Filling Speed	20-60 tubes per minute	Within Set Limits
Sealing Integrity	No leakage	100% compliance

Annexure-2: Filling Validation Report

Batch Number	Filling Volume	Weight Variation	Sealing Integrity	Final Approval
OINT-1301	50g	Within Limits	Compliant	QA Manager
OINT-1302	75g	Within Limits	Compliant	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