LC-MS (CAL-0124) – Calibration Documents

Calibration Documents: LC-MS (CAL-0124)

Asset ID CAL-0124
Equipment LC-MS
Equipment Type LC-MS
Department QC
Area/Location Instrument Room
Process Use MS analysis
Parameter Mass accuracy
Units amu
Range Min 0
Range Max 2000
Acceptance Criteria ±0.5
Calibration Frequency (days) 365
Calibration Type External
Traceability ISO17025

Table of Contents

  1. Calibration SOP
  2. Calibration Protocol
  3. Calibration Checklist
  4. Deviation Impact Assessment
  5. Calibration Certificate

Calibration SOP

1. Purpose

The calibration of the LC-MS is performed to ensure the accuracy of mass accuracy measurements, which is critical for maintaining patient safety, ensuring batch quality, and preserving data integrity. Accurate measurements are essential to prevent erroneous results that could impact product quality and regulatory compliance.

2. Scope

  • Asset ID: CAL-0124
  • Equipment Name/Type: LC-MS
  • Department/Area: QC / Instrument Room
  • Process Use: MS analysis
  • Parameter: Mass accuracy
  • Range: 0 – 2000 amu
  • Units: amu
  • Calibration Frequency: 365 days

3. Definitions

  • Calibration: The process of verifying and adjusting the accuracy of an instrument against a standard.
  • Verification: The process of confirming that an instrument meets specified requirements.
  • Adjustment: The act of modifying an instrument to bring it into compliance with specified standards.
  • As Found: The condition of the instrument prior to any adjustments.
  • As Left: The condition of the instrument after adjustments have been made.
  • OOT (Out of Tolerance): A condition where the measurement falls outside the specified acceptance criteria.
  • Drift: The gradual change in an instrument’s output over time.
  • Traceability: The ability to verify the history, location, or application of an item by means of documented recorded identification.
  • Measurement Uncertainty: A parameter that characterizes the range of values within which the true value is asserted to lie.
  • Intermediate Check: A periodic check of an instrument’s performance between calibrations.

4. References

  • Company Metrology SOP [TBD]
  • ISO/IEC 17025 traceability via calibration certificates
  • ALCOA+ principles

5. Responsibilities

  • Technician/Metrology: Perform calibration and maintain records.
  • QC/QA Reviewer: Review calibration results and documentation.
  • Owner Department: Ensure equipment is available and in good condition for calibration.
  • External Service Provider: Conduct external calibration as per the calibration type.

6. Safety & Preconditions

  • Environmental controls: Ensure temperature and humidity are within specified limits.
  • Warm-up/Stabilization: Allow the instrument to stabilize for [TBD] minutes before calibration.
  • Cleanliness: Ensure the instrument and surrounding area are clean and free from contaminants.
  • Leveling: Verify that the instrument is properly leveled.
  • Power Supply Checks: Confirm that the power supply is stable and within specifications.
See also  Incubator Temp Sensor (30-35°C) (CAL-0155) - Calibration Documents

7. Standards & Tools

  • Reference Standards: [TBD]
  • Traceability Statement: Calibration will be traceable to ISO17025.
  • Certificate Validity Check: Ensure all reference standards are within their validity period.
  • Standard ID: [TBD]

8. Calibration Strategy

The calibration will follow an As Found then As Left logic. The minimum number of test points will be five, including endpoints and midpoints. It is recommended to take three replicate readings at each point to ensure accuracy.

9. Step-by-Step Procedure

  1. Preparation: Gather all necessary tools and reference standards.
  2. Stabilization: Allow the LC-MS to warm up for [TBD] minutes.
  3. As Found Checks and Data Capture: Measure the mass accuracy at defined points and record the data contemporaneously.
  4. Adjustment Rules: If any measurement is OOT, follow the adjustment protocol; if adjustments are not allowed, escalate to QA.
  5. As Left Verification: Re-measure the mass accuracy to confirm adjustments are within acceptance criteria.
  6. Labeling + Documentation Completion: Complete all required documentation and label the equipment with calibration details.

