Standard Operating Procedure for Testing of API Intermediates and Final Batch

Department	API Manufacturing
SOP No.	SOP/API/144/2025
Supersedes	SOP/API/144/2022
Page No.	Page 1 of 9
Issue Date	13/04/2025
Effective Date	15/04/2025
Review Date	13/04/2026

1. Purpose

To establish a detailed procedure for sampling, testing, reviewing, and reporting of API intermediates and final batch samples to ensure conformance with approved specifications and regulatory compliance before batch release.

2. Scope

This SOP is applicable to all API intermediates and final batch samples generated and tested in the Quality Control laboratory of the API manufacturing facility.

3. Responsibilities

• QC Analyst: Perform sampling and testing as per approved specifications and STPs.
• QC Reviewer: Review analytical reports and supporting data for accuracy and compliance.
• QA Officer: Approve analytical reports and authorize batch release based on compliance status.

4. Accountability

The Head of Quality Control is accountable for testing timelines, documentation, and ensuring adherence to cGMP guidelines for all intermediate and final API batches.

5. Procedure

5.1 Sample Collection

1. Ensure batch production record is complete and approved for sampling.
2. Collect samples using appropriate sampling devices in a controlled area using aseptic techniques (if applicable).
3. Label each sample with:
   • Sample ID
   • Batch number
   • Date of sampling
   • Sample quantity
   • Analyst initials
4. Record details in the Sample Receipt Log (Annexure-1).

5.2 Testing Procedure

1. Perform tests as per the approved STP and product specifications for:
   • Appearance
   • Identification (UV/IR/HPLC)
   • Assay
   • Related substances or impurities
   • Residual solvents
   • Loss on drying / Moisture content
   • pH (if applicable)
2. Carry out system suitability checks before analysis.
3. Use approved reference standards and ensure calibration status of instruments.
4. Record results in the Analytical Worksheet (Annexure-2).

5.3 Data Review and Approval

1. Review raw data, instrument printouts, calculations, and result summaries.
2. Ensure all entries are signed, dated, and traceable.
3. Compare results with specifications.
4. If OOS or OOT, initiate investigation as per respective SOPs.
5. Prepare a Final Analytical Report (Annexure-3) and submit for QA approval.

5.4 Batch Release Authorization

1. QA verifies:
   • Conformance with specifications
   • Completion of all test parameters
   • Absence of any deviation impacting quality
2. Batch disposition is recorded in the Batch Status Register (Annexure-4).

6. Abbreviations

• QC: Quality Control
• QA: Quality Assurance
• API: Active Pharmaceutical Ingredient
• STP: Standard Test Procedure
• OOS: Out of Specification
• OOT: Out of Trend
• SOP: Standard Operating Procedure

7. Documents

1. Sample Receipt Log (Annexure-1)
2. Analytical Worksheet (Annexure-2)
3. Final Analytical Report (Annexure-3)
4. Batch Status Register (Annexure-4)

8. References

• ICH Q7 – GMP for Active Pharmaceutical Ingredients
• 21 CFR Part 211
• Internal Specifications and Test Procedures

9. SOP Version

Version: 2.0

10. Approval Section

	Prepared By	Checked By	Approved By
Signature
Date
Name
Designation
Department

11. Annexures

Annexure-1: Sample Receipt Log

Date	Sample ID	Batch No.	Quantity	Received By
13/04/2025	SMP-144	API-B144	50g	Sunita Reddy

Annexure-2: Analytical Worksheet

Test	Specification	Result	Pass/Fail
Assay	98.0–102.0%	99.5%	Pass

Annexure-3: Final Analytical Report

Report No.	Batch No.	Date	Tested By	Reviewed By
AR-20250413-144	API-B144	13/04/2025	Ravi Kumar	QA Officer

Annexure-4: Batch Status Register

Batch No.	Date Released	Status	Released By
API-B144	14/04/2025	Approved	QA Head

Revision History:

Revision Date	Revision No.	Details	Reason	Approved By
01/01/2022	1.0	Initial Version	New API Launch	QA Head
13/04/2025	2.0	Annexure inclusion and formatting updates	Audit Requirement	QA Head