Oos Out of Specification

STANDARD OPERATING PROCEDURE
DEPARTMENT:
QUALITY ASSURANCE DEPARTMENT
TITLE :
HANDLING OUT OF SPECIFICATION
1.0
PURPOSE
To describe procedure for Handling Out Of Specification (OOS).
2.0
SCOPE
This SOP shall be applicable to all OOS test results of Raw and Packaging Materials, In
Process Materials, Finished Products and Stability Samples at PEGASUS, Bhongir.
3.0
RESPONSIBILITIES
3.1
Originating Department shall be responsible for:

3.1.1
Verify the OOS results for accuracy and error.
3.1.2
Report questionable results to QC department.
3.1.3
Initiating the OOS investigation and documentation and reporting to QC

department.
3.1.4
Carrying out re-testing as per OOS investigation flowchart, wherever

applicable after approval of retest by QC department.
3.1.5
Archiving the OOS investigation reports.
Issue Date:-05.07.2014

DEPARTMENT:
Effective Date
01.08.2014
Review Date
31.07.2016
TITLE :
3.2
SOP No.
PB/SOP/QAD/032/00
Supersedes
NEW
Page No.
2 of 12
Head - Originating Department Shall be responsible for:

3.2.1
Providing training to the personnel of originating department.
3.2.2
Initiating the actions recommended in investigation report.
3.2.3
Monitor and confirm compliance to actions recommended in the

investigation report.
3.2.4
3.3
Head - Quality Assurance shall be responsible for:

3.3.1
4.0
Final disposal of material, if any.
Review and approval of final OOS investigation report.
LIST OF ATTACHMENTS
Annexure - 1: Format for OOS Logbook
F/PB/QAD/032/24
Annexure - 2: Department code for OOS
NA
Annexure - 3: Format for record and observation of OOS Results (Phase - I)

F/PB/QAD/032/25
Annexure - 4: Format for Checklist for Investigation of OOS
F/PB/QAD/032/26
Annexure - 5: Flowchart for OOS Investigation (Phase - I)
NA
Annexure - 6: Flowchart for OOS Investigation (Phase - II)
NA
Annexure - 7: Format for Investigation Report for Phase II

Prepared By:
Date:
SWATHI. KOTLA
(Officer QA)
Reviewed By:
Date:
M. RAJAREDDY
(Incharge QC)
F/PB/QAD/032/27
Approved By:
Date:
A. K. BHATTACHARYA
(Manager QA)

DEPARTMENT:
Effective Date
01.08.2014
Review Date
31.07.2016
TITLE :
5.0
SOP No.
PB/SOP/QAD/032/00
Supersedes
NEW
Page No.
3 of 12
PROCEDURE
5.1
Frequency:
Immediately on being aware of OOS results or within 1 or maximum 2 days after
completing analytical test (After being checked, audited and reviewed by immediate
supervisor).
5.2
Introduction:
OOS results obtained in the laboratory fall into three general categories:
5.2.1
Laboratory error
5.2.2
Non-process-related or operator error
5.2.3
Process-related or manufacturing error.
When an individual test result does not meet the specifications, it need not
necessarily indicate that the batch has failed. The cause of the OOS result should be
investigated adequately and thoroughly and in time. The results of such an
investigation should be documented. Corrective and preventive actions must be taken
and should be reviewed during batch release.
Phase - I means the Laboratory OOS investigation and Phase - II means the Full
scale OOS investigation.
Prepared By:
Date:
SWATHI. KOTLA
(Officer QA)
Reviewed By:
Date:
M. RAJAREDDY
(Incharge QC)
Approved By:
Date:
A. K. BHATTACHARYA
(Manager QA)

DEPARTMENT:
Effective Date
01.08.2014
Review Date
31.07.2016
TITLE :
5.3
SOP No.
PB/SOP/QAD/032/00
Supersedes
NEW
Page No.
4 of 12
Action to be taken by Analyst:

