reviews raw data for compliance with acceptance criteria.

QA Personnel: Reviews the final data and flags any anomalies or deviations.

Bioanalytical Reviewer: Performs second-level review of integration and calculates precision/accuracy values.

Bioanalytical Head: Approves the analytical run and determines acceptability for reporting.

4. Accountability

The Head of the Bioanalytical Department is accountable for ensuring that analytical runs are conducted and reviewed according to the approved method validation and regulatory requirements.

5. Procedure

5.1 Pre-Run Setup and Controls

1. Verify that the instrument is calibrated and meets system suitability criteria.
2. Prepare calibration standards, quality control (QC) samples, and blank samples according to the validated method.
3. Document the run sequence, including sample positions and file names in the Run Sequence Log (Annexure-1).

5.2 Acceptance Criteria for Calibration Curve

1. At least 75% of non-zero calibrators, including the lowest and highest, must meet the acceptance criteria:
   • Nominal concentration ±15% (±20% for LLOQ)
2. Regression coefficient (r²) should be ≥ 0.98.
3. Evaluate back-calculated concentrations of standards for compliance.

5.3 Quality Control (QC) Sample Acceptance Criteria

1. At least 67% of QC samples should meet ±15% of their nominal concentrations.
2. At least 50% of QC samples at each level (LQC, MQC, HQC) must be within ±15%.
3. Reject the entire run if QC fails to meet the above criteria.

5.4 Run Review Process

1. Perform chromatogram integration using predefined integration parameters.
2. Review each chromatogram for:
   • Retention time consistency
   • Peak shape and area
   • Baseline noise or interference
3. Document observations in the Run Review Checklist (Annexure-2).

5.5 Reinjection and Partial Reanalysis

1. If a sample chromatogram is abnormal:
   • Justify reinjection based on SOP criteria
   • Document the reason and outcome in the Reinjection Log (Annexure-3)
2. Partial reanalysis is allowed if approved by QA and documented appropriately.

5.6 Approval and Documentation

1. Only QA-reviewed and authorized runs are acceptable for final reporting.
2. Each run must be signed off by the analyst, reviewer, QA, and bioanalytical head.
3. Attach run data, chromatograms, and review forms to the Study Master File (SMF).

6. Abbreviations

• SOP: Standard Operating Procedure
• BA/BE: Bioavailability/Bioequivalence
• LLOQ: Lower Limit of Quantification
• QC: Quality Control
• SMF: Study Master File

7. Documents

1. Run Sequence Log – Annexure-1
2. Run Review Checklist – Annexure-2
3. Reinjection Log – Annexure-3

8. References

• ICH M10: Bioanalytical Method Validation
• US FDA Guidance for Industry – Bioanalytical Method Validation (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: Run Sequence Log

File Name	Sample ID	Injection No.	Retention Time	Processed By
BE0501	SUB001_0hr	1	2.53	Ajay Verma

Annexure-2: Run Review Checklist

Parameter	Acceptable (Y/N)	Remarks
Peak Shape	Y	Symmetrical
Baseline	Y	No noise

Annexure-3: Reinjection Log

Date	Sample ID	Reason for Reinjection	Approval By
17/04/2025	SUB009_6hr	Integration error	Sunita Reddy

Revision History:

Revision Date	Revision No.	Details	Reason	Approved By
01/01/2022	1.0	Initial SOP	Method validation alignment	QA Head
17/04/2025	2.0	Updated QC acceptance rules and run review process	ICH M10 Compliance	QA Head