SOP Guide for Pharma

API Manufacturing: SOP for Review of Chromatograms and Peak Integration – V 2.0

Auditor

API Manufacturing: SOP for Review of Chromatograms and Peak Integration – V 2.0

Standard Operating Procedure for Review of Chromatograms and Peak Integration in API Manufacturing

Department API Manufacturing
SOP No. SOP/API/147/2025
Supersedes SOP/API/147/2022
Page No. Page 1 of 10
Issue Date 13/04/2025
Effective Date 15/04/2025
Review Date 13/04/2026

1. Purpose

To provide a standardized and regulatory-compliant procedure for the review of chromatograms and peak integration for High Performance Liquid Chromatography (HPLC), Gas Chromatography (GC), and other applicable analytical methods used in API manufacturing.

2. Scope

This SOP applies to all analysts, reviewers, and quality assurance personnel involved in reviewing chromatographic data generated in the Quality Control laboratories for raw

materials, intermediates, in-process, and final API products.

3. Responsibilities

  • QC Analyst: Generate, print, and ensure the accuracy of chromatograms and peak integration as per approved STP.
  • QC Reviewer: Review chromatograms and integration parameters to ensure compliance, accuracy, and traceability.
  • QA Officer: Conduct random checks on chromatographic records and ensure compliance with data integrity practices.
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4. Accountability

The Head – Quality Control is accountable for the implementation and compliance of this SOP within the laboratory.

5. Procedure

5.1 General Guidelines

  1. All chromatographic data shall be generated using validated software systems that are password protected and provide an audit trail.
  2. System suitability criteria must be met and documented before analyzing samples.
  3. All chromatograms and associated metadata must be stored in a secure and retrievable manner, both electronically and physically.

5.2 Requirements for Chromatogram Review

  1. Ensure that all chromatograms are complete and include:
    • Sample name, ID, and injection sequence
    • Date and time of injection
    • System suitability data
    • Integration parameters used
  2. Verify that the peak shape, retention time, and resolution match expectations per the standard chromatogram.
  3. Ensure the baseline is stable and no manual baseline corrections are made without justification.

5.3 Peak Integration Review

  1. Peak integration must be performed using predefined and approved software parameters.
  2. Any manual peak integration must be justified with documentation and approved by a reviewer.
  3. The following must be checked:
    • Start and end points of peaks
    • Integration threshold levels
    • Consistency of integration across injections
  4. Ensure no overlapping peaks are incorrectly merged unless justified scientifically.
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5.4 Manual Integration and Justification

  1. Manual intervention should only be done if:
    • Baseline noise interferes with peak detection
    • Software fails to identify a valid peak
    • Known system error or spike is interfering with peak identification
  2. Document:
    • Why manual integration was performed
    • Before-and-after chromatogram comparison
    • Approval of reviewer with signature and date

5.5 Audit Trail and Data Integrity

  1. Ensure audit trail is reviewed in case of:
    • Peak edits
    • Method edits
    • Sequence modifications
  2. Log audit trail findings in the Audit Trail Review Log (Annexure-1).
  3. Do not delete or overwrite original chromatograms.

5.6 Documentation

  1. All chromatograms must be printed, signed by the analyst, and submitted to reviewer.
  2. Reviewer shall sign and date with remarks, if any.
  3. Ensure compliance with ALCOA+ principles:
    • Attributable
    • Legible
    • Contemporaneous
    • Original
    • Accurate
    • Complete, Consistent, Enduring, and Available

6. Abbreviations

  • HPLC: High Performance Liquid Chromatography
  • GC: Gas Chromatography
  • QA: Quality Assurance
  • QC: Quality Control
  • SOP: Standard Operating Procedure
  • ALCOA+: Data Integrity Principles
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7. Documents

  1. Audit Trail Review Log (Annexure-1)
  2. Chromatogram Integration Record (Annexure-2)
  3. Manual Integration Justification Form (Annexure-3)

8. References

  • MHRA Guidance on Data Integrity
  • ICH Q2(R1) – Validation of Analytical Procedures
  • 21 CFR Part 11 – Electronic Records and Signatures

9. SOP Version

Version: 2.0

10. Approval Section

Prepared By Checked By Approved By
Signature
Date
Name
Designation
Department

11. Annexures

Annexure-1: Audit Trail Review Log

Date System Reviewed By Findings Action Taken
13/04/2025 HPLC-05 QA Officer No edits detected Filed

Annexure-2: Chromatogram Integration Record

Date Sample ID Analyst Software Used Reviewer Comments
13/04/2025 SMP-147 Sunita Reddy Empower 3 Integration acceptable

Annexure-3: Manual Integration Justification Form

Date Sample ID Reason Before/After Comparison Attached Approved By
13/04/2025 SMP-147 Spike removed at 3.25 min Yes QA Head

Revision History:

Revision Date Revision No. Details Reason Approved By
01/01/2022 1.0 Initial Version Regulatory Requirement QA Head
13/04/2025 2.0 Added Audit Trail and Justification Forms Audit Feedback QA Head
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