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Janki Singh

Analyst Qualification of Quality Control Personnel

Standard Operation Procedure (SOP) of providing training and qualification of analyst for all new appointed personnel, and existing employees who are responsible for sampling & testing of incoming materials, in process samples and finished products.

Analyst Qualification Procedure

1.0   Objective :

    • To lay down a procedure of providing training and qualification of analyst for all new appointed personnel, and existing employees who are responsible for sampling & testing of incoming materials, in process samples and finished products in Quality Control Laboratory.

2.0   Scope :

    • This procedure applicable to all new appointed personnel, existing employees and who are intra transfer from another section for enhancing the skill or fulfill the requirement of any other section in Quality Control department.

3.0  Procedure for Analyst Qualification :

    • Training of New Appointed Personnel:

    • Induction training by HR, general training by QA shall be given to new employee as per the procedure described in SOP for Training Management.
    • After completion of induction and general training employee shall be handover to Quality Control.
    • Quality Control Department Head/Designee shall prepare job description of the employee as per SOP.
    • Enclose the controlled copy of JD in Personal Training File after approval.
    • Based on Job description, Training Need Identification of employee shall be prepared as per SOP and Training shall be conducted after QA approval.
    • After completion of trainings new appointed employee shall be recommended for analyst qualification based on Job description.

    • Training for existing employee:

    • Qualified trainer shall give scheduled training as per annual training schedule.
    • Qualified trainer shall give On Job Training, Refresher trainings, cGMP Trainings, Class Room Trainings as per the procedure described in SOP.

    • Analyst Qualification of New Appointed Personnel:

    • Quality Control shall inform Quality Assurance to collect the sample quantity of finished product required for analyst qualification during packaging stage of batch.
    • Similarly inform sampling person to collect sample quantity of raw material required for analyst qualification during sampling activity.
    • One batch of API or one batch of single drug formulation or multidrug formulation of any product shall be selected. If required, additional batch may be given.
    • Pre-tested sample (Sample of known analytical values & not more than 30days old pre-tested stable product) shall be identified.
    • If pre-approved sample is not available in such case certified standard shall be used for analyst qualification.
    • Use certified values for comparison.
    • The samples will be coded to protect its identity.
    • This code shall be mentioned on the analyst qualification forms.
    • The actual batch numbers are known only to Section Head QC and maintain the record in Annexure-XII.

    • The code number will be as follows:

AQ/YY/XXX

Where, 

AQ = Analyst Qualification

YY = Year (“20” for 2020, “21” for 2021 and so on)

XXX = Sequential number i.e. 001, 002 etc.

Example: AQ/20/001, AQ/20/002

    • Sample shall be allotted to analyst along with current specification/STP.
    • Work authorization shall be issued after the completion of qualification and shall be synchronized with job description as per SOP.

    • Qualification of Microbiologist :

    • Work authorization shall be issued after the completion of qualification and shall be synchronized with job description.

    • Evaluation:

    • RSD of all 3 set values and reference value (previous approved batch results) shall be calculated.
    • The acceptance criteria of RSD and for other requirements shall be as mentioned below:
    • The analyst qualification criteria shall be as mentioned in below Table-1.
    • All individual values shall meet the requirements as per specification.
    • Absolute difference of the mean of all 3 set values and reference value shall be calculated (in moisture content/LOD only) and acceptance criteria of RSD of the same shall be as per Table-1

Table-1

Sr. No Test Acceptance Criteria
1 Assay
  • (By HPLC, UV-VIS & Titrimetry)
  • ( Vit- B12 By Microbiological Method)
  • RSD of all 3 set values and reference value should be NMT 2%
  • RSD of all 3 set values and reference value should be NMT 3%
2 Dissolution

(Test shall be performed on 12 Units)

 Dissolution results shall be within specification limit.
3

Related Substances :

  • Total Related Substances
  • If the value obtained for any individual impurity is less than 0.1%w/w
  • Note: Acceptance criteria shall not be applicable to related substances that are less than or about limit of Quantitation.
  • RSD of all 3 set values and reference value should be NMT 15%
  • Shall not be comparable
4 Moisture(Water) content
  • If water content is ≤ 0.1%w/w
  • 0.11% to 1.55% w/w
  • 1.56% to 3.95% w/w
  • 3.96% and above
  • Difference of the individual values from the mean shall be NMT ±0.03
  • All 3 set values RSD and reference value should be NMT 15%
  • RSD of all 3 set values and reference value should be NMT 10%
  • RSD of all 3 set values and reference value should be NMT 5%
5 FTIR
  • Prepare three samples
  • Should be comparable with the reference standard/ working standard
6 Melting Point/Range
  • Prepare three samples
  • Results should meet the specification limit.
7