5.3.1
When any OOS test result is obtained, log the OOS entry in the OOS log
book as per Annexure - 1.
The numbering system for OOS shall be as follow:
PB / OOS / XXX / YY / NNN
PB
indicates Area code allotted by QAD to Pegasus, Bhongir.
OOS
indicates Out Of Specification.
XXX
indicates initiating Department

{as per SOP on SOP :- PB/SOP/QAD/001/01}.
YY
indicates two digits year code.
NNN
indicates three digits numerical OOS allocated in an incremental

manner starting from 001 from each calendar year.
i.e. PB/OOS/XXX/QCD/13/001
indicates that this is the first OOS raised by the QC department of the
Pegasus, Bhongir.
5.3.2
When instruments have been used, check whether they have been calibrated
and were suitable at the time of use.
5.3.3
Investigate for the miscalculations, weighing error, transcription errors,

incomplete transfer of material, and incorrect settings of instruments
parameters.
5.3.4
Retain all test preparations and check the raw data for any clear mistakes
such as incorrect preparation, dilution, injection or storage, inappropriate
environmental conditions. Also check

Prepared By:
Reviewed By:
Date:
Date:
SWATHI. KOTLA
M. RAJAREDDY
(Officer QA)
(Incharge QC)
if the containers of sample are

Approved By:
Date:
A. K. BHATTACHARYA
(Manager QA)

DEPARTMENT:
Effective Date
01.08.2014
Review Date
31.07.2016
TITLE :
SOP No.
PB/SOP/QAD/032/00
Supersedes
NEW
Page No.
5 of 12
incorrectly closed, improperly sampled and improperly stored and use of

expired working/reference standard microbial culture, air bubble in
spectrophotometer cell or HPLC system or specified conditions not
maintained in dissolution medium.
5.3.5
Check whether any deviations had been noted during the time of Analysis
and whether they were recorded in the worksheets.
5.3.6
Record the observations in the Annexure - 3 and hand over to the

immediate supervisor with all the original data. Do not repeat the testing.
5.3.7
Protocol / Worksheet should be attached to OOS investigation form and new

Protocol / Worksheet is issued by QC department.
5.4
Phase - I (Laboratory OOS Investigation)

Investigation by Quality control or immediate supervisor:
5.4.1
Carry out the assessment of the OOS result as soon as the result is
reported.
5.4.2
Discuss the test method with the analyst to confirm that the analyst had
performed the test procedure correctly.
5.4.3
Examine the test data sheet and accompanying attachments in order to find
out whether the results can be attributed to laboratory error.
5.4.4
Arrange for the re-examination of actual test preparations used by the

analyst and to the extent possible, the glassware used in the original testing.
Prepared By:
Date:
SWATHI. KOTLA
(Officer QA)
Reviewed By:
Date:
M. RAJAREDDY
(Incharge QC)
Approved By:
Date:
A. K. BHATTACHARYA
(Manager QA)

DEPARTMENT:
Effective Date
01.08.2014
Review Date
31.07.2016
TITLE :
5.4.5
SOP No.
PB/SOP/QAD/032/00
Supersedes
NEW
Page No.
6 of 12
Confirm the performance of the instruments and ascertain whether the

instrument was within the period of validity of calibration at the time of use.
5.4.6
Determine that appropriate reference standards, solvents, reagents and other

solutions were used and that they meet quality control requirements.
5.4.7
Evaluate the performance of the testing method to ensure that it is

performing according to the authorized documents (Specification / STP).
5.4.8
Record all the observations of the investigation using checklist for

investigation of OOS as per Annexure - 4. The checklist has to be filled by
other immediate supervisor.
5.4.9
Suspected error must be investigated by QC personnel and if the error found

is genuine then the OOS result must be immediately invalidated and
disregarded after appropriate recording and filing.
5.4.10
Analyst and QC personnel both shall review for completeness of entire

procedure using the available checklist.
5.5
Action to be taken by immediate supervisor / In-Charge QC Situations I:

