To lay down the procedure for out-of-specification. OOS investigations shall be divided into Laboratory Investigations (Initial and Secondary) and Manufacturing investigations.
3.0 RESPONSIBILITIES
3.1 Chemists of the QA department to follow the SOP.
3.2 Head – QA complies with SOP.
4.0 Out-of-Specification Procedure
4.1.1 GENERAL
4.1.1 OOS investigations shall be divided into
Laboratory Investigations (Initial and Secondary) and Manufacturing
investigations.
4.1.2 If any packing material is out of specification
in the description test/print/text, Quality Assurance shall decide whether the investigations are required or not required.
4.1.3 The minor deviations in dimensions of packing
materials, which were found suitable on the machine suitability test on the packing
line, shall be approved for use.
4.1.4 OOS shall be registered in “Investigation Form”
format.
{tocify} $title={Table of Contents}
4.2 Laboratory Investigations
4.2.1 This investigation should include an initial
assessment of the accuracy of the laboratory’s data The analyst and the
supervisor conduct a laboratory investigation to determine whether or not the
out-of-specification is assignable to the testing laboratory.
4.2.2 On notification of an OOS result, the head
Laboratory and Analyst shall jointly conduct an initial investigation
4.2.3 The first phase of such an investigation shall
include an initial lab investigation of the accuracy of the laboratory data
before test solutions are discarded, whenever possible.
4.2.4 Re-testing shall be done from the original sample
unless otherwise the original sample is consumed or spilled. Re-sampling shall
be done if an original sample is consumed or spilled.
4.2.5 Assignable cause
found during the investigation, the same analyst shall do the re-testing in
duplicate from the original sample.
4.2.2 If samples pass the tests, in such cases the
original OOS result may be invalidated the cause of OOS shall be documented and
the subjected batch shall be released.
4.2.3 If a sample fails the tests, in such cases the
original OOS results shall be valid and documented and the subjected batch
shall be rejected.
4.2.4 If the assignable cause is not found, in such cases
secondary lab investigation along with manufacturing investigations shall be
done to find out laboratory error or manufacturing error, respectively.
4.2.5 Investigation for laboratory error shall be done
as per the “Laboratory Investigations report” format.
4.2.6 If the assignable cause is found a laboratory
error like sample preparation, glassware, instrument malfunction, or any
other during an investigation, the different analysts shall do the re-testing
in duplicate.
4.2.7 If samples pass the tests in such cases the
original OOS result may be invalidated the cause of OOS shall be documented and
the subjected sample shall be released.
4.2.8 If the sample fails the tests in such cases the
original OOS results shall be valid and documented and the subjected sample
shall be rejected.
4.2.9 If no assignable cause is found as laboratory
error or manufacturing error, in such case different analysts shall do the
re-testing three times.
4.2.10 if samples pass the tests, in such cases the
original OOS result may be invalidated the cause of OOS shall be documented
and the subjected sample shall be released.
4.2.11 If a sample fails the tests in such cases the
original OOS results shall be valid and documented and the subjected sample
shall be rejected.
4.2.12 All steps leading to laboratory investigations
shall be documented and a review of each failure shall be correlated to the
occurrence of a similar failure in the past.
4.2.13 A corrective and preventive action plan shall be
prepared depending upon the nature of the failure which caused OOS.
4.3 Manufacturing Investigation
4.3.2 Out-of-specification results will be informed to
the manufacturer.
4.3.3 If the manufacturer is not satisfied with the
results he can perform a joint analysis. Reporting will be done as per the
“Joint Analysis Report” format.
4.4 Numbering System
4.4.2 The first three characters shall be OOS which
denotes ‘Out of Specification” which is followed by ‘/’ (oblique) and the
current year written as (XXXX) e.g. 2013.
4.4.3 The year shall be followed by ‘/’ (oblique) and
the sequential number of OOS.
4.4.4 A typical example for the numbering of the
first OOS for the year 2013 shall be OOS/2013/01.
4.2 REPORTING AND DOCUMENTATION
4.2.2 Copies of the final OOS Investigation Form shall be
distributed to the appropriate department.
4.2.3 Investigation and resolution of all OOS test
results is a priority matter, hence initial laboratory investigations shall be
completed within 03 working days.
4.2.4 In case of confirmed OOS results complete
investigation i.e. Secondary Laboratory and manufacturing investigation (to
identify the cause of failure) shall be completed within 20 calendar days.
4.2.5 A record of OOS shall be maintained as per the
“Format for Record of Out of Specification” format.
