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