Standard Operating Procedure for Handling Out of Calibration

1.0 Purpose:

To lay down a procedure for Handling out of Calibration observed in Quality Control Laboratory.

2.0 Scope:

The Scope of this SOP is applicable for Handling out of Calibration observed in Quality Control Laboratory.

3.0 Responsibility:

QC Personnel:

To calibrate the instruments as per the Calibration Schedule, To Intimate Supervisor about the out of Calibration results.

Section Head-QC/ Designee:

To Investigate the OOC investigation report, To prepare the OOC investigation report, To arrange service engineer visit to rectify the failure for OOC.

Head QC / Designee:

To ensure that the instruments are calibrated as per the calibration schedule and as per the calibration procedure, To Intimate Head QA/Designee about the “Out of Calibration”, To approve the action plan and proposed hypothesis testing.

Head QA/ Designee:

To approve the action plan and approval of “Out Of Calibration”.

Site Quality Head:

To approve the final “Out Of Calibration” investigation report.

4.0 Definitions:

5.0 Procedure:

5.1 The Instrument shall be calibrated as per the defined SOP and Calibration Schedule.

5.2 During the calibration of any instrument, if the calibration results are found to be “Out of acceptance criteria”, then immediately stop using the instrument and label it as “OUT OF CALIBRATION” as per the respective format.

5.3 Immediately inform the Section Head QC/Designee for further action.

5.4 The Section Head-QC/Designee shall inform the Head QC/Designee. The Head QC/Designee shall further inform the Head QA/Designee.

5.5 For the investigation of an out-of-calibration event, QC personnel shall raise a requisition for the “Out of Calibration Investigation Form” as per the respective format and a new calibration worksheet issuance form.

5.6 After receiving the requisition from the QC department, QA shall issue the “Out of Calibration” Investigation Form and a new calibration worksheet.

5.7 The QA Person shall assign a number to the “Out of Calibration Investigation Form”.

5.8 The QA Person shall make necessary entries in the “Out of Calibration Form Issuance Logbook”.

5.9 The OOC investigation report shall include, but is not limited to, the following points:

• Description of OOC: Mention the details of calibration failure like Test name, Calibration limit, result obtained during calibration.

• Background: Include details like previous calibration history, previous preventive maintenance history, and any abnormalities observed during present and previous calibrations.

• Investigation: Verify points including but not limited to,

o Review of analytical data & electronic data o Physical verification of instrument o Benchtop glassware’s verification

o Verification of analyst training record o Analyst interview

o Verification of chromatographic condition/method or whichever is applicable o Historical data review like standard response, chromatograms, system suitability parameters etc.

o Instrument history

o Details of service engineer visit

o Details of current calibration failure

• Impact Assessment: Check the analysis data performed between the previous and current calibration and review the impact of failure on products that were analyzed or processes that were measured. This can be done by reviewing but not limited to Sequential Log, Instrument Usage Log, Equipment History card and mention in the column.

• Conclusion: The conclusion of investigation should be mentioned based on the root cause identified during investigation.

5.10 Mention instrument and measuring device details in the investigation checklist.

5.11 If the investigation reveals an obvious error and there is sufficient data available to explain the discrepancy, then repeat calibration shall be performed.

5.12 If required, hypothesis testing and failure mode analysis shall be performed based on the preliminary investigational assessment to identify the root cause.

5.13 After recalibration, if the results are found within acceptance criteria, invalidate the initial OOC results for respective test.

5.14 If preliminary investigational assessment demonstrates that there is no root cause, then an extended investigation shall be carried out with help from a service engineer.

5.15 If no assignable root cause is identified after a thorough investigation, recalibration activity shall be performed under supervision of section in-charge.

5.16 A formal review shall be conducted as per Investigation form and an action plan shall be designed for affected product/process.

5.17 Under guidance from Head QA/Designee, Head QC/Designee shall review for,

• Description of “Out of Calibration”

• Any supporting criteria like System Suitability, System Performance

• Impact analysis for product/process which were analyzed/measured during calibration timeframe

5.18 Prepare an Action Plan after reviewing impact and description of “Out of Calibration”.

5.19 The Action Plan shall include, but not be limited to, the analysis of the Control Sample, which is analyzed on that particular Instrument.

5.20 In case other supporting data are available that can justify the impact, it may not be necessary to analyze the entire impacted product. These details need to be clearly mentioned in the Action Plan and justified.

5.21 Implement the Action Plan as per the suggestions.

5.22 After the completion and implementation of the Action Plan, the Head – QC/Designee and Head QA/Designee shall review the data and decide on appropriate action for the affected product. This may include, but is not limited to, product recall or informing customers if there is a failure of sample analysis.

