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Elango Minnoor, Ph.D., M.B.A.,Sr. Manager, Quality Control, Biocon Ltd
AgendaIntroductionEquipment/Instrument Qualification
Equipment/Instrument Calibration
Conclusion
Equipment/Instrument - ClassificationAll analytical devices can be classified under 2
categories viz. Equipment and Instrument.
Lab’s Goal - Reliable ResultsReliable instruments
Buying the right instrumentEnsuring its performance (accuracy, precision, etc)
Validity of analytical methodsProper training of analysts
Choosing the Right InstrumentStart with Accurate Monitoring Instruments:
No matter how sophisticated the calibration procedure is, it cannot compensate for the inherent performance limits of the instruments it calibrates.
No amount of calibration or re-calibration will improve the accuracy of an instrument as a measuring device.
Choosing the Right Instrument - ContdIs the instrument calibration NIST traceable?
Tells about the instrument/standard that was used for calibration
Nothing about the performance of the test instrument itself
Components of Analytical Instruments• The collective analytical measurement instruments, in
conjunction with firmware, assembled to perform a mechanical process.
• A device or collection of components that perform a process to produce a result
Instrument Procurement and Life Cycle
Why is Qualification & Calibration Necessary?Qualification
It basically proves that the equipment works correctly and actually leads to accurate and reliable results
CalibrationEnsures that on an on-going basis that the equipment is
performing properlyOften times, these tests are sub-set of the qualification
tests performed
Responsibility• "Users are ultimately responsible for instrument
operations and data quality. The user's group encompasses analysts, their supervisors, instrument specialists and organization management.”
• "Users should also be responsible for qualifying/calibrating their instruments, because their training and expertise in the use of instruments make them the best-qualified groups to design the instrument test(s) and specification(s) necessary for successful AIQ."
Classification of instrumentsClassify instruments into Group A, B and CGroup A
No measurement capability or requires calibration
Mixers, centrifuges, etcGroup B
Providing measurements or controlling physical parameters such as temperature, pressure,etc
Balance, thermometer, pH meterGroup C
Sophisticated instruments such as HPLC, GC, etc
Qualification - Four QsDesign Qualification (DQ)Installation Qualification (IQ)Operational Qualification (OQ)Performance Qualification (PQ)
Design Qualification• Documented collection of activities that defines
functional and operational specifications/requirements
• Criteria for selecting the vendor• Details the conscious decisions of the selection
of the supplier
Design Qualification - URSDefine location, shape and area neededDefine equipment (shelves, drawer needed?)Define safety and environmental aspects (fire
detector)Define security requirements (on-line
monitoring, locking system)Define budgetDefine basis and scale of qualification
Installation Qualification - IQ• Establishes that the instrument is delivered
as designed and specified, that it is properly installed in the selected environment, and that this environment is suitable for the operation and use of the instrument
• When to do:• After system reconfiguration
-Addition of modules-After system relocation.
Installation Qualification - IQRequirements
Description: Provides a description of the instrument including all components including serial number, hardware version, location, etc
Delivery: Ensure that all the components, manual and spares have arrived as per PO
Utility/Facility/Environment: Installation site meets manufacturer’s requirement
Assembly & Installation: Assemble, install and do preliminary diagnostics
Network & Data Storage: Connect to network and check functionality
Operational Qualification• The goal of this test is to demonstrate that the
system operates as intended after placement in a user's environment
• OQ verifies key aspects of instrument performance without the aspects of any contributory effects that could be introduced by a method.
• Verify that the main operating parameters—injection volume, flow rate, mobile-phase mixing, column thermostating temperature, and detection wavelength are within their specified limits for accuracy and precision.
Performance Qualification - PQDemonstrate that instrument performs
consistently as per specifications defined by the user and is appropriate for the intended use
Requirements Set up experiments to verify the performance
of the instrumentWhen to do:
• After Preventive Maintenance• After major module service• After system reconfiguration
Calibration Program – Quality System
System must be in place to ensure that all instruments are calibrated and also to prevent use of an instrument that is not calibrated, unusable due to damage or malfunction, or has exceeded its established calibration interval
System must be in place that identifies instruments that do not require calibration to be performed beyond the original or factory calibration to distinguish from those instruments that do require scheduled calibrations
Calibration Frequency
manufacturer’s recommendationsrelevant procedures – sensitive?instrument performance historyoverall impact of non-compliances in the
calibration process and previous experience of the laboratory technical staff.