(Conclusive error retest):
5.5.1
If clear error has occurred, arrange for the retesting of the second aliquot of
the same sample solution or aliquot prepared from the same portion of the
original sample by the same analyst in triplicate.
5.5.2
If all the three results of retesting are within the specification, average it,
and substitute the average result for the initial test result (ensure that the
Prepared By:
Reviewed By:
Approved By:
Date:
Date:
Date:
SWATHI. KOTLA
M. RAJAREDDY
A. K. BHATTACHARYA
(Officer QA)
(Incharge QC)
(Manager QA)

DEPARTMENT:
Effective Date
01.08.2014
Review Date
31.07.2016
TITLE :
SOP No.
PB/SOP/QAD/032/00
Supersedes
NEW
Page No.
7 of 12
averaged results are within the proven and acceptable range) and record it
along with an explanation for the initial analysis failure (Genuine lab error reversible error). Invalidate and disregard the previous results on knowing
the probable cause of error, (Record and file the observations with
signature) Retain all the data together.
Statistical acceptance criteria:
The percentage RSD of 3 replicate determinations should not exceed the established
precision for the test.
If immediate supervisor analyst investigation is inconclusive then Situation II:
(Inconclusive error retest):
5.5.3
If the result of retesting is outside the specification and there is no clear
error, arrange for the prompt retesting in replicates by a 2 nd analyst (with
higher experience of testing) using the additional portion of the original
sample. Involve Quality Assurance/Production to look at quality trend of
other batches for the same test to have an idea whether the results of the
earlier batches are within the proven and established range.
5.5.4
If the results of retesting (3 replicates) by the 2nd analyst are individually

within the specification, substitute average of these results for the initial test
results of the 1st analyst (ensure that the average results are within the
proven and acceptable range) and consider them for any decision on batch
release, after investigating the cause of the failure of initial results, (Genuine
lab error - Reversible error). Invalidate and disregard the previous results on
Prepared By:
Date:
SWATHI. KOTLA
(Officer QA)
Reviewed By:
Date:
M. RAJAREDDY
(Incharge QC)
Approved By:
Date:
A. K. BHATTACHARYA
(Manager QA)

DEPARTMENT:
Effective Date
01.08.2014
Review Date
31.07.2016
TITLE :
SOP No.
PB/SOP/QAD/032/00
Supersedes
NEW
Page No.
8 of 12
ascertaining the cause of error (sample integrity being biased); document the
investigation with the signature.
5.5.5
If the result of retesting (3 replicates) by the 2 nd analyst are outside the

specification, report all the results in the worksheet. It may still be possible
that the sample is biased and has laid to the failing results. Retain all the
data together.

The percentage RSD of 3 replicate determinations should not exceed the established
Situation III: (Investigation of sampling procedure and sample integrity
homogeneity and representative portion):
5.5.6
When the initial test and retest on the same sample produces the
OOS
results, determine whether it is possible that the original Sample was nonrepresentative of the whole lot and requires re-sampling.
5.5.7
Before re-sampling activity, it should be conclusively proved that the

original sample was non-representative and also the sampling procedure
should be thoroughly reviewed. Re-sampling is not permitted for uniformity
of content and dissolution testing failure.
5.5.8
Re-sampling is performed under the authority of Head-QA if the

investigation reveals that the integrity of sample is affected; in such
situation a portion of fresh sample from warehouse / manufacturing
Prepared By:
Date:
SWATHI. KOTLA
(Officer QA)
Reviewed By:
Date:
M. RAJAREDDY
(Incharge QC)
Approved By:
Date:
A. K. BHATTACHARYA
(Manager QA)

DEPARTMENT:
Effective Date
01.08.2014
Review Date
31.07.2016
TITLE :
SOP No.
PB/SOP/QAD/032/00
Supersedes
NEW
Page No.
9 of 12
department is subjected to reanalysis by an experienced analyst in

triplicates. If the results (3 replicates) are in conformance to the
specification individually, the batch may be released (ensure that the
average results are within the proven and acceptable range). Investigation
into sampling error is to be documented. Retain all the data on retesting and
re-sampling together.
Situation III is not applicable to content uniformity and dissolution test.
5.5.9
If in a situation where re-sampling does not meet specification it is not

reversible classification. Retesting for OOS stops here which has to go for
full scale investigation into manufacturing or processing through Quality
Assurance.

