ANALYST QUALIFICATION
PURPOSE of ANALYST QUALIFICATION:
To lay down the procedure for the qualification of analyst in order to confirm that the newly Joined employee analyst and analyst performing tests in quality control laboratory are adequately qualified to produce reliable and accurate results.
SOP SCOPE ANALYST QUALIFICATION:
This SOP applicable to Quality Control
RESPONSIBILITY:
Analyst: Responsible to read and follow the Standard Test Procedure for analyzing the Sample and follow respective SOP on Instrument Analysis and Documentation.
Section In-charge: Initiate and plan Qualification of each analyst/scientist working in laboratory as per procedure, and provide sample for Analyst qualification, and maintain record of Analyst Competency Profile and Qualification Certificate.
Head QC/Head AVL: Head-QC /Designee, Head AVL or designee shall be responsible for ensuring qualification of new joined on analytical technique prior to assigning analysis and requalification at defined frequency.
Quality Assurance: Quality Assurance (QA)/DQA (Development Quality Assurance) is responsible for distribution and control of the SOPs such as issuance, retrieval and archiving.
DEFINITIONS:
Analyst Qualification: Analyst qualification is a process to evaluate proficiency of the analyst to satisfactorily perform analysis using specific analytical technique with desired precision
PROCEDURE:
General Procedure:
HR Personnel shall accompany the newly joined employee to Quality control & Analytical Operations department and shall handover the duly filled Induction training record to the Manager / designate Safety and cGMP related training will be imparted by the responsible departments.
Whenever a new employee joins QC laboratory/AVL, Head-QC designee/Head AVL or designee shall decide the job responsibilities of the analyst.
After completion of the induction and procedural training, a qualification program shall be designed based on the job responsibilities. The analyst shall be assessed by Head-QC / designee, Head AVL or designee or Training coordinator prior to initiation of the qualification” Assessment Report”.
The qualification programmed must include the analytical techniques / tests which the analyst shall be performing while conducting routine analysis on day to day basis. The qualification shall be completed before starting use of the analytical technique for routine analysis.
Analyst qualification programmed may not include non-complex analytical methods like Residue on ignition (sulphated ash), limit tests, acid value, pH, conductivity measurements, and refractive index.
If any analyst is involved in the analytical method transfer/method validation/ method verification on a particular test / technique (i.e.-Method precision/intermediate precision) the analyst shall consider qualified to perform the routine analysis for those test “Qualification Certificate”.
Note: If analysts is involved XRD, DSC, TGA, CHNS, Surface area etc. techniques it shall be consider analyst is qualified for X-Ray diffraction, DSC, TGA, CHNS, Surface area techniques.
Note: If any analyst/scientist is involved in the Instrument Qualification/Schedule Calibration on Instruments, the analyst shall be consider as qualified to perform the routine Calibration only (Not eligible to perform the routine analysis) and same shall be maintained Qualification certificate.
The Head-QC /designee, Head AVL or designee shall decide and schedule analyst qualification for existing analyst on any new test and techniques considering the job responsibility which shall be assigned in future.
New Joined can complete the training of a particular section /system /technique by getting trained on that section /system /technique related SOPs & hands on training on that particular work area, then based on the completed training, new Joined can be certified as competent person for that particular section/ system /technique & he/she can start the routine activity of that section/ system /technique.
For Example: If any new Joined of QC Department/AVL, completed all the SOPs related to HPLC operation along with other related SOPs (e.g. Weighing balance, Mobile phase preparation but not limited to) & also completed the Analyst qualification on test HPLC analysis (e.g. Assay, Related substances and chromatographic purity but not limited to), then he/she can be certified for analysis on HPLC instrument for those particular tests and remaining qualification can be completed later on.
All the Analyst /Scientist shall be trained on the Instrument specific SOPs prior to handling the instruments. The list of SOPs to be covered by the analyst is selected by the Manager – Quality control/AVL-Group leader and Analytical Operations / designee depending on the scope of his / her job responsibility where Training application software is not available.
The analyst/scientist shall be issued Common TDS / product specific TDS for performing testing and recording the test results. If the product specific TDS contains 12 tests and only one test has been taken for qualification, then Head-QC or designee/Head AVL or designee shall issue the TDS by striking off the other tests which are not applicable along with initials and date.