5.0 ABBREVIATIONS
5.1 SOP:
Standard Operating Procedure
5.2
OOS: Out Of
Specification
5.3
QA: Quality
Assurance
5.4
QC: Quality Control
5.5 No. : Number
6.0 REFERENCE:
6.1 Nil
RELATED
FORMATS
4.2 REPORTING
AND DOCUMENTATION
4.2.2 Copies of the final OOS Investigation Form shall be
distributed to the appropriate department.
4.2.3 Investigation and resolution of all OOS test
results is a priority matter, hence initial laboratory investigations shall be
completed within 03 working days.
4.2.4 In case of confirmed OOS results complete
investigation i.e. Secondary Laboratory and manufacturing investigation (to
identify the cause of failure) shall be completed within 20 calendar days.
4.2.5 A record of OOS shall be maintained as per the
“Format for Record of Out of Specification” format.
7.0 Flow Chart for Investigation of Out-of-Specification Results
OOS INVESTIGATION FORM
|
OOS
No. |
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|
Date
Reported |
|
|
Description
of OOS |
|
|
Specification |
|
|
Test
Result |
|
|
Sample |
Pass
/ Fail / Investigation required / Not required |
|
Preliminary
Investigation Done on (date) / by |
|
|
Assignable
cause during Phase I |
Yes
No |
|
Phase
II Investigation is done on (date) / by |
|
|
Final
conclusion |
Pass
/ Fail |
|
Corrective
Action |
|
|
Preventive
Action |
|
|
Final
Review and Closing:
Manager-Quality Assurance |
|
LABORATORY INVESTIGATION REPORT
(This
format should be used for documentation of investigation)
OOS No.
Name
of Sample
Lot I Batch No.
A.R. No.
Mfg. Date
Exp. Date
Specification
No. & Review No. :
Test
in which O.O.S. result is found:
Result :
Specification
Limit (of the concerned test):
Analyst:
Date
of Analysis:
Date
of start for Investigation:
1.0 Initial Lab Investigations
|
DESCRIPTION |
OBSERVATION |
|
Samples
appearance |
|
|
Weighing
Errors (sample weight & measurement) |
|
|
Calculation
Errors (also the completeness of raw data) |
|
|
Protocol
review |
|
|
Another
observation if any |
|
2.0 Assignable cause / Non-Assignable cause
|
If cause is non-assignable |
Proceed for secondary Lab
investigations |
|
If the cause is assignable
Specify the cause (s) & Re-test in duplicate |
|
|
Re-test in Duplicate |
Results |
|
Re-test -I |
|
|
Re-test-II |
|
3.0 Secondary Lab Investigation:
|
DESCRIPTION |
OBSERVATION |
|
Errors
associated with dilutions, dilutions, Filters, conditions, etc. that are
Required by the corresponding analytical Procedure |
|
|
Review
of critical steps followed during analysis |
|
|
Whether
reference I working standards used in the Analysis are
correct (in terms of appearance, Expiry date potency, LOD / Water, and its
storage) And whether assay values are determined correctly. |
|
|
Whether
properly prepared test solution (s) or volumetric solution(s) |
|
|
Any
malfunctioning of the instrument |
|
|
Out-of-calibration analytical instruments were used in the analysis. |
|
|
Lab
glassware used. |
|
|
Review
specifications whether it is updated or not. |
|
|
Any
loss of standard solution or test solution during preparation. |
|
|
Any
other techniques in analytical procedures were not appropriately applied
during testing. |
|
|
Whether
the analysis is performed by any other alternate validated Procedure. |
|
|
Whether the analyst is trained to perform the test. |
|
|
Whether
the environmental condition is suitable to perform the test. |
|
|
Other
observations if any. |
Attach
extra sheet |
FORMAT FOR RECORD OF OUT OF SPECIFICATION
|
S.
No. |
OOS
Number |
Material
Name (Sample
) |
Final
Status (Approved
/ Rejected) |
OOS
Closed |
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Active ingredients | Total Active ingredients for sulfated oils
Sop and Calibration of Automatic Karl Fischer
SOP and Calibration of Refractor meter | Refractive Index
Out of Specifications (OOS) results
Handling of Out of Specifications (OOS) results for samples in XYZ Limited. It is the policy of XYZ Limited that written procedures shall be followed to carry out laboratory investigations/product re-test assign probable cause and initiate appropriate corrective and preventive action for out-of-specification results of samples.
This procedure is applicable whenever any out-of-specification result is observed.
Flow Chart for Investigation of Out-of-Specification Results
