This procedure is applicable for the New employee (experienced
or fresher), existing analyst who is changed from one section to another
section e.g. Raw material to Finished product or enlargement of
responsibility, to ensure the capability of the analyst to perform analysis
accurately and to demonstrate the analyst’s ability to perform specific methods
as a result of investigation in QC laboratory.
RESPONSIBILITIES:
Analyst: To perform the analysis
for the qualification as per approved procedures and go through all the
necessary trainings.
Quality Control Section In charge:
Responsible for the certification of Analyst and verification of results
and comparison with acceptance criteria.
Quality Control Head:
Responsible for the compliance to this SOP and to ensure the competence of
analyst who operate specific equipment, perform tests and calibrations.
DEFINITION :
Certification of
analyst: This procedure applies to all analyst
in Quality control laboratory in order to ensure that analyst performing the
tests are adequately trained to produce reliable and accurate results within
the specified acceptable limits.
PROCEDURE :
Analyst
certification shall involve determining the competency on following :
Understanding
of the MOA of the test and analysis performed by the analyst.
Knowledge
about the instruments used by analyst and ability to use them.
Performing
analysis according to approved MOA’s and STP’s.
Evaluation of
the analytical results and reporting.
Before analyst
certification, Section In charge / Nominee shall ensure that all necessary
training has been imparted to analyst.
Certification
of analyst is not applicable for the operation of physical parameter measuring
devices. Training is essential to operate the below equipment’s and measuring
devices but not limited to: Disintegration apparatus, Hardness tester, Tap
density tester, Sieve analysis, Refractometer, Melting point apparatus,
Analytical balance, Viscometer, Laboratory Oven, Fiability apparatus,
Muffle furnace, Scale etc.
Certification
of analyst is mandatory for the operation of instrument like HPLC and GC.
Others
instrument operation will be dealt according to the below matrix.
|
S.No
|
Section
|
Test
|
Instrument on which
qualification performed
|
Operation and calibration
|
|
|
Can perform
|
Can’t perform
|
||||
|
1
|
Finished product /Stability study
|
Assay or Dissolution or Related substances Chromatographic
purity
|
HPLC
|
HPLC, UV Visible spectrophotometer, FTIR, Polarimeter
and Auto- titrator.
|
GC
|
|
UV-Visible spectrophot-ometer
|
UV Visible spectrophotometer , FTIR , Polarimeter and
Auto- titrator.
|
HPLC and GC
|
|||
|
Identification
|
FTIR
|
FTIR,UV-Visible spectrophotometer, Polarimeter and
Autotirator.
|
HPLC and GC
|
||
|
Assay
|
Titrimetry (Manual)
|
Chemical analysis.
|
HPLC ,GC UV Visible spectrophoto-meter , FTIR, Polarimeter
|
||
|
Assay / water content
|
AutoTitrator
|
UV Visible Spectrophotometer, FTIR and Polarimeter.
|
HPLC and GC
|
||
|
Specific optical rotation
|
Polarimeter
|
UV Visible Spectrophotometer and FTIR.
|
HPLC and GC
|
||
|
2
|
Raw material
|
Assay or Related substances or Chromatographic purity
|
HPLC
|
UV Visible spectrophotometer, FTIR, Polarimeter and
Autotitrator.
|
GC
|
|
|
Assay
|
Titrimetry (Manual)
|
Chemical analysis.
|
HPLC ,GC UV Visible spectophotometer , FTIR and
Polarimeter
|
|
|
|
Assay / Water content
|
Auto Titrator
|
UV Visible, FTIR and Polarimeter.
|
HPLC and GC
|
|
|
Assay or Related substances or Residual solvents
|
GC
|
UV Visible spectrophotometer, FTIR and Polarimeter.
|
HPLC
|
||
|
Specific optical rotation
|
Polarimeter
|
UV Visible and FTIR.
|
HPLC and GC
|
||
|
3
|
Packing Material
|
Grammage of aluminium foil
|
–
|
Bursting strength tester
|
HPLC, GC
|
|
Identification
|
FTIR
|
FTIR
|
HPLC, GC, UV, Polarimeter, Autotitrator
|
||
- Recently fresh approved raw material or finished product or packing material shall be given to the analyst to perform testing .The samples are to be coded accordingly.
- These samples packed in a manner which can prevent exposure to moisture, light and heat.
- While performing the analysis the analyst must trained to follow the general laboratory practices and general safety requirements.
- The coded sample are to be analysed in triplicate except dissolution and the analysis shall be completed within 10 working days from the receipt date.
- Evaluate the capability of the analyst in terms of its precision to perform the tests and Laboratory practices followed by the analyst.
- The Quality control Section In charge shall verify the results and compare with acceptance criteria
- The analyst shall be considered qualified if the results obtained by him / her within the specification limit and within acceptable limit (as mentioned below) for certification of analyst.
- ACCEPTANCE CRITERIA:
- Assay of Finished product and Raw material : Mean difference should not be more than ± 3 % and RSD of three values should not be more than 1.0 %.
- Dissolution: Mean difference should not differ by 5 % from original value and % RSD should not be more than 10.0 %.
- Water content by KF apparatus: RSD of three values should not be more than 1.0 %.
- Loss on drying : RSD of three values should not be more than 1.0 %.
- Residual solvents: Mean difference should not be more than 7.5% and RSD of three values should not be more than 10.0 %.
- Specific optical rotation : Mean difference should not be ± 3 % and RSD of three values should not be more than 10.0 %.
- FTIR : Results should be comparable with the IR spectrum obtained with reference Standard.
- Melting point : Results should meet the specification.
- Grammage of aluminium foil : Results should meet the specification.
- Related substances in Finished product and Raw material: Any individual impurity:
- ± 25 % from the original reported value (if the value is between 0.1 – 0.2 %).
- ± 15 % from the original reported value (if the value is above 0.2 %).
- (Values below 0.1 % shall not be considered)
- Total Impurities; ± 25 % from the original reported value.
- If the results found out of acceptance criteria, Section In Charge or his nominee shall conduct investigation through deviation for the cause and if it is due to analytical error, then the analyst shall be retrained for the respective SOP’s /Procedure and shall be again qualified.
- The analyst is to be considered as certified, if the analytical results reported by the analyst during the evaluation study meet the established acceptance criteria.
- ABBREVIATIONS:
- SOP : Standard Operating Procedure
- QC : Quality Control
- FTIR : Fourier Transform infrared
- MOA : Method of analysis
- GLP : Good Laboratory Practices
- HPLC : High Performance Liquid
Chromatograohy
- UV : Ultra Voilet Visible
- GC : Gas Chromatography
- RSD : Relative Standard deviation
- STP : Standard testing procedure
