Annexure – I

OOS investigation

Product Name : Pseudoephedrine HCl

Batch Number : 500116-500216

OOS Number : OOS/014/16

Test Parameter : Residual solvents analysis by GC

Description of the OOS:

 During the residual solvents analysis of pseudoephedrine HCl the Methanol result is obtained
149 ppm which does not complies specification limit of Not more than 100 ppm.
Detailed Investigation:

 The analysis was performed in GC ID. NO-GC004 ,Verified it's calibration status found
satisfactory.
 Interacted with the analyst about his knowledge in instrument and test method found
satisfactory.
 Reviewed the raw data (Preparation of sample standard) and system suitability chromatogram
there is no discrepancy observed.

 Verified the system suitability parameters as per test method ,the resolution and %RSD of six
replicates injection were met the acceptance criteria.
 In the same sequence other one batches has been analyzed i-e 500216 .In that
500116 batch only out of specification observed in Methanol .The results were tabulated below

Solvents Batch number/result in ppm Spec. limit

500116 500216
Methanol 149 6 Not more than 100 ppm
Acetone 246 282 Not more than 500 ppm
Toluene 2 0.1 Not more than 150 ppm

 To find out the rootcause for OOS for the batch number 500116 ,the OOS investigation started
as per laboratory investigation check list.
 Investigating testing not performed due to non availability of original solution. There is no
obvious laboratory error found after completion of preliminary laboratory investigation.
  Hence it is decided to do retest with another chemist after get approval from QA.

 Retest with another analyst started with fresh preparation of sample along with previous
sequence analysed and passed sample of batch number 500216.

 After completion of sequence the chromatogram taken and raw data completed and verified
there is no discrepancy observed and the obtained results were tabulated as below

Solvents Batch number/result in ppm Spec. limit

Initial- Retest Initial- Retest
500116 500116 500216 500216
Methanol 149 10 6 7 Not more than 100 ppm
Acetone 246 178 282 185 Not more than 500 ppm
Toluene 2 ND 0.1 ND Not more than 150 ppm

 Retest-2 performed

Root cause

 Based on the above detailed investigation the root cause of the OOS it may be due to
Contamination of glassware's or solution during the preparation.

Corrective action

 The initial analysis result invalidated.

 Reanalysis of original sample results were taken for release the batch

Preventive action

 The training has to be given as per glassware cleaning standard operation procedure for all
analyst and casual labors who are all involving cleaning of glasswares.

Prepared by Reviewed by

Date : Date :