SOP for Calibration of Analytical Instruments in the AMD Laboratory
| Department | Analytical Method Development |
|---|---|
| SOP No. | SOP/AMD/035/2025 |
| Supersedes | SOP/AMD/035/2022 |
| Page No. | Page 1 of 15 |
| Issue Date | 19/05/2025 |
| Effective Date | 20/05/2025 |
| Review Date | 19/05/2026 |
1. Purpose
This SOP defines the procedure for performing and documenting the calibration of analytical instruments used in the Analytical Method Development (AMD) department 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
- Maintain a centralized Calibration Master Schedule covering all instruments.
- Frequency to be based on:
- Manufacturer’s recommendation
- Instrument usage
- Historical performance
- Document schedule in Annexure-1: AMD Instrument Calibration Schedule.
5.2 Pre-Calibration Preparation
- Ensure instrument is clean, in idle state, and under GMP control.
- Use certified reference materials (CRMs) or NIST-traceable standards.
- Ensure environmental conditions are suitable (temperature, humidity, power).
5.3 Calibration Execution
- Follow instrument-specific calibration SOPs (e.g., SOP/INST/HPLC/011/2025).
- For example:
- HPLC: Flow rate, wavelength accuracy, injection precision
- pH Meter: Two-point buffer calibration
- Balance: Internal and external standard weights
- Record observations in Annexure-2: Instrument Calibration Log Sheet.
5.4 Acceptance Criteria
- Define specific tolerance limits per equipment:
- pH meter: ±0.05 units
- UV wavelength: ±1 nm
- Balance: ±0.1 mg for 200 mg standard
- Results outside limits to be treated as calibration failure and investigated.
5.5 Post-Calibration Actions
- Affix calibration label with:
- Calibration date
- Next due date
- Initials of calibration personnel
- Update calibration tracker and submit record for QA review.
- Record results in Annexure-3: Instrument Calibration Summary Register.
5.6 Out-of-Tolerance and Failures
- If calibration fails:
- Label instrument as “Out of Calibration”
- Initiate deviation via SOP/QMS/045/2025
- Perform impact assessment on previous usage
- Recalibrate after correction or service. Document rework in Annexure-4: Calibration Deviation Report.
5.7 Recalibration and Unplanned Events
- Recalibrate in case of:
- Instrument relocation
- Software/hardware upgrade
- Electrical surge, major repair
- 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
- AMD Instrument Calibration Schedule – Annexure-1
- Instrument Calibration Log Sheet – Annexure-2
- Instrument Calibration Summary Register – Annexure-3
- 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 |