The percentage RSD of 3 replicates determination should not exceed the established
5.5.10 Corrective measures / actions to be taken by QA/QC:
5.5.10.1 Training to the 1st analyst to perform the test, if a laboratory error has
occurred and the same should be documented.
5.5.10.2 If the testing procedure/sampling procedure needs updation, it
should be done promptly with due analytical method validation and
all concerned should be informed.
5.5.11
If the OOS is not sorted at laboratory stage i.e. Phase - I, then Full scale
OOS investigation of production process review is required i.e. Phase - II.
Prepared By:
Date:
SWATHI. KOTLA
(Officer QA)
Reviewed By:
Date:
M. RAJAREDDY
(Incharge QC)
Approved By:
Date:
A. K. BHATTACHARYA
(Manager QA)

DEPARTMENT:
Effective Date
01.08.2014
Review Date
31.07.2016
TITLE :
5.6
SOP No.
PB/SOP/QAD/032/00
Supersedes
NEW
Page No.
10 of 12
Phase II: Full Scale OOS Investigation:

5.6.1
When the initial assessment does not determine that laboratory error caused
the OOS result and testing results appear to be accurate, a full-scale OOS
investigation is required. This investigation may consist of a production
process review and/or additional laboratory work. The objective of such an
investigation should be to identify the root cause of the OOS result and take
appropriate corrective and preventative action. A full-scale investigation
should include a review of production. Such investigations should be given
the highest priority.
5.6.2
Full scale OOS investigation should be carried out when a product does not
meet the approved specification or any unusual observations are made
during the process of storage, handling, manufacturing or testing of the
product and /or initiated by any of the following conditions.
5.6.2.1 OOS investigation (not due to analytical error)
5.6.2.2 Market complaint.
5.6.2.3 Product recall.
5.6.3
Whenever a failure is identified in product or process or system the same

should be immediately brought to the notice of Head QA.
5.6.4
The Quality Assurance department under instruction of Head QA shall

initiate failure investigation.
5.6.5
Investigation should be extended to all the batches/products, which could

have possibly been affected by the failure.
Prepared By:
Date:
SWATHI. KOTLA
(Officer QA)
Reviewed By:
Date:
M. RAJAREDDY
(Incharge QC)
Approved By:
Date:
A. K. BHATTACHARYA
(Manager QA)

DEPARTMENT:
Effective Date
01.08.2014
Review Date
31.07.2016
TITLE :
5.6.6
SOP No.
PB/SOP/QAD/032/00
Supersedes
NEW
Page No.
11 of 12
Head QA shall hold the release of the batch during investigation of the
subjected batch. Such batch should be quarantine and should not be released
for dispatch, till investigation is complete and a decision is made.
5.6.7
If required, Head QA shall decide the cause of action to be taken after

consultation with Head-CQA to recall those which might have been affected
by the subjected failure.
5.6.8
An investigation report shall be prepared as per given format in Annexure

7
5.6.9
The Flow chart for OOS investigation (Phase - I) given in Annexure - 5

and Flow chart for OOS investigation (Phase - II) given in Annexure - 6
shall be followed in case of an investigation of out of specification / failure.
5.7
Corrective Actions
5.7.1
Based on the outcome of the investigation one or many of the following

appropriate activity should be initiated by QA / Production.
5.7.1.1 Change in the process
5.7.1.2 Instrument servicing
5.7.2
Whenever assignable cause is identified and is attributed to improper

interpretation of method, the concerned analyst should be provided
appropriate training in order to avoid such OOS in the future.
Prepared By:
Date:
SWATHI. KOTLA
(Officer QA)
Reviewed By:
Date:
M. RAJAREDDY
(Incharge QC)
Approved By:
Date:
A. K. BHATTACHARYA
(Manager QA)

