Calibration Documents: GC-MS (CAL-0125)

Asset ID	CAL-0125
Equipment	GC-MS
Equipment Type	GC-MS
Department	QC
Area/Location	Instrument Room
Process Use	MS analysis
Parameter	Mass accuracy
Units	amu
Range Min	0
Range Max	1000
Acceptance Criteria	±0.5
Calibration Frequency (days)	365
Calibration Type	External
Traceability	ISO17025

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Calibration SOP

1. Purpose

The calibration of the GC-MS (Asset ID: CAL-0125) 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 compliance with regulatory standards.

2. Scope

• Asset ID: CAL-0125
• Equipment Name/Type: GC-MS
• Department/Area: QC / Instrument Room
• Process Use: MS analysis
• Parameter: Mass accuracy
• Range: 0 – 1000 amu
• Units: amu
• Calibration Frequency: 365 days

3. Definitions

• Calibration: The process of verifying and adjusting the accuracy of an instrument against a recognized 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 made during calibration.
• As Left: The condition of the instrument after adjustments have been made during calibration.
• OOT (Out of Tolerance): A condition where the instrument’s measurements fall outside the defined acceptance criteria.
• Drift: The gradual change in an instrument’s measurement accuracy 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 associated with the result of a measurement that characterizes the dispersion of the values that could reasonably be attributed to the measurement.
• Intermediate Check: A verification process conducted between calibrations to ensure ongoing accuracy.

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 compliance with calibration schedules.
• External Service Provider: Conduct external calibrations as required.

6. Safety & Preconditions

• Ensure environmental controls are in place (temperature, humidity).
• Allow for warm-up/stabilization of the GC-MS as per manufacturer specifications.
• Maintain cleanliness of the instrument and surrounding area.
• Verify leveling of the instrument.
• Check power supply stability and functionality.

7. Standards & Tools

• Reference standards required: [TBD]
• Traceability Statement: ISO17025
• Certificate validity check: Ensure all calibration certificates are current and valid.
• Standard ID placeholders: [TBD]

8. Calibration Strategy

The calibration will follow an As Found and As Left logic:

• Minimum number of points: At least 5 points including endpoints and midpoints across the range of 0 – 1000 amu.
• Replicate readings: A minimum of 3 repeats at each point is recommended for accuracy.

9. Step-by-Step Procedure

1. Preparation: Gather all necessary tools and reference standards.
2. Stabilization: Allow the GC-MS to warm up for the specified time.
3. As Found checks and data capture: Record initial measurements before any adjustments.
4. Adjustment rules: If OOT is found, follow the adjustment protocol if permitted; otherwise, escalate to QA.
5. As Left verification: Confirm that the instrument is within specifications after adjustments.
6. Labeling + documentation completion: Ensure all calibration records are filled out accurately and contemporaneously (ALCOA+).

10. Acceptance Criteria & Calculations

Acceptance criteria for mass accuracy is ±0.5 amu.

Error calculation formula: Error = Observed Value – True Value

Pass/Fail Logic: If the absolute value of the error is within the acceptance criteria, the calibration passes; otherwise, it fails.

Rounding rule placeholder: [TBD]

11. Handling OOT / Failures

• Immediate containment: Tag the equipment and stop its use.
• Notification & deviation initiation: Notify QA and document the deviation.
• Impact assessment trigger: Define the impact window and review affected results/batches.
• Recalibration after repair/adjustment: Ensure recalibration is performed post-adjustment.
• QA disposition placeholders: [TBD]

12. Records & Retention

• Logbook entries: Document all calibration activities.
• Calibration report/certificate filing: Maintain records in accordance with company policy.
• e-Records if applicable: [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]

Annexure B: Quick Checklist

• Environmental controls verified
• Instrument warm-up completed
• Calibration standards prepared
• 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-0125	GC-MS	GC-MS	QC	Instrument Room	MS analysis	Mass accuracy	amu	0 – 1000	±0.5	365 days	External	ISO17025

Environmental Conditions

Temperature: [TBD]

Relative Humidity: [TBD]

Vibration: [TBD]

Drafts: [TBD]

Test Point Selection

• Min: 0 amu
• 25%: 250 amu
• 50%: 500 amu
• 75%: 750 amu
• Max: 1000 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]
250 amu	[TBD]	[TBD]	[TBD]	±0.5	[TBD]	[TBD]	[TBD]	[TBD]
500 amu	[TBD]	[TBD]	[TBD]	±0.5	[TBD]	[TBD]	[TBD]	[TBD]
750 amu	[TBD]	[TBD]	[TBD]	±0.5	[TBD]	[TBD]	[TBD]	[TBD]
1000 amu	[TBD]	[TBD]	[TBD]	±0.5	[TBD]	[TBD]	[TBD]	[TBD]

Stepwise Instructions

1. Preparation: Ensure the GC-MS is clean and calibrated as per the manufacturer’s guidelines.
2. Stabilization: Allow the instrument to stabilize for [TBD] minutes before performing readings.
3. Performing Readings: Take three replicate readings at each test point.
4. Calculating Error: Calculate the error for each test point 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, errors, and results in the results table.

Deviation Instruction for OOT

If any observed value is outside the acceptance criteria:

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

Approvals

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

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Calibration Checklist

Asset ID	Equipment	Dept	Area	Parameter	Range	Acceptance	Frequency	Traceability
CAL-0125	GC-MS	QC	Instrument Room	Mass accuracy	0 – 1000 amu	±0.5	365 days	ISO17025

Pre-calibration

• [ ] Verify environmental conditions are within specified limits
• [ ] Ensure equipment has been warmed up for the required duration
• [ ] Clean the equipment as per SOP
• [ ] Level the instrument if applicable
• [ ] Confirm validity of reference standards
• [ ] Ensure calibration logbook is ready for entries

As Found Execution

• [ ] Set the instrument to specified setpoints
• [ ] Perform repeat measurements as required
• [ ] Record all raw data accurately
• [ ] Perform necessary calculations for results

OOT Immediate Actions

• [ ] Tag out the instrument
• [ ] Stop use of the instrument immediately
• [ ] Notify the QA department
• [ ] Document deviation from acceptance criteria
• [ ] Trigger impact review as per SOP

As Left Verification

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

Documentation & Closure

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

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Deviation Impact Assessment

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

Immediate Containment Checklist

• Stop use of the asset
• Label/tag the asset 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-0125	GC-MS	GC-MS	QC	Instrument Room	[TBD]	[TBD]	[TBD]	Mass accuracy (0 – 1000 amu)	±0.5

Conditions

Environment: [TBD]

Reference Standards

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

Results

As Found Results

Test Point	Measurement (amu)	Pass/Fail
1	[TBD]	[TBD]
2	[TBD]	[TBD]
3	[TBD]	[TBD]
4	[TBD]	[TBD]
5	[TBD]	[TBD]

As Left Results

Test Point	Measurement (amu)	Pass/Fail
1	[TBD]	[TBD]
2	[TBD]	[TBD]
3	[TBD]	[TBD]
4	[TBD]	[TBD]
5	[TBD]	[TBD]

Measurement Uncertainty Statement: [TBD]

Statement of Conformity: [Pass/Fail overall]

Remarks: [TBD]

Signatures

Performed by: ____________________ Date: ___________

Checked by: ______________________ Date: ___________

Approved by: _____________________ Date: ___________

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