10. Acceptance Criteria & Calculations

The acceptance criteria for mass accuracy is ±0.5 amu. The error calculation formula is:

Error = Observed Value – True Value

Pass/Fail Logic: If the absolute value of the error is less than or equal to 0.5 amu, the calibration passes; otherwise, it fails.

Rounding Rule: [TBD]

11. Handling OOT / Failures

  • Immediate Containment: Tag the equipment and cease use until resolved.
  • Notification & Deviation Initiation: Notify QA and initiate a deviation report.
  • Impact Assessment Trigger: Define the impact window and review affected results/batches.
  • Recalibration After Repair/Adjustment: Ensure recalibration is performed after any adjustments.
  • QA Disposition: [TBD]

12. Records & Retention

  • Logbook Entries: Document all calibration activities in the logbook.
  • Calibration Report/Certificate Filing: Maintain a file of calibration reports and certificates.
  • E-Records: [TBD]
  • Label Content Requirements: Include calibrated date, due date, technician name, and status.

13. Annexures

Annexure A: Calibration Data Sheet

Test Points Reference Observed Error Acceptance Pass/Fail As Found As Left
[TBD] [TBD] [TBD] [TBD] [TBD] [TBD] [TBD] [TBD]
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Annexure B: Quick Checklist

  • Environmental conditions checked
  • Instrument warm-up completed
  • Calibration standards verified
  • Documentation ready

Annexure C: Example Label Text

Calibration Date: [TBD]

Due Date: [TBD]

Calibrated By: [TBD]

Status: [TBD]

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Calibration Protocol

Calibration Protocol

Protocol ID Asset ID Equipment Name Equipment Type Dept Area Process Use Parameter Units Range Acceptance Criteria Frequency Calibration Type Traceability
[TBD] CAL-0124 LC-MS LC-MS QC Instrument Room MS analysis Mass accuracy amu 0 – 2000 ±0.5 365 days External ISO17025

Environmental Conditions

Temperature: [TBD]

Relative Humidity: [TBD]

Vibration: [TBD]

Drafts: [TBD]

Test Point Selection

  • Minimum: 0 amu
  • 25%: 500 amu
  • 50%: 1000 amu
  • 75%: 1500 amu
  • Maximum: 2000 amu

Results Table

Test Point Ref Value Observed (As Found) Error Limit Pass/Fail Observed (As Left) Error Pass/Fail
0 amu [TBD] [TBD] [TBD] ±0.5 [TBD] [TBD] [TBD] [TBD]
500 amu [TBD] [TBD] [TBD] ±0.5 [TBD] [TBD] [TBD] [TBD]
1000 amu [TBD] [TBD] [TBD] ±0.5 [TBD] [TBD] [TBD] [TBD]
1500 amu [TBD] [TBD] [TBD] ±0.5 [TBD] [TBD] [TBD] [TBD]
2000 amu [TBD] [TBD] [TBD] ±0.5 [TBD] [TBD] [TBD] [TBD]

Stepwise Instructions

  1. Preparation: Ensure the LC-MS is clean and calibrated according to the manufacturer’s specifications.
  2. Stabilization: Allow the instrument to stabilize for at least [TBD] minutes before taking measurements.
  3. Performing Readings: Take three replicate readings at each test point.
  4. Calculating Error: Calculate the error for each reading using the formula: Error = Observed – Ref Value.
  5. Evaluation: Compare the calculated error against the acceptance criteria of ±0.5 amu.
  6. Documentation: Record all observations in the results table and ensure data integrity (ALCOA+).

Deviation Instruction for OOT

  • Stop use of the equipment immediately.
  • Notify the QA department.
  • Open a deviation report.
  • Quarantine impacted results window: [TBD]
  • Await QA decision on further actions.

