Standard Operating Procedure for High-Pressure Homogenization Analysis for Coated Tablets

Department	Quality Control
SOP No.	SOP/TAB/117/2025
Supersedes	SOP/TAB/117/2022
Page No.	Page 1 of 7
Issue Date	01/03/2026
Effective Date	06/03/2026
Review Date	01/03/2027

1. Purpose

To define the procedure for conducting high-pressure homogenization analysis of coated tablets, ensuring uniform distribution of active pharmaceutical ingredients (APIs) and excipients within the tablet coating.

2. Scope

This SOP applies to the testing of tablet coatings subjected to high-pressure homogenization processes. The procedure assesses the uniformity of the coating, ensuring consistency in the API distribution, thickness, and performance of the coating during tablet manufacturing.

3. Responsibilities

• Quality Control (QC): Responsible for performing high-pressure homogenization testing, ensuring uniform distribution of coating materials and APIs within the tablets.
• Quality Assurance (QA): Ensures the analysis is conducted according to this SOP and reviews results to confirm compliance with product specifications and regulatory guidelines.
• Laboratory Personnel: Responsible for preparing the sample, performing the homogenization analysis, and recording the results.

4. Accountability

The QC Manager is accountable for ensuring that high-pressure homogenization analysis is performed accurately and consistently, adhering to quality standards. The QA Manager is responsible for reviewing and approving results to ensure that the product complies with the necessary regulatory and internal requirements.

5. Procedure

5.1 Sample Preparation

1. Obtain a representative batch of coated tablets to be tested.
2. If testing coated tablets, ensure that they are free from damage and defects such as chips or cracks in the coating.
3. Prepare the sample by crushing the tablets gently, ensuring uniform powder distribution, if required, for analysis.
4. Weigh an appropriate amount of the tablet powder for homogenization testing (usually 100 mg or more depending on the protocol).

5.2 Setting Up High-Pressure Homogenization

1. Ensure the homogenizer is set to the appropriate pressure range for tablet coating analysis (typically 500-2000 bar, depending on the coating material).
2. Fill the homogenization chamber with the prepared tablet sample.
3. Adjust the homogenizer settings for the required cycle time and pressure based on the tablet formulation.
4. Check that the homogenizer is properly calibrated before starting the analysis to ensure accurate results.

5.3 Performing Homogenization Analysis

1. Run the homogenization process for the selected number of cycles to ensure uniform distribution of the coating material within the tablet matrix.
2. Record the pressure, temperature, and cycle time used for the process for each sample.
3. After completion, collect a small sample of the homogenized coating and tablet powder for analysis.

5.4 Particle Size Distribution and Coating Thickness Measurement

1. Perform particle size distribution analysis on the homogenized sample using appropriate equipment, such as laser diffraction or sieve analysis.
2. Measure the coating thickness of a few representative tablets using a micrometer or optical microscopy. Record the results in a detailed report.
3. Ensure the coating thickness and particle size distribution fall within the acceptable range, typically ensuring a consistent and uniform coating.

5.5 Data Analysis and Evaluation

1. Analyze the data to evaluate the uniformity of the coating, API distribution, and particle size range. The coating should exhibit minimal variation within the sample.
2. If the results show excessive variation or deviations from the expected particle size or coating thickness, investigate the cause of inconsistency.
3. Document the results and compare them to the predefined specifications. The analysis should show a consistent and uniform coating without agglomeration or particle size abnormalities.

5.6 Acceptance Criteria

1. The coated tablets should have uniform particle size distribution with minimal deviation between individual tablets.
2. The coating thickness should be within the acceptable range specified in the product’s formulation guidelines (typically ±10% of the target thickness).
3. If the results do not meet the acceptance criteria, initiate corrective actions, such as adjusting the homogenization parameters or modifying the coating process.

5.7 Documentation and Record-Keeping

1. Record all high-pressure homogenization analysis results, including cycle conditions, particle size distribution, and coating thickness data, in the batch record (Annexure-2).
2. Ensure all records are signed, dated, and stored in accordance with the company’s record retention policy.
3. Maintain raw data, including chromatograms, particle size analysis results, and any deviation reports, for regulatory compliance and future reference.

5.8 Post-Test Actions

1. Clean the homogenizer and associated equipment after each use to remove any residual sample material and prevent cross-contamination.
2. Dispose of used tablet samples and solvents according to the company’s waste disposal procedures.
3. Ensure that the homogenizer is regularly serviced and calibrated according to the manufacturer’s guidelines and company SOPs.

6. Abbreviations

• SOP: Standard Operating Procedure
• GMP: Good Manufacturing Practice
• QC: Quality Control
• QA: Quality Assurance
• API: Active Pharmaceutical Ingredient
• HPLC: High-Performance Liquid Chromatography
• SEM: Scanning Electron Microscopy

7. Documents

1. Batch Record (Annexure-2)
2. Deviation Report (Annexure-1)

8. References

• USP <1161> – Granulation and Coating Techniques
• 21 CFR Part 211 – Current Good Manufacturing Practice for Finished Pharmaceuticals (US FDA)
• European Pharmacopoeia (EP) – Stability Testing and Coating Standards

9. SOP Version

Version: 2.0

10. Approval Section

	Prepared By	Checked By	Approved By
Signature
Date
Name
Designation
Department

11. Annexures

Annexure-1: Deviation Report

Deviation Date	Batch Number	Deviation Description	Corrective Action	Responsible Person
15/12/2025	Batch 001	Inconsistent particle size in coating	Adjusted homogenizer settings and re-tested	John Doe

Annexure-2: Batch Record

Batch Number	Sample Weight (g)	Homogenization Pressure (bar)	Particle Size (µm)	Coating Thickness (µm)	Result
Batch 001	100 g	1500 bar	150 µm	25 µm	Pass

Revision History:

Revision Date	Revision No.	Revision Details	Reason for Revision	Approved By
01/01/2024	1.0	Initial Version	New SOP Creation	QA Head
01/02/2025	2.0	Updated homogenization pressure limits	Improved testing conditions	QA Head