DEPARTMENT:
Effective Date
01.08.2014
Review Date
31.07.2016
TITLE :
6.0
Rev. No.
SOP No.
PB/SOP/QAD/032/00
Supersedes
NEW
Page No.
12 of 12
REVISION HISTORY:
Effective Date
Prepared By:
Date:
SWATHI. KOTLA
(Officer QA)
Details of revision and Reason of revision
Reviewed By:
Date:
M. RAJAREDDY
(Incharge QC)
Approved By:
Date:
A. K. BHATTACHARYA
(Manager QA)

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STANDARD OPERATING PROCEDURE

Originating Department shall be responsible for:

Verify the OOS results for accuracy and error.

Report questionable results to QC department.

Initiating the OOS investigation and documentation and reporting to QC

Carrying out re-testing as per OOS investigation flowchart, wherever

Archiving the OOS investigation reports.

STANDARD OPERATING PROCEDURE

Head - Originating Department Shall be responsible for:

Providing training to the personnel of originating department.

Initiating the actions recommended in investigation report.

Monitor and confirm compliance to actions recommended in the

Head - Quality Assurance shall be responsible for:

Final disposal of material, if any.

Review and approval of final OOS investigation report.

Annexure - 3: Format for record and observation of OOS Results (Phase - I)

Annexure - 6: Flowchart for OOS Investigation (Phase - II)

Annexure - 7: Format for Investigation Report for Phase II

STANDARD OPERATING PROCEDURE

Non-process-related or operator error

Process-related or manufacturing error.

STANDARD OPERATING PROCEDURE

Action to be taken by Analyst:

indicates Area code allotted by QAD to Pegasus, Bhongir.

indicates Out Of Specification.

indicates initiating Department

indicates two digits year code.

indicates three digits numerical OOS allocated in an incremental

Investigate for the miscalculations, weighing error, transcription errors,

environmental conditions. Also check

if the containers of sample are

STANDARD OPERATING PROCEDURE

incorrectly closed, improperly sampled and improperly stored and use of

Record the observations in the Annexure - 3 and hand over to the

Protocol / Worksheet should be attached to OOS investigation form and new

Phase - I (Laboratory OOS Investigation)

Arrange for the re-examination of actual test preparations used by the

STANDARD OPERATING PROCEDURE

Confirm the performance of the instruments and ascertain whether the

Determine that appropriate reference standards, solvents, reagents and other

Evaluate the performance of the testing method to ensure that it is

Record all the observations of the investigation using checklist for

Suspected error must be investigated by QC personnel and if the error found

Analyst and QC personnel both shall review for completeness of entire

Action to be taken by immediate supervisor / In-Charge QC Situations I:

STANDARD OPERATING PROCEDURE

If the results of retesting (3 replicates) by the 2nd analyst are individually

STANDARD OPERATING PROCEDURE

If the result of retesting (3 replicates) by the 2 nd analyst are outside the

Statistical acceptance criteria:

Before re-sampling activity, it should be conclusively proved that the

Re-sampling is performed under the authority of Head-QA if the

STANDARD OPERATING PROCEDURE

department is subjected to reanalysis by an experienced analyst in

If in a situation where re-sampling does not meet specification it is not

Statistical acceptance criteria:

STANDARD OPERATING PROCEDURE

Phase II: Full Scale OOS Investigation:

Whenever a failure is identified in product or process or system the same

The Quality Assurance department under instruction of Head QA shall

Investigation should be extended to all the batches/products, which could

STANDARD OPERATING PROCEDURE

If required, Head QA shall decide the cause of action to be taken after