Approvals

Prepared Reviewed Approved
[Signature/Date] [Signature/Date] [Signature/Date]

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Calibration Checklist

Asset ID Equipment Dept Area Parameter Range Acceptance Frequency Traceability
CAL-0124 LC-MS QC Instrument Room Mass accuracy 0 – 2000 amu ±0.5 365 days ISO17025

Pre-calibration

  • [ ] Verify environmental conditions are within specifications
  • [ ] Ensure equipment has been warmed up
  • [ ] Clean the equipment as per SOP
  • [ ] Level the equipment if necessary
  • [ ] Check validity of reference standards
  • [ ] Ensure logbook is ready for entries
See also  Inline Conductivity Sensor (PW) (CAL-0094) - Calibration Documents

As Found Execution

  • [ ] Set initial measurement setpoints
  • [ ] Perform repeat measurements
  • [ ] Record all raw data accurately
  • [ ] Perform necessary calculations

OOT Immediate Actions

  • [ ] Tag out the equipment
  • [ ] Stop use of the equipment
  • [ ] Notify the supervisor
  • [ ] Document deviation
  • [ ] Trigger impact review

As Left Verification

  • [ ] Conduct post-adjustment checks
  • [ ] Confirm all measurements are within acceptance limits

Documentation & Closure

  • [ ] Update equipment label
  • [ ] Attach calibration certificate
  • [ ] Obtain reviewer sign-off
  • [ ] Update next due date in logbook

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Deviation Impact Assessment

Event Summary
Asset: LC-MS
Date: [TBD]
Discovered By: [TBD]
Document References: [TBD]
As Found Results Summary: [TBD]

Immediate Containment Checklist

  • Stop use of the equipment
  • Label/Tag the equipment as out of tolerance
  • Segregate impacted work

Define Impact Window

Last known in-tolerance date: [TBD] to discovery date: [TBD]

Product/Batch/Test Impact Review

Batch/Study/Report ID Results Potentially Impacted Re-test/Re-weigh Decision
[TBD] [TBD] [TBD]

Data Integrity Review Prompts (ALCOA+)

  • Attributable: [TBD]
  • Legible: [TBD]
  • Contemporaneous: [TBD]
  • Original: [TBD]
  • Accurate: [TBD]
  • Complete: [TBD]
  • Consistent: [TBD]
  • Enduring: [TBD]
  • Available: [TBD]

Risk Assessment

Severity Probability Detectability Rationale Overall Risk
[TBD] [TBD] [TBD] [TBD] [TBD]

Investigation Summary

Root Cause: [TBD]

CAPA Plan

Action Owner Due Date Effectiveness Check
[TBD] [TBD] [TBD] [TBD]

QA Disposition

Release/Hold/Retest/Recall Triggers: [TBD]

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Calibration Certificate

Certificate No: [TBD]

Date: [TBD]

Next Due Date: [TBD]

Asset Details

Asset ID Equipment Name Equipment Type Dept Area Make/Model Serial No Location Parameter/Range/Units Acceptance Criteria
CAL-0124 LC-MS LC-MS QC Instrument Room [TBD] [TBD] [TBD] Mass accuracy (0 – 2000 amu) ±0.5

Conditions

Environment: [TBD]

Reference Standards

Standard Name/ID Certificate No Due Date Traceability Statement
[TBD] [TBD] [TBD] Traceability: ISO17025

Results

As Found Results

Test Point Result (amu)
1 [TBD]
2 [TBD]
3 [TBD]
4 [TBD]
5 [TBD]

As Left Results

Test Point Result (amu)
1 [TBD]
2 [TBD]
3 [TBD]
4 [TBD]
5 [TBD]

Measurement Uncertainty Statement: [TBD]

Statement of Conformity: [Pass/Fail]

Remarks: [TBD]

Signatures

Performed by: ______________________ Date: ___________

Checked by: ______________________ Date: ___________

Approved by: ______________________ Date: ___________

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