Procedure for Checking the Homogeneity of Ointment Batches
| Department | Production/Quality Control (QC)/Quality Assurance (QA) |
|---|---|
| SOP No. | SOP/Ointment/075 |
| 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 checking the homogeneity of ointment batches to ensure consistency in composition, texture, and distribution of active ingredients throughout the product.
2. Scope
This SOP applies to all personnel in the Production, Quality Control (QC), and Quality Assurance (QA) departments responsible for verifying the uniformity and homogeneity of ointment formulations during manufacturing and prior to batch release.
3. Responsibilities
- Production Operator: Ensures the mixing process is performed according to batch manufacturing instructions.
- Production Supervisor: Verifies that homogeneity tests are performed and documented.
- Quality Control Analyst: Conducts laboratory tests to confirm uniform distribution of active and inactive ingredients.
- Quality Assurance (QA) Personnel: Reviews batch records and approves batch release based on homogeneity compliance.
4. Accountability
The Production, QC, and QA Managers are accountable for ensuring that homogeneity testing is properly conducted and documented as per GMP and regulatory standards.
5. Procedure
5.1 Equipment and Materials
- Mixing tanks with agitators
- Viscometer
- pH meter
- UV-Vis spectrophotometer or HPLC
- Glass slides and microscope (for microscopic evaluation)
- Sampling containers
- Batch Manufacturing Record (BMR)
5.2 Pre-Homogeneity Check Preparations
- Ensure raw materials are weighed and mixed according to the standard formula.
- Verify that mixing parameters (speed, time, temperature) are set correctly.
- Confirm that the batch is within the defined temperature and viscosity limits.
- Ensure that sampling tools and containers are sterile and suitable for use.
5.3 Homogeneity Testing Procedure
5.3.1 In-Process Homogeneity Check
- Take samples from three different points in the mixing tank:
- Top
- Middle
- Bottom
- Compare the physical characteristics of each sample.
- Check for color uniformity, phase separation, or presence of air bubbles.
5.3.2 Laboratory Homogeneity Tests
5.3.2.1 Active Ingredient Assay
- Use HPLC or UV-Vis spectroscopy to check active ingredient concentration.
- Ensure that variation among samples does not exceed ±5% of the target value.
5.3.2.2 pH Measurement
- Measure the pH of samples taken from different sections of the batch.
- Ensure pH consistency across all samples within an acceptable range.
5.3.2.3 Viscosity Testing
- Measure viscosity using a viscometer to confirm uniformity.
- Compare the viscosity of all three samples to ensure uniformity.
5.3.2.4 Microscopic Evaluation
- Prepare slides of ointment samples and observe under a microscope.
- Confirm uniform dispersion of particles without aggregation.
5.4 Acceptance Criteria
- The active ingredient should be evenly distributed within ±5% of the label claim.
- pH variation should not exceed 0.5 units across samples.
- Viscosity differences between samples should not exceed 10%.
- There should be no visible phase separation or air entrapment.
5.5 Documentation
- Record all homogeneity test results in the Homogeneity Test Log.
- Ensure all deviations and corrective actions are documented.
- QA personnel must review and approve test reports before batch release.
6. Abbreviations
- GMP – Good Manufacturing Practices
- QA – Quality Assurance
- QC – Quality Control
- BMR – Batch Manufacturing Record
- HPLC – High-Performance Liquid Chromatography
7. Documents
- Homogeneity Test Log (Annexure-1)
- Batch Release Report (Annexure-2)
8. References
- WHO GMP Guidelines for Pharmaceutical Manufacturing
- USP <905> – Uniformity of Dosage Units
- ICH Q6A – Specifications: Test Procedures and Acceptance Criteria
9. SOP Version
Version 2.0
10. Approval Section
| Prepared By | Checked By | Approved By | |
|---|---|---|---|
| Signature | |||
| Date | |||
| Name | |||
| Designation | |||
| Department |
11. Annexures
Annexure-1: Homogeneity Test Log
| Date | Batch Number | Sample Location | Active Ingredient (%) | pH | Viscosity | Result | Verified By |
|---|---|---|---|---|---|---|---|
| 01/02/2025 | OINT-101 | Top | 98.5% | 6.3 | 45,000 cP | Pass | QA Officer |
| 01/02/2025 | OINT-101 | Middle | 98.8% | 6.4 | 45,500 cP | Pass | QA Officer |
| 01/02/2025 | OINT-101 | Bottom | 98.2% | 6.3 | 44,900 cP | Pass | QA Officer |
Annexure-2: Batch Release Report
| Date | Batch Number | Homogeneity Test | Acceptance Criteria | Result | Final Status | Approved By |
|---|---|---|---|---|---|---|
| 01/02/2025 | OINT-101 | HPLC Assay | 95% – 105% | 98.5% | Approved | QA Head |