3. Responsibilities

• QC Analyst: Collect and label control samples properly, record storage location, and conduct periodic testing.
• QC Reviewer: Review control sample records and confirm adherence to retention and testing schedule.
• QA Officer: Ensure control samples are handled as per SOP and available for investigation or inspection.

4. Accountability

The QC Head is accountable for the integrity, compliance, and traceability of all control samples retained in the facility.

5. Procedure

5.1 Collection of Control Samples

1. After completion of testing and approval of a batch, collect a sufficient quantity of each sample:
   • Raw materials: 100 g or as per material characteristics
   • API/intermediates: Minimum 2x the quantity required for complete testing
2. Use clean, inert, leak-proof containers labeled with:
   • Product name and code
   • Batch number
   • Date of manufacture
   • Storage conditions
   • Signature of person collecting
3. Record entries in the Control Sample Collection Log (Annexure-1).

5.2 Storage Conditions

1. Store control samples in dedicated cabinets or chambers with environmental monitoring.
2. Maintain temperature and humidity conditions as specified in the master specification file:
   • Room temperature: 25°C ± 2°C / 60% RH ± 5%
   • Refrigerated storage (if required): 2–8°C
3. Log storage location in the Control Sample Register (Annexure-2).

5.3 Testing of Control Samples

1. Perform testing annually or as per defined stability schedule.
2. Tests to include:
   • Appearance
   • Assay
   • Impurities/Degradation Products
   • Moisture Content
   • Any product-specific critical attributes
3. Document results in the Control Sample Testing Log (Annexure-3).
4. If any deterioration is found, initiate investigation and notify QA.

5.4 Retention Period

1. Retain control samples for:
   • 3 years post-manufacture or 1 year after expiry, whichever is later
   • For registered products: as per regulatory requirement
2. Maintain samples in an orderly manner for easy retrieval during inspections or investigations.

5.5 Disposal of Control Samples

1. At the end of the retention period, QA to authorize disposal.
2. Record disposal details in the Disposal Log (Annexure-4).
3. Ensure destruction is done in line with environmental and EHS policies.

5.6 Inspections and Audits

1. Control samples should be readily available for:
   • Regulatory inspections
   • Internal QA audits
   • Batch failure investigations
2. Maintain traceability from batch record to control sample log.

6. Abbreviations

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

7. Documents

1. Control Sample Collection Log (Annexure-1)
2. Control Sample Register (Annexure-2)
3. Control Sample Testing Log (Annexure-3)
4. Control Sample Disposal Log (Annexure-4)

8. References

• ICH Q1A(R2) – Stability Testing of New Drug Substances
• 21 CFR 211.170 – Reserve Samples
• WHO TRS 1010 – Annex 2

9. SOP Version

Version: 2.0

10. Approval Section

	Prepared By	Checked By	Approved By
Signature
Date
Name
Designation
Department

11. Annexures

Annexure-1: Control Sample Collection Log

Date	Batch No.	Product	Qty	Container No.	Analyst
13/04/2025	API-B150	Metronidazole	200g	CN-27	Sunita Reddy

Annexure-2: Control Sample Register

Sample Code	Batch No.	Location	Storage Condition	Remarks
CS-MTZ-150	API-B150	Shelf 3-A	25°C / 60% RH	None

Annexure-3: Control Sample Testing Log

Date	Batch No.	Test Performed	Result	Remarks
12/04/2025	API-B150	Assay	98.7%	Complies

Annexure-4: Control Sample Disposal Log

Date	Batch No.	Disposal Approved By	Method	Remarks
13/04/2028	API-B150	QA Officer	Incineration	Retention expired

Revision History:

Revision Date	Revision No.	Details	Reason	Approved By
01/01/2022	1.0	Initial version	New product line	QA Head
13/04/2025	2.0	Added disposal procedure and log format	Audit Requirement	QA Head