Weighing & Pipetting

  • Prepare three samples
  • RSD of all 3 set values should be NMT 0.5%
8 Viscometer
  • Prepare three samples
  • RSD of all 3 set values and reference value should be NMT 2%
9 Gas chromatography
  • If the analyte level  is > 100 ppm
  • The analyte level  is > 50 ppm and <100 ppm
  • If the analyte level  is < 50 ppm
  • Note: The acceptance criteria shall not be applicable if the analyte level is less than or about limit of quantitation.
  • RSD should be NMT 15 %
  • NMT 25 %
  • NMT 40 %
10 Microbial Limit Test Variation NMT 30% from the results reported by trainer
    • The Head-QC will review the Analyst Qualification report and qualify the Analyst.
    • If the results are not within the acceptable range, invalidate the data and record in invalid data log.
    • Further training shall be given and the analyst shall be re-qualified.

    • Analyst Re- Qualification of Existing Employee:

    • Qualification of regular analyst shall be carried out in the following conditions:
    • Periodic re-qualification of the analyst shall be done at-least once in a two year (+01 month of scheduled month) based on his current job responsibility.
    • Frequent Analyst error observed during OOS investigation.
    • Major changes in analytical techniques.
    • Changes in Job Description.
    • In case if analyst does not meet the acceptance criteria during re-qualification, Quality Control Head/Designee shall evaluate the performance of testing, analysis and then investigate the same.
    • If the root cause of failure is not related to analyst (for example- instrument error/variability) the same set of solutions shall be re-injected after rectification of instrument.
    • If the root cause of failure is due to analyst error, the analyst shall be quarantined and an impact assessment on his/her historical testing results and released batches back to the last successful qualification has to be performed.
    • After the completion of investigation, the analyst shall be explained his/her deficiency/ mistake and trained accordingly. In this case analyst shall be re-qualified before deploying on job.
    • An yearly schedule for analyst qualification shall be prepared in the beginning of each calendar year as per Annexure-XIII.

4.0   Annexure – Analyst Qualification :

Annexure I : Professional Curriculum Vitae

  • Personal Information

Name:…………………………………………………    Employee code no.:…………………………………………

Date of birth :…………………………………………    Male/ Female: ………………………………………………

Qualification :…………………………………………   Place of birth:   ………………………………………………

Date of joining: ………………………………….         International: ………………………………………………

Date of joining in QC dept.: ……………………           Marital status :…………………………………………

Resident address: …………………………………………………………………………………………………………

Contact address: ………………………………………………………………………Tel. no. :………………………

Previous Experience : ……………………………………………………………………………………………

Signature:                                                                                          Head QC:

  • General Education

Date (From……. To……)

 Degree of certificate School/College/Institute/University Subject

Updated by
  • Professional Training Courses
Date

(From……To…..)

 Title of

Training courses

 Training Organization Type of certificate

(Attendant or successful)

 Certificate no. Updated by
  • Work Experience
Date

(From……To…..)

 Name of team Work experience Job title

Updated by

Annexure II : Analyst Qualification weighing and pipetting technique

Test: Weighting and Pipetting Technique

Topic Pipetting

Results

 Acceptance criteria

Sample 1

 2 3

RSD

 

Weighing and pipetting techniques

(1, 2, 5 and 10 ml in triplicate)

 1 ml RSD: <= 0.5% for values obtained for Set 1 , Set 2 & Set 3
2 ml
5 ml
10 ml

 Evaluation       :   The trainee has understood / not understood this phase of the training and qualifies / does not qualify for weighting and pipetting techniques.

Annexure III : Analyst Qualification for Karl Fischer Apparatus

Product/Material Name:

Instrument: Karl Fischer Apparatus

Sample Code:

Topic Analyst

Results

 Acceptance criteria Analyst Name Sign/Date
Set – 1 2 3 Mean

RSD
Factor determination Trainee RSD ≤ 1.0 % for values obtained for set 1, 2 and 3.

 

Topic Analyst Results Acceptance criteria Analyst Name Sign/Date

Set 1

 2 3 Mean

RSD

Water Determination in previously analyzed sample

 Trainee Over all% RSD/Difference of individuals value from the mean

 
Previous result Results:

 Evaluation: The trainee has understood / not understood this phase of the training and qualifies / does not qualify for the sample analysis by Karl-Fischer Apparatus.

Annexure IV : Analyst Qualification for HPLC

Product/Material Name:

Instrument: HPLC (Assay)

Sample Code : 

Topic Analyst

Results

 Acceptance Criteria Analyst Name Sign/Date

Set 1

 2 3 Mean

RSD
Sample analysis

by HPLC

 Trainee RSD of all 3 set values and reference value should be NMT 2%
Previous

Result

 Result:

(% RSD)

Evaluation       :   The trainee has understood / not understood this phase of the training and qualifies / does not qualify for the sample analysis of Assay by HPLC

Annexure V : Analyst Qualification Titrimetric Analysis

Product/Material Name:

Test: Titrimetric Analysis

Sample Code:

Topic Analyst Results Acceptance criteria Analyst Name Sign/Date

Set 1

 2 3 Mean

RSD
Sample analysis

by titration

 Trainee RSD of all 3 set values and previous value should be NMT 2%
Previous

result

 Results:

(% RSD )

 

Evaluation   :   The trainee has understood / not understood this phase of the training and qualifies / does not qualify for the sample analysis by Titration.

