OUT OF SPECIFICATION (OOS)
1.0 OBJECTIVE:
To
lay down a procedure for handling out of specification results obtained during
analysis.
2.0 SCOPE:
This
SOP is applicable to the results, which is out of specification obtained in
Quality Control Laboratory for Raw/ Packaging materials, finished products for
releasing parameters. This SOP is not applicable for informative parameters.
3.0 RESPONSIBILITY:
3.1 Quality Control
Analyst:
3.1.1
To inform out of
specification results to the quality control in-charge.
3.2 Quality Control
in-charge:
3.2.1
To issue out of
specification investigation form after entering in the form in out of
specification log book.
3.2.2
To investigate out
of specification results.
4.0 ACCOUNTABILITY:
4.1 Head of the Q.C Department:
4.1.1
To verify the
investigation form at each and every stage and to give final conclusion about
the status of the material.
5.0 PROCEDURE:
5.1
On receipt of
report for the out of specification (OOS) of results from the analyst, Q.C
in-charge shall issue OOS form after duly entering in the out of specification
log book.
5.2
Q.C in-charge or
designee shall carry out the investigation and fill in the form (Stage A).
5.3
If it is found
that the parameter of stage A is not satisfactory, any error is reported,
correct the parameter and same sample shall be reanalyzed by another analyst.
5.4
If the material
meets the requirement, release the material; the analyst shall be re-trained
for the error parts.
5.5
If the parameter
of stage A is found satisfactory, the superior shall allot the same material
for re-analysis to another senior analyst (Stage B).
5.6
If (Stage B)
result is within specification, the material shall be reanalyzed by first
analyst with same sample material and to investigate the first analysts.
5.7
If investigation
of first analysts found satisfactory then release the material.
5.8
If the material
fails in Stage B also, by senior analyst, simultaneously analyse after
re-sample with the previously approved material (Stage C).
5.9
Material under investigation
(Stage C) should be re-sampled with the authorization of Head Quality and then
proceeds for the further analysis (Stage C).
5.10
If material has
been received first time, no previous sample is available, than stage C is not
applicable and rejects the material.
5.11
If the previously
approved material passes within the specification and the material under
investigation fails to meet the specification, the material shall be rejected.
5.12
If the previously
approved material passes within the specification and the material under
investigation also with the specification than the material shall be reanalyze
by another analyst and investigate the second analysis (Stage B).
5.13
If investigation
of second analysis (Stage B) found satisfactory than release the material.
5.14
The repeat
analysis can be carried out in separate sheet allotted by the supervisor duly
authorized or in the particular hard book and all printouts shall be attached
with the document.
5.15
Cross-references
of analysis shall be attached with OOS investigation form.
5.16
Final conclusion
shall be made in the OOS investigation form for rejection/ approval by Quality
Head.
5.17
Cross-reference of
OOS investigation form shall be given in the analytical report.
6.0 REVISION LOG:
|
Revision No. |
Effective Date |
Reason |
|
00 |
|
New
SOP |
7.0 REFERENCES:
7.1
Not Applicable.
8.0 ANNEXURES:
Annexure 1: GENERAL
DETAILS.
Annexure 2:
Annexure:
1
GENERAL
DETAILS
|
Form
No.: |
Issued
by: |
|
Issued
to: |
Date: |
|
Product/
Item: Batch
No./ Lot No.: Stage: Out
of specification test: Analyzed
by:_______________ Date:
______________ Reference: _______________ |
|
Details
of Investigation
STAGE
A
|
Sr.# |
Item |
Observation |
Sign |
|
1. |
Condition of sample to
be checked. |
|
|
|
2. |
Balance checked for its
calibration. |
|
|
|
3. |
Instrument calibration
check. |
|
|
|
4. |
Volumetric standard/
reagent used for analysis checked for its validity. |
|
|
|
5. |
Analytical template/
Hard book checked for dilution, calculation, weighing titer values and
readings. |
|
|
|
6. |
Working standard
checked for its validity. |
|
|
|
7. |
Chromatograms/ printouts/
TLC plates checked. |
|
|
|
8. |
Glassware checked for
its accuracy and calibration. |
|
|
|
Remarks
of the investigator: Not satisfactory/ Satisfactory. Sign:
_______________ Date:
_______________ |
|||
STAGE B
|
Repeat
analysis allotted to: Date: |
|
Observation
of the result: Analyzed
by: ________________ Date: _____________ Reference: _______________ |
|
Remarks
of the investigator: Sign:
_____________ Date:
_____________ |
Note: If
the material fails in the above stage i.e. Stage B, the material will resample
with the authorization shall be analyzed by senior analyst along with the
previously approved material.
MATERIAL/
PRODUCT RESAMPLE AUTHORIZATION FORM
|
A.R.
No.: |
Qty.:
|
Authorization
by/ Date: |
Sampled
by/ Date: |
STAGE
C
|
Name
of the senior chemist: Date
of analysis: |
|
Approved
batch taken for comparison: |
|
Observation
of the result: Approved
batch: Current
batch: Analyzed
by: _____________ Date: _______________ Reference: ________________ |
|
FINAL
CONCLUSION: |
|
Head
Quality: __________________ Date:
__________________________ |
Attachments:-
Stage A: ______________
Stage B: ______________
Stage C: ______________
Investigation report.
Annexure:
2
|
OOS Applicable |
OOS Not Applicable |
||
|
Sr. No. |
Tests of Releasing Parameters |
Sr. No. |
Tests of Informative Parameters |
|
1. |
Identification. |
1. |
Description. |
|
2. |
Assay. |
2. |
Particle size
distribution (sieve tests). |
|
3. |
Related substances/
Chromatographic purity/ Degradation profiles. |
3. |
Bulk density. |
|
4. |
Solubility |
4. |
Physical parameters
(i.e. Hardness, friability, dimensions). |
|
5. |
Dissolution (USP
guidelines to be followed). |
|
|
|
6. |
Content uniformity (USP
guidelines to be followed). |
|
|
|
7. |
Chemical purity tests
(i.e. Melting points/ colour index, chlorides/ sulphates, SOR, etc.) |
|
|
|
8. |
Test matters, grammage,
and colour scheme. |
|
|
9.0 ABBREVIATIONS:
|
Abbreviation |
Expanded Form |
|
S |
Standard operating
procedure |
|
& |
And |
|
% |
percentage |
|
Sr. No. |
Serial number |
|
OOS |
Out of specification |
|
A.R. No. |
Analytical report
number |
|
Qty. |
Quantity |
|
USP |
United States
Pharmacopoeia |