SOP for Handling of Out of Calibration

OBJECTIVE

To lay down a procedure for investigating and handling of out-of-calibration (OOC) measuring devices/Instruments.

SCOPE

This SOP is applicable to Out of Calibration of measuring devices or instruments which are used for testing Raw materials, Packaging materials, Finished Products, and stability samples in the Quality Control Department.

RESPONSIBILITY

Analyst: To perform calibration and report the calibration status.

Section Head: To coordinate with Head-QC regarding OOC results and participate in the investigation for the same.

Head QC: To ensure that this SOP is followed during an investigation of OOC results.

To investigate Out of Calibration.

Head QA: To Investigate Out of Calibration and approval.

ACCOUNTABILITY

Quality Control Head and Quality Assurance Head

DEFINITION

Calibration is a set of operations that establish, under specified conditions, the relationship between values of quantities indicated by a measuring instrument or measuring system, or values represented by a material measure or a reference material, and the corresponding values realized by standards.

It is the setting correcting or adjusting of a measuring device or base level, to match or conform to a known and unvarying measure.

PROCEDURE

• The calibration of instruments is a critical activity and it is carried out to ensure the performance and suitability of the instruments.
• The calibration of instruments, apparatus, gauges, and recording devices at suitable intervals in accordance with an established written program containing specific directions, schedules, limits for accuracy and precision, and provision for remedial action in the event accuracy and /or precision limit is not met.
• Instruments, apparatus, gauges and recording devices not meeting established specifications shall not be used.
• The procedure of calibration of each instrument is mentioned in the SOP of the respective instrument.
• The frequency of each instrument is ± 5 days of defined interval, mentioned in the respective SOP.
• The schedule for calibration is prepared at the beginning of the year as per Annexure No. 01.
• The calibration schedule is checked by the QC Head and approved by the QA Head.

Out of Calibration

• It is defined as a failure to meet the acceptance criteria during the calibration.
• If out-of-calibration results are found, affix a status label “OUT OF CALIBRATION” immediately. The failure to meet the limits during the calibration (OOC) shall be thoroughly investigated to find the root cause, and its impacts and to take corrective and preventive action to avoid the recurrence of such an incidence.
• Since the result is out of calibration, it needs to be checked for analyst/instrument error quickly for the further decision-making process, as below.

ALSO READ: SOP for Handling of Out of Trend (OOT)

A. Analyst error

• Check the competency of the analyst by verifying analyst qualification, training, knowledge and experience, expertise in calibration, any objectionable issue, recording and reporting, and behavioral patterns.

B. Instrument error

• Verify earlier calibration/ qualification records, previous instrument history, cleanliness, chocking/ blocking of the material, preventive engineering status, and physical condition.
• Check standards/ chemicals used for calibration and their validity, Glassware, and instrument consumables spares.
• Check SOP for operation and calibration of the instrument and its format, environment conditions (temperature/humidity), dilution of solution (concentration), relevancy of methodology, calibration frequency, calibration limit too stringent, etc.
• Rectify and repeat the calibration, if an error is observed in the investigation, after approval from quality assurance.
• It will be documented properly and appropriate corrective and preventive action will be taken.
• If no error is found, the instrument is required to be checked and serviced as follows;

1. Inform the Engineering Department to carry out in-house rectification of the instrument.
2. If the in-house Engineering Department can rectify the defect, then use the instrument after proper calibration.
3. In case the in-house Engineering Department is unable to rectify the defect, call the service engineer of the instrument.
4. Once the said instrument is repaired by a small correction or major part replacements based on the recommendation of the service engineer, then carry out calibration and ensure that it is working satisfactorily.
5. If the external expert performs the servicing satisfactorily, use the instrument after calibration for routine analysis.
6. If the external expert fails to rectify the instrument, affix a status label “OUT OF ORDER”.
7. Arrange to replace the instrument for analysis, if available in the lab, or send the sample to an approved external laboratory for testing.
8. If required, based on the recommendations and our assessment, the instrument may be discontinued with proper documentation.

• If no error is found in an investigation related to the instrument, analyst, used materials, and process, product product-related investigation is started.
• It is not possible to judge, the exact date from the instrument was not suitable. The following points are necessary for the product-related investigation.

1. List out the number of samples tested on the suspected instrument.
2. List out the number of samples approved in the recent past.
3. List out a number of samples rejected in the recent past.
4. Review of a trend of analyzed product for confirming OOC period.
5. Check testing methodology and the relevancy of testing methodology.
6. Verify the details of the instruments used.
7. Check analytical data including system suitability/ instrument verification before the start of the analysis.

• All products tested on the suspected instruments are kept on “HOLD”, since earlier successful calibration and labeled appropriately.
• If the OOC period is identified, all products are re-tested on an urgent basis on similar other instruments or alternate instruments or outside the laboratory whatever is feasible.
• If the OOC period is not identified, the last ten batches are selected for re-testing based on the criticality of the test and analyzed on an urgent basis.
• If the re-testing results are found satisfactory, it shows that it is not impacted the product quality. An effective risk assessment is carried out for the efficacy and quality of drug products and safety for patients.
• If any abnormality is observed in re-testing results, the batch/ batches will be recalled from the market as per SOP for Product Recall.
• Available products shall be reprocessed/reworked after appropriate approvals and documentation procedures.
• The instrument calibration frequencies shall be kept in such a way that the situation must be under control in any incidences happening with respect to operation, calibration, and engineering procedures.
• The analyst, who is responsible for calibration and related activities, should be well-trained and experienced in the operation and calibration of the instrument.

ABBREVIATIONS

QC: Quality Control

UV: Ultra Violet

QA: Quality Assurance

OOC: Out Of Calibration

SOP: Standard Operating Procedure

ANNEXURES

Annex. No. 01 - Calibration Schedule

Annex. No. 02 - Label for Out of Calibration

Annex. No. 03 - Label for Out of Order

REVISION HISTORY

Nil

ALSO READ: SOP for Handling Out of Specification (OOS)