5.23 After the completion of Corrective action, OOC shall be closed, while for preventive action, the CAPA form shall remain open.

5.24 “Out of Calibration” shall be closed out by QA after a thorough review of the action plan, execution, data review, and action. A conclusion shall be drawn based on the findings.

5.25 The final approval of the “Out of Calibration” report shall be done by Head QC/Designee & Head QA/Designee and Site Quality Head/Designee.

5.26 Parallel activities shall be carried out to rectify the instrument/measuring device and recalibration shall be performed before putting it into actual practice.

5.27 “Out of Calibration” shall be reported in the Instrument History Card.

6.0 Acceptance Criteria:

As per respective Calibration Protocol.

7.0 Frequency:

As and when Instrument is found “Out of Calibration”.

8.0 Format for recording:

8.1 Format for “OOC Investigation Form”

OOC Investigation No. : __________________

Date of OOC Investigation

Date of OOC Observed

Date of Laboratory

Investigation initiated

Name of the Instrument:

Instrument Id.:

Previous calibration date:

Calibration Parameter:

Calibration SOP No.:

Obtained Result:

Calibration Acceptance Limit:

OOC details:

Potential impact assessment:

Analyst Interview:

Potential Laboratory Error
Absence of transcription and calculation errors?
Correct method and method version used?
Method properly executed?
Recall any special occurrences during the testing of the sample(s) that could have contributed to result?
Could glassware have been contaminated?
Was glassware used cracked or chipped?
Was the correct glassware used?
Was the laboratory equipment operating normally prior to this testing process?
Were the correct instrument parameters used (i.e., correct wavelength, etc.)?
Was the laboratory equipment in proper working order (i.e., no leaks, air bubbles, etc.)?
Are standards chromatograms are typical in appearance?
Are the standard within expiration date?
Were the reagent solutions correctly prepared and within expiration date?
Was correct column used?
Was integration optimized?
Excessive base line noise?
Was any volumetric solution properly standardized and within expiration date?
Are the users training records adequate & up to date?
Is there any adverse environmental conditions?
All concurrent data typical/acceptable?
Any other potential contributory observations?

List all other calibration testing along with results already completed prior to this OOC results:

Analyst Summary:

QC Supervisor Comments:

Analyst Name: Sign/Date

QC Supervisor Name: Sign/Date

QA Supervisor Name: Sign/Date

Investigational Testing Plan

Investigational Testing to be performed: (Tick mark (√) which is applicable)

□ Re-injection/Re-scan of original standard solution

□ Re-vial of original standard solution

□ Re-mix (shake or Sonication) and re-measurement of original standard solution

□ Re-mix (shake or Sonication) and new dilutions (if applicable) of stock standard Preparation.

Other hypothesis plan if any:

QC Supervisor Name: Sign/Date:

Head-QC / Designee Name: Sign/Date:

QA Supervisor Name: Sign/Date :

“Investigational Testing Summary”

Results from Investigational testing performed (outline here list of Investigational testing performed along with results):

Hypothesis conclusion:

Data transcription Done By:

(Sign and date) Verified By:

(Sign and date)

Root cause identified: (Tick mark on applicable)

[ ] YES (Assignable root cause identified)-Propose immediate corrective action

[ ] NO ( Extended investigation)

Corrective action:

QC Supervisor Name: Sign/Date:

Head QC / Designee Name: Sign/Date:

Head QA / Designee Name: Sign/Date :

In case of ‘No’ root cause (Extended investigation required if):

Re-visit of initial & hypothesis analysis data
Evaluation through Service engineer
Historical data verification
Failure mode analysis

Supervisor comments:

Investigational conclusion:

Corrective actions:

QC Supervisor Name: Sign/Date:

Head QC/ Designee Name: Sign/Date:

Head QA / Designee Name: Sign/Date:

Investigation Findings:

Consideration of results:

CAPA No. (If applicable) :__________________________

Corrective Action Preventative Action Details :

OOC Evaluation

□ Valid

□ Invalid

Instrument release status for further usage:

□ YES

□ NO

Investigation Reviewed By:

Head QC/Designee: (Name & Sign/Date)

Investigation Reviewed By:

Head QA/Designee: (Name & Sign/Date)

Site Quality Head /Designee: (Name & Sign/Date)

8.2 Format for “Out of Calibration Label”.

OUT OF CALIBRATION

Instrument

Instrument No.

Calibration Result

Signature

Date

8.3 Format for “Out of Calibration Form Issuance Logbook”.