to ensure reliable, reproducible, and accurate performance throughout the method development lifecycle.

2. Scope

This SOP is applicable to all analytical instruments used in the AMD laboratory including but not limited to HPLC, GC, UV-Vis spectrophotometers, pH meters, balances, FTIR, dissolution testers, and conductivity meters.

3. Responsibilities

• Instrument Owner: Ensures calibration is scheduled and performed as per SOP, maintains calibration logs.
• Calibration Personnel: Conduct calibration activities using certified standards and document results.
• QA: Reviews and approves calibration records and nonconformances if applicable.
• Head – AMD: Ensures instruments are not used if calibration is overdue or out-of-tolerance.

4. Accountability

The Head of AMD is accountable for ensuring that no analytical method development activity is conducted on instruments with expired, failed, or overdue calibration status.

5. Procedure

5.1 Calibration Planning

1. Maintain a centralized Calibration Master Schedule covering all instruments.
2. Frequency to be based on:
   • Manufacturer’s recommendation
   • Instrument usage
   • Historical performance
3. Document schedule in Annexure-1: AMD Instrument Calibration Schedule.

5.2 Pre-Calibration Preparation

1. Ensure instrument is clean, in idle state, and under GMP control.
2. Use certified reference materials (CRMs) or NIST-traceable standards.
3. Ensure environmental conditions are suitable (temperature, humidity, power).

5.3 Calibration Execution

1. Follow instrument-specific calibration SOPs (e.g., SOP/INST/HPLC/011/2025).
2. For example:
   • HPLC: Flow rate, wavelength accuracy, injection precision
   • pH Meter: Two-point buffer calibration
   • Balance: Internal and external standard weights
3. Record observations in Annexure-2: Instrument Calibration Log Sheet.

5.4 Acceptance Criteria

1. Define specific tolerance limits per equipment:
   • pH meter: ±0.05 units
   • UV wavelength: ±1 nm
   • Balance: ±0.1 mg for 200 mg standard
2. Results outside limits to be treated as calibration failure and investigated.

5.5 Post-Calibration Actions

1. Affix calibration label with:
   • Calibration date
   • Next due date
   • Initials of calibration personnel
2. Update calibration tracker and submit record for QA review.
3. Record results in Annexure-3: Instrument Calibration Summary Register.

5.6 Out-of-Tolerance and Failures

1. If calibration fails:
   • Label instrument as “Out of Calibration”
   • Initiate deviation via SOP/QMS/045/2025
   • Perform impact assessment on previous usage
2. Recalibrate after correction or service. Document rework in Annexure-4: Calibration Deviation Report.

5.7 Recalibration and Unplanned Events

1. Recalibrate in case of:
   • Instrument relocation
   • Software/hardware upgrade
   • Electrical surge, major repair
2. QA may waive recalibration based on risk-based justification.

6. Abbreviations

• AMD: Analytical Method Development
• QA: Quality Assurance
• CRM: Certified Reference Material
• NIST: National Institute of Standards and Technology
• SOP: Standard Operating Procedure

7. Documents

1. AMD Instrument Calibration Schedule – Annexure-1
2. Instrument Calibration Log Sheet – Annexure-2
3. Instrument Calibration Summary Register – Annexure-3
4. Calibration Deviation Report – Annexure-4

8. References

• ICH Q10 – Pharmaceutical Quality System
• USP <1058> – Analytical Instrument Qualification
• WHO TRS 986 Annex 1 – Equipment Calibration
• 21 CFR Part 211.68 – Automatic, Mechanical, and Electronic Equipment

9. SOP Version

Version: 2.0

10. Approval Section

	Prepared By	Checked By	Approved By
Signature
Date
Name
Designation
Department

11. Annexures

Annexure-1: AMD Instrument Calibration Schedule

Instrument	ID	Calibration Frequency	Last Calibrated	Next Due
UV-Vis	UV-03	Monthly	01/05/2025	01/06/2025

Annexure-2: Instrument Calibration Log Sheet

Date	Parameter	Expected	Observed	Status
02/05/2025	Wavelength	245 nm	244.9 nm	Pass

Annexure-3: Instrument Calibration Summary Register

Instrument	Calibration Date	Calibrated By	Status	Remarks
HPLC-02	03/05/2025	Ajay Mehra	Pass	Routine

Annexure-4: Calibration Deviation Report

Deviation ID	Date	Instrument	Nature of Deviation	Action Taken
DEV/CAL/2025/014	05/05/2025	pH Meter	Buffer drift	Recalibrated and replaced buffer

Revision History:

Revision Date	Revision No.	Details	Reason	Approved By
04/05/2025	2.0	Expanded sections for deviation handling and recalibration triggers	Audit recommendation