SOP for Creating Prototype Ointment Samples for Clinical Studies – V 2.0

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:

API dispersion.
Viscosity.
pH balance.

Record batch preparation details in the **Prototype Batch Record (Annexure-2).**

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