Procedure for Performing Rinse Sampling for Validation
| Department | Quality Assurance (QA)/Validation/Quality Control (QC)/Production |
|---|---|
| SOP No. | SOP/Ointment/129 |
| 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 process for performing rinse sampling for cleaning validation in ointment manufacturing. This ensures that cleaning procedures effectively remove residues and comply with regulatory requirements.
2. Scope
This SOP applies to all personnel in the Quality Assurance (QA), Validation, Quality Control (QC), and Production departments responsible for conducting rinse sampling, analyzing results, and maintaining validation records.
3. Responsibilities
- QA Officer: Ensures compliance with rinse sampling protocols.
- Validation Team: Develops and validates rinse sampling methods.
- QC Analyst: Conducts analytical testing on rinse samples.
- Production Supervisor: Ensures correct execution of rinse sampling.
- QA Manager: Approves final validation reports and maintains documentation.
4. Accountability
The QA and Validation Managers are accountable for ensuring that rinse sampling for validation is conducted as per GMP, FDA, ICH, and WHO guidelines.
5. Procedure
5.1 Selection of Rinse Sampling Locations
- Identify critical surfaces requiring rinse sampling.
- Focus on:
- Hard-to-clean areas
- Equipment contact surfaces
- Pipes and tubing where residues may accumulate
- Define specific sampling points in the validation protocol.
5.2 Preparation for Rinse Sampling
- Ensure equipment is cleaned as per standard cleaning
procedures.
Prepare required materials:
Label collection containers appropriately before sampling.
- Sterile rinse solution (e.g., purified water or buffer solution)
- Sterile collection containers
- Personal protective equipment (PPE)
- Calibrated measuring instruments
5.3 Execution of Rinse Sampling
- Introduce a measured volume of rinse solution into the equipment.
- Ensure the solution contacts all surfaces for adequate sampling.
- Collect the rinse solution from the designated sampling points.
- Transfer samples into labeled containers and seal securely.
- Transport samples to the QC laboratory for analysis.
5.4 Analytical Testing of Rinse Samples
- Analyze samples using:
- High-Performance Liquid Chromatography (HPLC) for API residues
- Total Organic Carbon (TOC) analysis for organic residues
- pH testing for cleaning agent residues
- Microbial testing (if applicable)
- Compare results with predefined acceptance limits.
5.5 Acceptance Criteria and Compliance
- Residue levels must be below established limits.
- No visible particulates or discoloration should be present.
- Equipment must pass visual inspection before release for production.
5.6 Handling Deviations
- If rinse sample results exceed acceptance criteria:
- Notify the QA and Production teams immediately.
- Initiate re-cleaning and document corrective actions.
- Repeat rinse sampling and confirm compliance.
5.7 Documentation and Review
- Record all rinse sample data in the Rinse Sampling Log.
- QA must review and approve all results before final validation approval.
- Maintain records for regulatory audits and compliance verification.
6. Abbreviations
- GMP – Good Manufacturing Practices
- QA – Quality Assurance
- QC – Quality Control
- HPLC – High-Performance Liquid Chromatography
- TOC – Total Organic Carbon
7. Documents
- Rinse Sampling Protocol (Annexure-1)
- Rinse Sampling Log (Annexure-2)
8. References
- ICH Q7 – Good Manufacturing Practice Guide
- WHO Guidelines for Cleaning Validation
- US FDA Guidance on Cleaning 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: Rinse Sampling Protocol
| Test Parameter | Method | Acceptance Criteria |
|---|---|---|
| API Residue | HPLC | < 10 ppm |
| Organic Residue | TOC Analysis | < 5 ppm |
| Cleaning Agent Residue | pH Test | Neutral |
Annexure-2: Rinse Sampling Log
| Date | Equipment ID | Rinse Solution Used | Test Performed | Result | Reviewed By |
|---|---|---|---|---|---|
| 01/02/2025 | MIX-1001 | Purified Water | HPLC | Pass | QA Manager |
| 02/02/2025 | FILL-2002 | Buffer Solution | TOC | 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 |