Annexure VI : Analyst Qualification for Dissolution apparatus and UV-Vis Spectrophotometer

Product/Material Name:

Instrument: Dissolution Apparatus and UV-VIS Spectrophotometer

Sample Code:

Topic Analyst Results Acceptance criteria Analyst Name Sign/Date
Sample analysis

On Dissolution & UV-VIS Spectrophotometer

Trainee

 Tablet-1 Tt-2 T-3 Result Should be within specification limit.

Spec Limit:

…………….
Tablet-4 T-5 T-6
Tablet-1 T-2 T-3
Tablet-4

 

 T-5 T-6
Results: (Average of 12 units):

Evaluation       :   The trainee has understood / not understood this phase of the training and qualifies / does not qualify for the sample analysis by Dissolution & UV-VIS Spectrophotometer.

Annexure VII : Analyst Qualification for Viscometer

Product/Material Name:

Instrument: Viscometer

Sample Code :

Topic Analyst

Results

 Acceptance criteria Analyst Name Sign/Date

Set 1

 2 3 Mean

RSD
Sample analysis for Viscosity Measurements on  Brookfield Viscometer

Trainee

 RSD of all 3 set values and previous value should be NMT 2%
Previous Result Results:

(% RSD )

Evaluation : The trainee has understood / not understood this phase of the training and qualifies / does not qualify for the sample analysis by Viscometer.

Annexure VIII : Analyst Qualification for FTIR

Product/Material Name:

Instrument: FTIR

Sample Code:

Topic Analyst

Results

 Acceptance criteria Analyst Name Sign/Date
Set 1 2

3
Sample analysis by using FTIR

Trainee

 Should be comparable with the reference standard/ working standard
Result:

Evaluation :  The trainee has understood / not understood this phase of the training and qualifies / does not qualify for the sample analysis by FTIR.

Annexure IX : Analyst Qualification for Melting Point apparatus

Topic Analyst Results Acceptance criteria Analyst Name Sign/Date
1 2 3 Mean
Analysis of melting point of sample by melting point apparatus. Trainee Results should meet the specification limit.

Spec Limit:

……………

 

 

Evaluation       :   The trainee has understood / not understood this phase of the training and qualifies / does not qualify for the sample analysis by Melting Point Apparatus.

Annexure X : Analyst Qualification for microbiological testing

Topic Analyst Results Limit Name/sign

Set 1

 2 3 Mean RSD
Sample analysis by using zone reader Trainee Variation: ±5% of previous results.

RSD: ≤ 3%

For values obtained for

set 1 , 2 and 3
Previous

result

Variation: 

RSD: 

Evaluation : The trainee has understood / not understood this phase of the training and qualifies / does not qualify for Microbiological Assays.

Annexure XI : Analyst Qualification for Gas Chromatography

Topic Analyst Results Acceptance Criteria Analyst Name Sign/Date

Set 1

 2 3 Mean

RSD
Sample analysis

by

GC

 Trainee RSD of all 3 set values and reference value should be NMT

……….

 
Previous Result Result: (% RSD)

Evaluation  :   The trainee has understood / not understood this phase of the training and qualifies / does not qualify for the sample analysis by GC.

Annexure XII  : Record of product for analyst Qualification

Sr.No.

 Date Analyst Name EMP Code Product /Material Name Batch /

A.R No.

 Test/

Technique

 Sample Code Allotted Allotted By

Remarks

Annexure XIII : Analyst Qualification Schedule

Sr. No. Analyst Name Emp. Code Qualification Done On Re-Qualification Due On Remarks

5.0   Glossary

  • SOP                     :          Standard Operating Procedure
  • QC                       :          Quality Control
  • CGMP                 :          Current Good Manufacturing Practices
  • GLP                     :          Good Laboratory Practices
  • HPLC                  :          High Pressure Liquid Chromatography
  • QA                       :          Quality Assurance
  • NMT                    :         Not More Than
  • Reference Value:         A value reported by previously qualified analyst
  • GC                       :          Gas chromatography

*********************************************END*********************************************

Categories: Microbiology Quality Quality Assurance Quality Control SOP's Validation
Tags: Analyst TrainingAnalyst Validation
Janki Singh: Mrs. Janki Singh is the professional pharmaceuticals Blogger. She has already posted more than #1000 articles on varrious topics at different blogging plateforms. Contact : guideline.sop@gmail.com

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