Standard Operating Procedure for Homogeneity Sampling in Elixir Manufacturing

Department	Elixir Department
SOP No.	SOP/ELX/200/2025
Supersedes	SOP/ELX/200/2022
Page No.	Page 1 of 9
Issue Date	11/04/2025
Effective Date	15/04/2025
Review Date	11/04/2026

1. Purpose

To establish a procedure for conducting homogeneity sampling during elixir manufacturing to ensure uniform distribution of active pharmaceutical ingredients (APIs) and excipients throughout the batch before release for filtration and filling.

2. Scope

This SOP applies to all batches of elixir products manufactured in the Elixir Department where homogeneity is a critical quality attribute. It covers the sampling process, location, frequency, and evaluation methods prior to bulk storage or packing.

3. Responsibilities

• Production Operator:
  • Assist in collecting samples from the designated tank levels.
• QC Analyst:
  • Analyze homogeneity samples for uniformity of API content and appearance.
• QA Officer:
  • Verify compliance with sampling protocol and approve results for batch continuation.

4. Accountability

The Production Head is accountable for coordinating the sampling process. The QC Head is responsible for evaluating sample results. QA Head is responsible for final release decisions.

5. Procedure

5.1 Sampling Location and Time

1. Sampling should be done after final mixing and before filtration.
2. Collect samples from three locations:
   • Top layer (after gentle stirring)
   • Middle of the tank
   • Bottom layer (through sampling valve or manual dipping)

5.2 Sampling Procedure

1. Use clean and dry glass or amber vials for sample collection.
2. Collect 50 mL from each location and label with:
   • Product name
   • Batch number
   • Sampling point (Top/Middle/Bottom)
   • Date and time
3. Ensure thorough mixing before each draw to mimic the actual distribution within the tank.
4. Seal and transport samples to QC immediately for analysis.

5.3 Analytical Testing

1. Perform assay for API content from each sample.
2. Analyze appearance, pH, and alcohol content (if applicable).
3. Results must comply with the following acceptance criteria:
   • API content variation between any two layers should not exceed ±5% of the average value.
   • Appearance and clarity must be uniform across all samples.

5.4 Actions in Case of Failure

1. If variation exceeds acceptable range, inform QA immediately.
2. Repeat mixing for an additional defined time and re-sample.
3. If second attempt fails, initiate deviation as per SOP/QMS/DEV/001.

5.5 Documentation

1. Record results in the Homogeneity Sampling Logbook (Annexure-1).
2. Attach printouts of assay and appearance test reports.
3. Ensure QA signs off the log and approves for next processing step.

6. Abbreviations

• SOP: Standard Operating Procedure
• QA: Quality Assurance
• QC: Quality Control
• API: Active Pharmaceutical Ingredient

7. Documents

1. Homogeneity Sampling Logbook (Annexure-1)
2. Batch Manufacturing Record (BMR)
3. Assay Test Report

8. References

• ICH Q8 – Pharmaceutical Development
• 21 CFR Part 211.110 – In-Process Sampling and Testing
• WHO TRS 986 – GMP Guidelines for Pharmaceuticals

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 Sampling Logbook

Date	Batch No.	Sampling Point	API Assay (%)	Appearance	Result	QC Analyst	QA Review
11/04/2025	ELX-0425-019	Top	98.2%	Clear	Pass	Rajesh Kumar	Sunita Reddy
11/04/2025	ELX-0425-019	Middle	98.5%	Clear	Pass	Rajesh Kumar	Sunita Reddy
11/04/2025	ELX-0425-019	Bottom	98.4%	Clear	Pass	Rajesh Kumar	Sunita Reddy

Revision History:

Revision Date	Revision No.	Revision Details	Reason for Revision	Approved By
01/01/2024	1.0	Initial Release	New SOP	QA Head
11/04/2025	2.0	Added sample acceptance criteria and three-point testing requirement	Regulatory Compliance	QA Head