Unplanned Calibration
“Unplanned” Calibration can be called for:
When the instrument is physically moved to a different location within a lab
Questionable or ambiguous results are obtained – perhaps as a part of investigation
Calibration SpecificationInstrument calibration tolerance limits should be
established so problems are identified and corrected in a timely manner
When assigning tolerances, considerations given to: Capability of the instrument being calibrated (what
the manufacturer claims the instrument can achieve).Parameters at which the instrument operates (ex: if
testing accuracy of + 0.5% is required, the instrument calibration tolerances should be <0.5%)
Work environment - environmental conditions can affect the performance of the instrumentation
Success of CalibrationSuccess of calibration depends on the
following :Consistency of results obtainedRecognition and mitigation of
outlier/potential outliersScientifically designed calibration
frequency
Calibration – Quality SystemSpecific DirectionsSchedulesLimits of accuracy & precisionRemedial ActionsSystems to prevent usage of instruments
failing calibration
Tracking Instruments for Calibration Status
Each instrument given a unique identifierInstrumentation details associated with this
number must be documented and available (e.g. serial number, model number, location, etc.)
Each instrument should be labeled with the unique identifier
Calibration status of each instrument , the date of calibration, the next calibration date and the identification of person performing calibration should be readily available
Appropriate systems to document calibration status include calibration logs and calibration stickers
Calibration ProcessWritten calibration procedures that use
traceable calibration standards or calibration equipment.
Qualified individuals (having the appropriate education, training, background and experience) responsible for calibrating & maintaining instrumentation
Second person check of all calibration testsQualified individuals responsible for monitoring
the calibrationEnsure the calibration program and procedures
are reviewed and approved by Quality
Calibration Process - ContdEach calibration & maintenance procedure should
include the following:Identification of department responsible to perform the
calibration or maintenanceStep-by-step calibration instructions, reference to
appropriate calibration procedures or instrument manuals
Methods for preventive maintenance or reference to appropriate instrumentation manuals
Calibration equipment used in the calibration are valid (e.g. spectroscopy filters, voltmeters, digital thermometers, etc)
Calibration parameter and tolerance ( + )
Out-of-Calibration Procedure
If calibration is not complete within time.Results from the calibration do no meet set criteria.
Identification of CausesTraining of analyst for calibration procedures.Glassware/Standards – Cleanliness, Validity etc.History of malfunction/breakdown and
maintenance.Review of previous calibration report.
Out-of-Calibration Procedure - Contd
Data generated from the successful calibration till the next calibration is evaluated for the “Impact”. If Impact analysis reveals suspect results, random batches/products are picked up and analyzed and results are compared to the ones obtained from OOC instrument.
If the results are different, then appropriate evaluation and justification need to be provided (QC/QA).
Based on the outcome of the investigation, CAPA is implemented and the re-calibration is performed.
Records for CalibrationAll calibration records must be retained per
document retention proceduresShould include “as found” measurements,
results of adjustments (“as left”) and appropriate review & approval of all results
Tolerance or limit for each calibration pointIdentification of standard or test instrument
usedIdentification of persons performing the work
and checking the results with dates
After CalibrationReview must ensure the approved activities
have been completed and all results have passed the established acceptance criteria
Actions to be taken if instrumentation cannot be calibrated (e.g. contact appropriate service people, label and remove from service)
A step to record all calibration & maintenance activities
Periodic review of historic calibration & maintenance data to evaluate appropriateness of established frequencies
HPLC – Calibration TestsInjection Volume
AccuracyPrecisionLinearity
Mobile phaseFlow rate precisionAccuracyPrecision
HPLC – Calibration Tests - ContdColumn Oven
Thermostat accuracyThermostat precision
DetectorsWavelength accuracyResponse linearitySignal-to-noise ratio
ConclusionQualification/Calibration are not optional but
needed for regulatory complianceA strong calibration program ensures:
Highly Efficient LabReliable ResultsQuality ProductPatient Safety
Thank YouAny Questions?