HPLC System (CAL-0120) – Calibration Documents

Calibration Documents: HPLC System (CAL-0120)

Asset ID CAL-0120
Equipment HPLC System
Equipment Type HPLC
Department QC
Area/Location Instrument Room
Process Use Chromatography
Parameter Flow rate
Units mL/min
Range Min 0.1
Range Max 5
Acceptance Criteria ±2%
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 HPLC System (CAL-0120) is performed to ensure the accuracy of the flow rate parameter, which is critical for maintaining patient safety and batch quality in the QC department. Proper calibration mitigates risks associated with inaccurate measurements that could lead to compromised data integrity and non-compliance with regulatory standards.

2. Scope

  • Asset ID: CAL-0120
  • Equipment Name/Type: HPLC System / HPLC
  • Department/Area: QC / Instrument Room
  • Process Use: Chromatography
  • Parameter: Flow rate
  • Range: 0.1 – 5 mL/min
  • Units: mL/min
  • Calibration Frequency: 365 days

3. Definitions

  • Calibration: The process of verifying and adjusting the accuracy of an instrument.
  • Verification: The confirmation that an instrument meets specified requirements.
  • Adjustment: The act of modifying an instrument to bring it into compliance with specifications.
  • As Found: The state of the instrument prior to any adjustments.
  • As Left: The state of the instrument after adjustments have been made.
  • OOT (Out of Tolerance): A condition where the measurement falls outside the defined acceptance criteria.
  • Drift: The gradual change in the measurement output of an instrument 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 verification 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 compliance and readiness of the equipment.
  • External Service Provider: Conduct external calibration as per schedule.

6. Safety & Preconditions

  • Ensure environmental controls are in place (temperature, humidity).
  • Allow equipment warm-up/stabilization period as per manufacturer guidelines.
  • Maintain cleanliness of the instrument and surrounding area.
  • Check leveling of the instrument.
  • Verify power supply stability and functionality.
See also  CO2 Incubator Temp Sensor (CAL-0306) - Calibration Documents

7. Standards & Tools

  • Reference Standards Required: [TBD]
  • Traceability Statement: ISO17025
  • Certificate Validity Check: Ensure all calibration certificates are current and valid.

8. Calibration Strategy

Calibration will follow the As Found then As Left logic. A minimum of 5 measurement points will be taken across the specified range (0.1 – 5 mL/min), including endpoints and midpoints. Each point will have 3 replicate readings taken as a best practice.

9. Step-by-Step Procedure

  1. Preparation: Gather all necessary tools and reference standards.
  2. Stabilization: Allow the HPLC System to stabilize for the required period.
  3. As Found checks and data capture: Measure the flow rate at each of the defined points and record raw observations contemporaneously.
  4. Adjustment rules: If any measurement is OOT, escalate for adjustment as per SOP.
  5. As Left verification: Re-measure the flow rate after adjustments and document results.
  6. Labeling + documentation completion: Ensure all calibration records are completed and labeled appropriately.

10. Acceptance Criteria & Calculations

The acceptance criteria for the flow rate is ±2%. The error calculation formula is:

Error (%) = [(Measured Value – Target Value) / Target Value] x 100

Pass/Fail Logic: If the error falls within ±2%, the calibration is considered a pass; otherwise, it is a fail.

Rounding rule: [TBD]

11. Handling OOT / Failures

  • Immediate containment: Tag the equipment and cease 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: Schedule recalibration as necessary.
  • QA disposition: [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
  • Warm-up period completed
  • Cleanliness checked
  • Leveling confirmed
  • Power supply verified

Annexure C: Example Label Text

Calibration Date: [TBD]

See also  ICP-OES (CAL-0116) - Calibration Documents

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-0120 HPLC System HPLC QC Instrument Room Chromatography Flow rate mL/min 0.1 – 5 ±2% 365 days External ISO17025

Environmental Conditions

Temperature: [TBD]

Relative Humidity: [TBD]

Vibration: [TBD]

Drafts: [TBD]

Test Point Selection

Test points for Flow rate (mL/min):

  • Minimum: 0.1
  • 25% of Range: 1.3
  • 50% of Range: 2.5
  • 75% of Range: 3.8
  • Maximum: 5.0

Results Table

Test Point Ref Value Observed (As Found) Error Limit Pass/Fail Observed (As Left) Error Pass/Fail
0.1 [TBD] [TBD] [TBD] ±0.02 [TBD] [TBD] [TBD] [TBD]
1.3 [TBD] [TBD] [TBD] ±0.03 [TBD] [TBD] [TBD] [TBD]
2.5 [TBD] [TBD] [TBD] ±0.05 [TBD] [TBD] [TBD] [TBD]
3.8 [TBD] [TBD] [TBD] ±0.08 [TBD] [TBD] [TBD] [TBD]
5.0 [TBD] [TBD] [TBD] ±0.10 [TBD] [TBD] [TBD] [TBD]

Stepwise Instructions

  1. Preparation: Ensure the HPLC system is clean and calibrated as per the last calibration record.
  2. Stabilization: Allow the system to stabilize for at least 30 minutes before taking measurements.
  3. Performing Readings: Take three replicate measurements at each test point.
  4. Calculating Error: Calculate the error for each observed value using the formula: Error = (Observed – Ref Value) / Ref Value * 100.
  5. Evaluation: Compare the calculated error against the acceptance criteria of ±2%.
  6. Documentation: Record all findings in the results table and ensure data integrity (ALCOA+).

Deviation Instruction for OOT

If any observed value is outside the acceptance criteria:

  • Stop use of the HPLC system.
  • Notify the QA department immediately.
  • 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-0120 HPLC System QC Instrument Room Flow rate 0.1 – 5 mL/min ±2% 365 days ISO17025

Pre-calibration

  • [ ] Verify environmental conditions are within specified limits
  • [ ] Ensure HPLC system has been warmed up for the required time
  • [ ] Clean the equipment as per SOP
  • [ ] Level the HPLC system
  • [ ] Check validity of reference standards
  • [ ] Ensure logbook is ready for recording
See also  Airborne Particle Counter (CAL-0173) - Calibration Documents

As Found Execution

  • [ ] Record initial setpoints for flow rate
  • [ ] Perform repeat measurements as required
  • [ ] Record raw data accurately
  • [ ] Perform necessary calculations for analysis

OOT Immediate Actions

  • [ ] Tag out the equipment
  • [ ] Stop use of the HPLC system
  • [ ] Notify the appropriate personnel
  • [ ] Document deviation
  • [ ] Trigger impact review

As Left Verification

  • [ ] Conduct post-adjustment checks
  • [ ] Confirm all parameters 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 Details
Asset HPLC System
Date [TBD]
Discovered By [TBD]
Document References [TBD]
As Found Results Summary [TBD]

Immediate Containment Checklist

  • Stop use of the HPLC System
  • Label/Tag the equipment as out of service
  • Segregate impacted work

Define Impact Window

Last Known In-Tolerance Date Discovery Date
[TBD] [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-0120 HPLC System HPLC QC Instrument Room [TBD] [TBD] [TBD] Flow rate (0.1 – 5 mL/min) ±2%

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 Measured Value (mL/min) Deviation
1 [TBD] [TBD]
2 [TBD] [TBD]
3 [TBD] [TBD]
4 [TBD] [TBD]
5 [TBD] [TBD]

As Left Results

Test Point Measured Value (mL/min) Deviation
1 [TBD] [TBD]
2 [TBD] [TBD]
3 [TBD] [TBD]
4 [TBD] [TBD]
5 [TBD] [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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