A unique number to each common TDS shall be assigned during TDS preparation.
The analyst/scientist shall independently perform the analysis and record the test details, calculations and results in TDS. The TDS shall be reviewed by reviewer along with the relevant supportive data e.g. weight prints, chromatograms, spectra etc.
The results reported by the analyst /scientist under qualification shall be compared with the results of initial analysis of the coded sample given to analyst as per acceptance criteria included in below Table.
The analyst /scientist evaluation report shall be prepared by compiling the data of qualification and shall be evaluated against the acceptance criteria “Analyst evaluation Report”. The qualification of the analyst shall be considered satisfactory if the results meet acceptance criteria.
In case if the result reported by the analyst does not meet the acceptance criteria; the section In-charge QC/AVL-Group leader shall investigate and evaluate the performance of testing, as per SOP of Laboratory Incidents or respective site SOP. The analyst shall be explained the deficiency/mistakes and shall be retrained.
The analyst shall once again undergo qualification (testing) procedure.
New Joinee:
Head-QC/Head AVL shall assign a qualified analyst to train the new Joined, to train him/her on the analysis technique.
The new Joinee shall read and understand relevant QC department /AVL Standard operating procedures and may interact with other departments such as Warehouse, Production, Quality Assurance and Development quality assurance.
Head-QC/Head AVL shall design a qualification programmed considering the area of work assigned to the analyst/scientist. The qualification programmed shall include the techniques / tests on which the analyst shall be qualified prior to start of routine sample analysis.
The new Joinee who has past experience of quality control testing /AVL shall be assessed by Head-QC/Head AVL and a suitable qualification program shall be designed by taking into consideration his / her prior analytical knowledge and experience. The training and qualification may also be initiated in parallel.
The qualification shall be initiated after satisfactory assessment / evaluation of the new Joinee by Head-QC / designee. Head AVL or designee as per “Assessment Report”
Sample Selection and Coding:
Samples of commercial batches within expiry period shall not be selected for analyst /scientist qualification. Other samples such as exhibit batch sample, control sample of expired batch (commercial/ exhibit), R&D sample etc. which shall comply with the respective specification shall be selected.
The analyst/scientist qualification samples shall not be more than three months old from the date of analysis for the test of related substance and residual solvent. For other tests the samples shall not be more than six months old from the date of analysis.
In case if the available samples are analyzed more than 3 months / 6 months old (e.g. samples of exhibit batch manufactured for regulatory filing) the samples shall be independently analyzed by a qualified analyst and analyst under qualification. The results shall be compared as per the acceptance criteria included in below Table .During analyst/scientist qualification if observed results are not meeting the acceptance criteria of analyst qualification the such events shall be handle through SOP “Laboratory Incidents” or respective site SOP.
The Section In-charge shall ensure that the preferably samples selected for related substance test, residual solvent test shall not have all specified impurities/ solvents below detection limit.
The coded samples shall be allotted to the analyst under qualification along with the test data sheet (TDS) and relevant standard test procedure (STP), without disclosing, any batch specific details or initial results. The allotment details shall be recorded in sample allocation record as per “Sample allocation record”.
The codification of sample shall be done as described below and “Sample for Analyst Qualification” label shall be affixed on the coded sample after including the details on the “Label for analyst qualification sample”.
Analyst Qualification Table:
The analyst shall be qualified as per the below table
Tests & Acceptance Criteria:
The Analyst shall be evaluated for the test as mention in the first Table but not limited to, and the acceptance criteria for all tests described in below second Table
| Balances | LCMS |
| Water content – Karl Fischer | Particle size analysis by Malvern |
| Melting Range | Near IR |
| Loss on Drying | PXRD |
| TOC | NMR |
| Identification by IR | GC-MS |
| Identification by UV | ICP-MS |
| Assay by manual titration | Dissolution |
| Assay by Auto Titrator | Headspace GC & Direct injection (Liquid injection) |
| Optical Rotation/Specific optical Rotation by Polari meter | Related substances by HPLC |
| Assay by HPLC | |
| Test | Analysis | Acceptance Criteria |
| Dissolution | 1 set of 6 Unit | Mean values difference should not be more than 7.5% absolute at any given time point.
