SOP on Handling of Laboratory Incident

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1.0 Objective:

To lay down the procedure for the handling of any Laboratory Incident in the Quality Control Laboratory.

2.0 Scope:

This SOP is applicable to Quality Control Laboratory of pharmaceutical company.

3.0 Responsibility:

Chemist or above of QC laboratory.

4.0 Accountability:

Head – Quality Control

Head – Quality Assurance

5.0 Abbreviations and Definitions

  • SOP :           Standard Operating Procedure
  • STP :           Standard Testing Procedure
  • QC :            Quality Control
  • QA :            Quality Assurance
  • SP :             Specific
  • HPLC :        High Performance Liquid Chromatography
  • GC :            Gas Chromatography
  • TOC :          Total Organic Carbon
  • R. No. :       Analytical Reference Number
  • No. :            Batch Number

6.0 Procedure:

6.1 The source of incidents / discrepancies includes but is not limited to the following examples:

6.1.1 General Incidents:

6.1.1.1 Borderline results

6.1.1.2 Tested for parameter other than given in specification.

6.1.1.3 Mistake in calculation and or reporting.

6.1.1.4 Any contamination during sample / standard preparation / storage of sample.

6.1.1.5 Usage of Instruments like analytical balance, pH meter, conductivity meter etc. before calibration etc.

6.1.1.6 STP deviation with respect to weighing, dilutions, standards etc.

6.1.1.7 Wrong entry of method parameter, sequence etc in the application software.

6.1.1.8 Improper sample handling during analysis.

6.1.1.9 Glassware breakage with sample or standard.

6.1.1.10 Discontinue analysis for electrical problems, urgent re-planning of work.

6.1.1.11 Sample spills during the test for e.g. Loss on Drying, Sulphated Ash or Water Content.

6.1.1.12 System suitability parameter failure.

6.1.2 Chromatography:

6.1.2.1 Injection Carryover

6.1.2.2 Additional / Unknown Impurities

6.1.2.3 Shift in Retention Time / Relative Retention Time (Not more than 10 %)

6.1.2.4 Improper Peak Shape and Peak Splitting

6.1.2.5 Baseline Drift

6.1.2.6 Bracketing standard Were does not meet acceptance criteria

6.1.3 Spectroscopy:

6.1.3.1 Extra peaks in the spectrum

6.1.3.2 Low Correlation with standard spectrum

6.1.4 Microbiology:

6.1.4.1 Out of trend, borderline to trend

6.1.4.2 TOC baseline noise

6.1.4.3 Wrong media preparation

6.1.5 Entry missing in instrument log book.

6.2 Based upon sound scientific principles, analyst shall discontinue testing and immediately notify supervisor or designee if an incident, problem or error is suspected or recognized.

6.3 All Incidents shall be logged as per respective Annexure.

6.4 The Incident Report Number shall be assigned as follows:

QCI/YY/XXX,

Where,

First, second and third characters ‘QCI’ stand for Quality Control Incident.

Forth characters is ‘/’

Fifth and Sixth characters YY stand for year (‘16’ for year 2016)

Seventh characters is ‘/’

Eighth, Ninth and Tenth characters serial no. starting from 001.

Serial no will start from 001 for every year.

6.5 The analyst / reviewer shall write the brief of incident in the laboratory incident / discrepancy report as per respective Annexure and shall attach all relevant data with report.

6.6 When an incident has been observed during analysis on HPLC or GC, analyst shall fill checklist as per respective Annexure in case of HPLC and as per respective Annexure in case of GC as a part of investigation.

6.7 Manager–QC shall review the report and shall recommend the corrective or preventive action plan based on the investigation done.

6.8 Manager-QA shall approve the incident report.

6.9 Any Laboratory incident observed shall be logged within one working day of discovery of a discrepant laboratory and incident investigations shall be closed within thirty working days from the date incident is reported. The reasons and rationale for any extension will be documented.

