evaluates each sample’s condition before processing.

Sample Custodian: Retrieves and verifies samples against the log.

QA Representative: Verifies documentation and reviews deviations.

Lab Manager: Authorizes sample rejection or reprocessing as required.

4. Accountability

The Head of the Bioanalytical Department is accountable for ensuring sample quality verification before analysis and for maintaining accurate integrity records.

5. Procedure

5.1 Sample Retrieval from Storage

1. Retrieve samples based on the Sample Analysis Plan and Sample Inventory Sheet.
2. Document retrieval date, time, and analyst in Annexure-1: Sample Movement Log.

5.2 Visual Inspection

1. Inspect each sample vial for:
   • Label integrity (study code, subject ID, time point)
   • Frosting or condensation on vials
   • Leakage, breakage, discoloration, or particulate matter
2. Document any discrepancies in Annexure-2: Sample Integrity Check Form.

5.3 Thawing and Equilibration

1. Thaw samples at 4°C or as per method SOP, avoiding repeated freeze-thaw cycles.
2. Mix gently by inversion or vortexing to homogenize contents before analysis.
3. Do not use samples exhibiting signs of hemolysis or phase separation unless justified and documented.

5.4 Temperature and Storage Condition Review

1. Review freezer log entries for temperature maintenance throughout storage period.
2. If any temperature excursions occurred, check associated CAPA and QA approval before proceeding.
3. Verify sample batch storage mapping from Annexure-3: Freezer Inventory Sheet.

5.5 Sample Qualification for Analysis

1. Only samples that meet the following criteria qualify for analysis:
   • Properly labeled and sealed
   • No visual defects or contamination
   • Maintained within validated temperature range
2. Segregate and label rejected samples with “Not for Analysis” and document in Annexure-4: Rejected Sample Log.
3. Notify Study Manager and QA for confirmation and further instruction.

5.6 Documentation

1. All forms must be signed by the analyst and reviewed by QA before start of analysis.
2. Attach integrity forms to the Study Master File (SMF).
3. Retain all integrity records for at least 5 years or as per sponsor-specific retention policy.

6. Abbreviations

• BA/BE: Bioavailability/Bioequivalence
• SOP: Standard Operating Procedure
• QA: Quality Assurance
• SMF: Study Master File

7. Documents

1. Sample Movement Log – Annexure-1
2. Sample Integrity Check Form – Annexure-2
3. Freezer Inventory Sheet – Annexure-3
4. Rejected Sample Log – Annexure-4

8. References

• ICH M10: Bioanalytical Method Validation
• US FDA Bioanalytical Method Guidance (2022)
• OECD GLP Principles

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 Movement Log

Date	Time	Study Code	Retrieved By	Location
17/04/2025	09:30	BE/XYZ/2025/06	Rajesh Kumar	FZ-02

Annexure-2: Sample Integrity Check Form

Subject ID	Time Point	Label Status	Vial Condition	Remarks
SUB003	2 hr	Clear	OK	—

Annexure-3: Freezer Inventory Sheet

Freezer ID	Study Code	Box ID	Samples Range	Date Stored
FZ-03	BE/XYZ/2025/06	Box-02	SUB001–SUB020	10/04/2025

Annexure-4: Rejected Sample Log

Date	Subject ID	Reason	Disposition	Reviewed By
17/04/2025	SUB010	Label missing	Not used	Sunita Reddy

Revision History:

Revision Date	Revision No.	Details	Reason	Approved By
01/01/2022	1.0	Initial SOP	New Procedure	QA Head
17/04/2025	2.0	Expanded integrity check and rejection criteria	Regulatory Update	QA Head