Procedure for Testing Residue Levels After Cleaning
| Department | Quality Control (QC)/Quality Assurance (QA)/Validation |
|---|---|
| SOP No. | SOP/Ointment/122 |
| 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 testing residue levels after cleaning 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 Control (QC), Quality Assurance (QA), and Validation departments responsible for conducting residue level testing and ensuring compliance.
3. Responsibilities
- QC Analyst: Conducts residue analysis and documents test results.
- QA Officer: Reviews test results and ensures compliance with acceptance criteria.
- Validation Team: Develops and approves residue testing methods.
- Production Supervisor: Ensures adherence to validated cleaning procedures.
- QA Manager: Approves residue testing protocols and reports.
4. Accountability
The QA and QC Managers are accountable for ensuring that residue testing is conducted as per GMP, FDA, ICH, and WHO guidelines.
5. Procedure
5.1 Selection of Residue Testing Methods
- Choose appropriate residue testing methods based on:
- Nature of the cleaning agents used
- Characteristics of residual materials
- Regulatory requirements and acceptance criteria
- Common residue testing methods include:
- Swab Sampling Method
- Rinse Sampling Method
- Total Organic Carbon (TOC) Analysis
- High-Performance Liquid Chromatography (HPLC)
- Visual Inspection
5.2 Preparation for
Residue Testing
- Ensure that all test equipment is calibrated before use.
- Prepare test reagents and standards as per validated protocols.
- Assign trained personnel to conduct residue testing.
5.3 Execution of Residue Testing
5.3.1 Swab Sampling Method
- Use sterile swabs to collect samples from designated equipment surfaces.
- Swab a predefined surface area in a systematic pattern.
- Place swabs in sterile vials and transport them to the laboratory for analysis.
5.3.2 Rinse Sampling Method
- Collect rinse water samples from equipment after cleaning.
- Ensure sample volumes meet minimum testing requirements.
- Transport samples under controlled conditions to the laboratory.
5.3.3 Analytical Testing
- Perform analytical testing using methods such as:
- HPLC for active pharmaceutical ingredient (API) residue detection
- TOC analysis for detecting organic residues
- pH testing for confirming removal of acidic or alkaline cleaning agents
- Record and analyze test results to determine compliance.
5.4 Acceptance Criteria and Compliance
- Compare test results against predefined acceptance limits.
- Residue levels must meet established criteria to ensure equipment cleanliness.
- Document deviations and implement corrective actions if required.
5.5 Documentation and Review
- Record test results in the Residue Testing Log.
- QA must review and approve test results before equipment release.
- Maintain records for regulatory audits.
6. Abbreviations
- GMP – Good Manufacturing Practices
- QA – Quality Assurance
- QC – Quality Control
- HPLC – High-Performance Liquid Chromatography
- TOC – Total Organic Carbon
7. Documents
- Residue Testing Protocol (Annexure-1)
- Residue Testing Log (Annexure-2)
8. References
- ICH Q7 – Good Manufacturing Practice Guide
- WHO Guidelines for Residue Testing
- 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: Residue Testing 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: Residue Testing Log
| Date | Equipment ID | Sample Type | Test Performed | Result | Reviewed By |
|---|---|---|---|---|---|
| 01/02/2025 | MIX-1001 | Swab | HPLC | Pass | QA Manager |
| 02/02/2025 | FILL-2002 | Rinse | 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 |