6.10 All personnel involved in the investigation process from identifying a discrepant laboratory test result through record retention of such an event shall be properly trained to perform assigned tasks.

7.0 Forms and Records (Annexures)

Laboratory Incident Register                         – Annexure-I

Laboratory Incident / Discrepancy Report     – Annexure-II

Analyst Checklist HPLC                                  – Annexure-III

Analyst Checklist GC                                     – Annexure-IV

8.0 References (if any):

In-house.

9.0 Distribution

  • Master copy –           Quality Assurance
  • Controlled copies- Quality Control, Microbiology Section

 

10.0 History

     Date    Revision Number                       Reason for Revision
                       New SOP

 

Annexure-I

LABORATORY INCIDENT REGISTER

Sr. No. Date Incident Report number Name of Product Batch Number Description of Incident Analyst Checked by Remarks

 

Annexure-II

Laboratory Incident / Discrepancy Report

Name of  Material / Product :   Incident Report No. :  
B. No. / A. R. No. :   Equipment Involved :  
Test :   Name of Analyst :  
Date of Incident Observed :   Date of Analysis :  
STP No. :   Specification No. :  
Brief Description of Incidence / Discrepancy:
 
Analyst:

Signature / Date:

Reviewer:

Signature / Date:                  

Investigation :
 
Analyst:

Signature / Date:

Reviewer:

Signature / Date:                  

Proposed corrective action on Incidence / Discrepancy:
 

 

 

 

Reviewer:

Signature / Date: 

Head QC:

Signature / Date: 

 

Corrective action taken:
 

 

 

Analyst:

Signature / Date:                          

Reviewer:

Signature / Date:                          

Preventive Action (if any) :
 

 

 

 

Head QC:

Signature / Date:

Head QA:

Signature / Date:

 

 Annexure-III

ANALYST CHECKLIST – HPLC

 

PRODUCT :                                                      INSTRUMENT No.:

STP No.:                                                          TEST:

ANALYST :

PROBLEM:

Sr. No. Parameters Observations Option
1. Pressure Fluctuation OK / Not OK
2. Condition of Column

(Date of Issue :                             )

(Back Pressure:                      psi )

OK / Not OK
3. Mobile Phase Preparation OK / Not OK
4. Any Leakage in system Yes / No
5. Integration Parameters OK / Not OK
6. Instrument Method Parameters OK / Not OK
7. Condition of Degasser OK / Not OK
8. Condition of Auto Sampler Vial OK / Not OK
9. Rinsing / Purging Solvents OK / Not OK
10. System Suitability OK / Not OK

 

Analyzed By:                                                  Checked By:

Sign/Date:                                                       Sign/Date:

Annexure-IV

ANALYST CHECKLIST – GC

 

PRODUCT :                                       INSTRUMENT No.:

STP No.:                                           TEST:

ANALYST :

PROBLEM:

Sr. No. ACTIVITY YES NO
1 Leakage Check    
1a Leak check at injector port    
1b Leak check at detector port    
1c Leak check at septa end ( injector top)    
 
2 Column Check    
2a Check column end both end should be flat    
2b Check ferrules for both column ends    
2c Install column    
2d Check both column ends for proper fitting    
 
3 Check Septa    
3a Check septa condition replace it if required    
3b Septa should be proper tighten    
 
4 Injector Port    
4a Check glass liner condition    
4b Clean liner to remove residue particles    
4c Check both end of the liner – it should be flat    
4d Replace the liner if required    
 
5 Detector Port    
5a Check collector assembly clean it if required    
5b Clean jet if required    
5c Check signal – it should not fluctuate    
 
6 Check Gases    
6a Check gases (H2, air, N2 cylinders)    
6b Check leakage on the joints of connection    
6c Replace the cylinder if abnormal signal has been observed    
7 Check Syringe    
7a Check the plunger for smooth functioning    
7b Clean the syringe with water / solvent according to analysis    
7c Check barrel properly if crack is observed replace the syringe    
7d Check Head space needle – clean it if found to be chocked    

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