Analytical Method Development (AMD). The procedure emphasizes adherence to ALCOA+ principles to maintain data integrity.

2. Scope

This procedure applies to all chromatographic data generated within the AMD department of pharmaceutical API and formulation development units. It includes both electronic and hard copy data, raw files, processed results, calibration curves, audit trails, and metadata.

3. Responsibilities

• Analyst: Responsible for proper entry, review, and labeling of chromatographic data.
• Reviewer/QA: Verifies completeness, accuracy, and traceability of chromatographic documentation.
• IT Admin/Data Integrity Officer: Ensures system access controls, backup policies, and audit trail management are implemented.

4. Accountability

The Head of Analytical Method Development is accountable for enforcing this SOP and ensuring that all chromatographic data handling complies with regulatory expectations (FDA, MHRA, WHO, EMA, CDSCO).

5. Procedure

5.1 General Principles

1. All chromatographic data must comply with ALCOA+ principles: Attributable, Legible, Contemporaneous, Original, Accurate, Complete, Consistent, Enduring, and Available.
2. Each chromatographic run must be traceable to an authorized method development activity, project, or validation study.

5.2 System Logins and User Access

1. Only authorized personnel shall access chromatographic software (e.g., Empower, Chromeleon, OpenLab).
2. Access must be role-based: Analyst (Data Entry), Reviewer (Data Review), Admin (System Configuration).
3. Audit trails must be enabled for all activities including data acquisition, processing, modification, and deletion.

5.3 Sample Sequence and Data Entry

1. Create a sequence log with sample ID, standard ID, batch number, analyst initials, date, and method file name.
2. Ensure system suitability runs are recorded at the beginning of each batch.
3. Record injections in chronological order, avoiding any overwriting or manual reinjections without justification.

5.4 Review and Approval

1. All chromatograms must be printed or archived electronically with clear identification of analyst, instrument ID, method version, and analysis date.
2. Use the Chromatogram Review Checklist (Annexure-1) to verify peak integrity, integration parameters, system suitability, and calibration data.
3. Reviewer must document comments and any observed discrepancies.

5.5 Data Backup and Security

1. Chromatographic data must be backed up daily through centralized servers or validated data archival systems.
2. Ensure redundant storage with role-based access controls and audit logging of backups.
3. Backups should be validated periodically for restoration capability and completeness.

5.6 Retention and Disposal

1. Retain chromatographic data and reports for a minimum of five years or as per regulatory project lifecycle.
2. Destruction must be authorized and documented as per the Data Retention Policy (Annexure-2).

6. Abbreviations

• HPLC: High Performance Liquid Chromatography
• UPLC: Ultra Performance Liquid Chromatography
• GC: Gas Chromatography
• QA: Quality Assurance
• ALCOA+: Data Integrity Principles

7. Documents

1. Annexure-1: Chromatogram Review Checklist
2. Annexure-2: Data Retention and Destruction Form
3. Annexure-3: Analyst Sequence Log Template

8. References

• FDA Guidance on Data Integrity and Compliance with cGMP
• MHRA GXP Data Integrity Guidance and Definitions
• WHO Technical Report Series No. 996, Annex 5
• 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	Vinay Dubey	Kavita Mehra	Dr. Meenal Joshi
Designation	Senior Analyst – AMD	QA Lead	Head – Analytical Method Development
Department	Analytical Method Development	Quality Assurance	Analytical Method Development

11. Annexures

Annexure-1: Chromatogram Review Checklist

• Sample ID and run sequence verified
• Integration parameters documented and justified
• System suitability met
• Calibration curve linearity acceptable
• Audit trail reviewed and clean

Annexure-2: Data Retention and Destruction Form

Record Type	Date of Generation	Retention Period	Disposal Date	Authorized By
HPLC Data	01/06/2020	5 Years	01/06/2025	QA Head

Annexure-3: Analyst Sequence Log Template

Run ID	Date	Analyst	Sample Details	Instrument ID	Method File
AMD-SEQ-457	01/06/2025	P. Jain	API 100 mg/ml	HPLC-06	AMV-API-HPLC-002

Revision History:

Revision Date	Revision No.	Details	Reason	Approved By
01/06/2025	2.0	Added audit trail and backup procedure	Regulatory Requirement	Dr. Meenal Joshi
15/03/2022	1.0	Initial release	New SOP	QA Head