Procedure for Creating Prototype Ointment Samples for Clinical Studies
| Department | Research and Development (R&D)/Quality Assurance (QA)/Quality Control (QC)/Clinical Research |
|---|---|
| SOP No. | SOP/Ointment/190 |
| 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 a systematic approach for creating prototype ointment samples intended for clinical studies. This process ensures that the formulation meets safety, efficacy, and regulatory requirements before large-scale production.
2. Scope
This SOP applies to all personnel involved in prototype development, formulation trials, analytical testing, stability studies, and regulatory documentation in the Research and Development (R&D), Quality Assurance (QA), and Quality Control (QC) departments.
3. Responsibilities
- Formulation Scientist: Develops and refines prototype formulations.
- QA Officer: Ensures compliance with regulatory guidelines.
- QC Analyst: Conducts quality testing on prototype batches.
- Clinical Research Scientist: Coordinates clinical trial sample preparation.
- Regulatory Affairs Specialist: Ensures adherence to regulatory submission requirements.
4. Accountability
The R&D Manager is accountable for ensuring that all prototype development activities comply with GMP, FDA, ICH, WHO, and company policies.
5. Procedure
5.1 Selection of Prototype Formulation
- Select formulations based on:
- API stability and solubility.
- Intended therapeutic effect.
- Regulatory compliance with clinical study requirements.
- Document prototype selection in the **Prototype Development Log (Annexure-1).**
5.2 Preparation of Prototype Batches
- Prepare
small-scale batches using GMP-compliant methods.
Use **pilot-scale equipment** to ensure consistency with final production.
Ensure uniformity in:
Record batch preparation details in the **Prototype Batch Record (Annexure-2).**
- API dispersion.
- Viscosity.
- pH balance.
5.3 Quality Control Testing
- Conduct **analytical testing** for:
- Assay of active ingredients.
- Impurity profiling.
- Microbial contamination.
- Perform **physical characterization**:
- Appearance, spreadability, and texture.
- pH and viscosity testing.
- Document results in the **QC Analysis Report (Annexure-3).**
5.4 Stability Studies
- Conduct **accelerated and real-time stability testing**:
- Storage conditions: **40°C / 75% RH and 25°C / 60% RH.**
- Time points: **0, 1, 3, 6, and 12 months.**
- Evaluate **degradation, phase separation, and viscosity changes.**
- Record findings in the **Stability Study Report (Annexure-4).**
5.5 Clinical Study Sample Packaging and Labeling
- Select appropriate **packaging materials**:
- Air-tight tubes for moisture-sensitive formulations.
- Opaque containers for light-sensitive ingredients.
- Ensure labeling includes:
- Study protocol reference number.
- Storage conditions.
- Investigator’s use only statement.
- Document packaging details in the **Clinical Sample Packaging Log (Annexure-5).**
5.6 Regulatory Documentation and Approval
- Prepare regulatory submission documents including:
- CMC (Chemistry, Manufacturing, and Controls) data.
- Certificate of Analysis (CoA).
- QA must review and approve all documentation before release.
- Maintain records for **five years** for regulatory audits.
6. Abbreviations
- API – Active Pharmaceutical Ingredient
- GMP – Good Manufacturing Practices
- QA – Quality Assurance
- QC – Quality Control
- ICH – International Council for Harmonisation
- FDA – Food and Drug Administration
7. Documents
- Prototype Development Log (Annexure-1)
- Prototype Batch Record (Annexure-2)
- QC Analysis Report (Annexure-3)
- Stability Study Report (Annexure-4)
- Clinical Sample Packaging Log (Annexure-5)
8. References
- ICH Q1A – Stability Testing of New Drug Substances and Products
- FDA Guidance on Clinical Trial Materials
- WHO Guidelines on Pharmaceutical Development
9. SOP Version
Version 2.0
10. Approval Section
| Prepared By | Checked By | Approved By | |
|---|---|---|---|
| Signature | |||
| Date | |||
| Name | |||
| Designation | |||
| Department |
11. Annexures
Annexure-1: Prototype Development Log
| Date | API | Base Type | Formulation Notes | QC Review |
|---|---|---|---|---|
| 02/02/2025 | Clobetasol Propionate | Petrolatum | High absorption | Approved |
Annexure-2: Prototype Batch Record
| Date | Batch No. | Ingredient Composition | Final Yield | QA Approval |
|---|---|---|---|---|
| 02/02/2025 | OINT-1001 | API 0.05%, Base 99.95% | 100 g | Approved |
12. Revision History
| Revision Date | Revision No. | Details | Reason | Approved By |
|---|---|---|---|---|
| 02/02/2025 | 2.0 | Expanded Stability and Clinical Trial Testing | Regulatory Compliance | QA Head |