All the obtained results should be within the specification limits |
| Identification
. By IR . By UV . By XRD |
Single scan for each test | IR scan of the coded sample shall be concordant with the IR scan of standard or shall meet the specification Maxima and minima of coded sample shall be comparable with standard/spectra (as applicable) or shall meet the specification.
The XRD scan of the coded sample shall be concordant with the XRD scan of standard or, shall meet the specification. |
| Water content by
KF /LOD |
Triplicate | All obtained results shall meet specification limit.
<1.0 test results should meet the specification limit, 1.0 to 3.0 RSD NMT 15%,3.1 to 7.5 RSD NMT 10.0 %,> 7.5 RSD NMT 5%. |
| Particle size | Triplicate | All obtained results shall meet specification
d(0.1) RSD NMT 15% d(0.5) RSD NMT 10% d(0.9) RSD NMT 15% If the particle size value is less than 10 microns, then the above limits shall be doubled for RSD. All obtained results |
| SOR | Triplicate | All obtained results shall meet specification |
| Assay Drug Substance
By HPLC |
Triplicate | Difference between the obtained results and initial results should not be more than 2.0%.
All the obtained results should be within the specification limits |
| Assay Drug product By
HPLC |
Triplicate | Difference between the obtained results and initial results should not be more than 3.0%
All the obtained results should be within the specification limits. |
| Related Substances | Triplicate | Initial Value % obtained Results of coded sample
Below 0.1 % Should meets the specification Between 0.11 % to 0.34% Difference should NMT 0.1 Between 0.35% to 0.54% Difference should NMT 0.15 Between 0.55% to 0.84% Difference should NMT 0.20 Between 0.85% to 3.0% Difference should NMT 0.30 More than 3.0% Difference should NMT 10 % All the obtained results should be within the specification limits. |
| Residual Solvent | Triplicate | The difference between the initial results and obtained results should not be more than 15%
All the obtained results should be within the specification limits Comparison shall not be applicable if the initial results is less than 20% of the specification limit for the respective solvent. |
| Melting Point | Triplicate | All the obtained results should be within the specification limits. |
| TOC | Determined on Purified Water | Should be within the specification limit. |
| Assay by manual titration | Triplicate | Difference between the obtained results and initial results should not be more than 3.0%.
All the obtained results should be within the specification limits |
Also read – ANALYTICAL INSTRUMENT QUALIFICATION
Note: For those test which are not the part of above table, Analyst qualification shall be performed by analyzing the test sample in triplicate analysis, the obtained results should meets the specification limits.
Procedure for Balance methodology/technique:
Select three, 25 ml dry volumetric flask
Weight of empty volumetric flask shall be measured of individually
Volumetric flask shall be filled up to the mark with water maintained and weight shall be measured
Weight of water shall be calculated by subtracting weight of empty flask from weight of filled flask and volume of water shall be calculated using below defined formula
0.997 Density of water at 25 Degree of temperature
Volume = Weight of water / 0.997
Acceptance criteria limit as defined
| Designed Volume | 25 |
| Limit of error (ml) | 0.03 |
| Limit of error (%) | 0.12 |
Record the values on respective TDS
Note: All three value must be complying with in the acceptance criteria limit.
Certification:
An entry of analyst qualification shall be made in the certificate on successful completion’ of qualification / re-qualification, and shall be approved by Head-QC / designee. Head AVL or designee as per “Qualification certificate format”. The different test and technique shall be included under one certificate and respectively signed by the analyst and Head-QC/Head AVL.
A list of qualified analyst along with technique / test shall be maintained. This Annexure shall be updated after certification of analyst.
Requalification:
All analysts shall be re-qualified once in three years & not exceeding due date by more than a month for all the testing techniques which he/she will be using for batch release. The requalification activity shall be performed along with routine analysis.
The requalification evaluation report shall be prepared by compiling the data and shall be evaluated against the acceptance criteria.as mention in above Table.
In case of inter site transfer of analyst from one manufacturing site to another manufacturing site; the certified copy of analyst qualification documents shall be archived for records. The qualification programmed shall be designed considering the techniques on which the analyst was already qualified.
Site QC/AVL shall maintain the track record of the analyst qualification as mentioned.
Person resuming to duties after gaps of three month/more shall be requalified on all of the relevant techniques.
Re-qualification/ qualification date shall be consider from the initiation date of analysis.
If analyst qualification document is loss, re qualification shall be performed.
