Systacare STABILITY STUDY PROTOCOL Protocol No.

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Format No: SYS/SOP/QA/049-F01/00

STABILITY STUDY PROTOCOL

FOR

------------------------

Label Claim : Each Vial Contains:

-------------------
Primary Packing Configuration -----------------------------------------------------

Secondary Packing Configuration --

Actual Market Pack…………………………………………
Charged Secondary Pack in the Chamber…………………..
……………………………………………………………….
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PROTOCOL CONTENTS

S. No. TITLE PAGE No.

1.0 PROTOCOL APPROVAL 3
2.0 OBJECTIVE 4
3.0 SCOPE 4
4.0 RESPONSIBILITY 5
5.0 REASON FOR STABILITY STUDIES 6
6.0 TRAINING DETAILS 6
7.0 SPECIFICATION AND TEST METHODOLOGY INFORMATION 7
8.0 TYPES OF STUDIES 7
9.0 TEST RESULTS ACCEPTANCE CRITERIA 8
10.0 REFERENCE TO ANALYTICAL VALIDATION [STABILITY INDICATING] 8
11.0 STUDY DESIGN AND CONDITION 9-10
12.0 STABILITY TESTING MATRIX 11
13.0 STABILITY STUDY REPORT 12
14.0 OUT OF SPECIFICATIONS 12
15.0 DEVIATIONS 12
16.0 CHANGE CONTROL 12
17.0 EQUIPMENT AND STORAGE MALFUNCTION 12
18.0 COMMITMENT 12
19.0 CONCLUSION 13
20.0 REFERENCE DOCUMENTS 13
21.0 ABBREVIATIONS 14
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1.0 PROTOCOL APPROVAL:

INITIATED BY:

DESIGNATION NAME SIGNATURE DATE

OFFICER/EXECUTIVE
(QUALITY CONTROL )

REVIEWED BY:

DESIGNATION NAME SIGNATURE DATE

HEAD
(PRODUCTION)
HEAD
(QUALITY CONTROL)
EXECUTIVE/SR.
EXECUTIVE
(QUALITY ASSURANCE)

APPROVED BY:

DESIGNATION NAME SIGNATURE DATE

HEAD
(QUALITY ASSURANCE)
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Format No: SYS/SOP/QA/049-F01/00

2.0 OBJECTIVE:

2.1 To Design Stability Study Plan for ------------------------------- manufactured at SYSTACARE

REMEDIES, AMRITSAR (PUNJAB)., as per ICH [Q1A (R2)] Guideline and SOP No.

SYS/SOP/QAD/049 to assess Physico-Chemical and Microbiological activities attributes when exposed

to various storage conditions in its Market pack/Secondary Packing Material Equivalent to Market Pack

and to verify its Shelf-Life and Storage Condition.

2.2 The objective of Stability Study Testing is to provide evidence on how the quality of a drug

product varies with time under the influence of a variety of environmental factors such as Temperature,

Relative Humidity to assess the Shelf Life for the Drug Product and recommended Storage Conditions.

3.0 SCOPE:

3.1 This Stability Study Protocol is applicable to conduct the Stability Study of

-------------------------, manufactured at M/s SYSTACARE REMEDIES, AMRITSAR (PUNJAB) and

tested in it's own Quality Control Lab.

3.2 Stability Studies shall be carried out on Annual Stability Batch of the Year, Process validation

batches & if there is change in Active / Excipients Grade & Active Vendor, manufactured as per the

Manufacturing formula ………………………….and tested in Quality Control Department at

SYSTACARE REMEDIES, AMRITSAR (PUNJAB), as per STP No………………………

3.3 Stability Studies shall be carried out with.

o Pack Type:…………………………

 ____ Such Carton Shrink Wrapped.

3.4 Batches involved in Stability Study:

Sr. No. Batch No. Batch Size Mfg. Date Exp. Date
1.
2.
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3.

4.0 RESPONSIBILITY:

DEPARTMENTS RESPONSIBILITIES

 To Prepare the Protocol and Report.

 To Prepare the Stability Study Summary Report.

Quality Control  To review of Protocol and Report.

 Test the samples as per the Sampling and Testing Plan

 To Compile the Stability Data

 To review of the Protocol.

Production
 To arrange for Stability Samples as per Protocol.

 To review and Approve the Protocol

 Protocol Training

 To monitor all Stability Study Activities and ensuring the Stability Studies

are as per the Protocol.

Quality Assurance  To arrange the Stability Samples in Stability Chambers.

 To withdraw the Stability Study Samples and Handover to Quality Control

Department for online testing.

 To Review the compiled Stability Data

 To maintain the Records of Stability Studies

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Format No: SYS/SOP/QA/049-F01/00

5.0 REASON FOR STABILITY STUDIES:

5.1 The purpose of Stability Study Testing is to provide evidence on how the quality of a drug

product varies with time under the influence of a variety of environmental factors such as Temperature,

Relative Humidity and to establish the Shelf Life for the Drug Product and recommended Storage

Conditions.

Put a tick √ in Appropriate box.

5.2 Annual Stability Batch of the Year

5.3 Process Validation Batches

5.4 Change in the Manufacturing Formulae/Manufacturing Procedure

5.5 Change in Active Material Grade, Site Change and vendor change

5.6 Party Requirement

6.0 TRAINING DETAILS:

All personnel involved in the Stability Studies, Sampling and Testing of samples should be
appropriately trained both in their job related activities and on the Stability Study Protocol by Head-QA
or his/her Designee. The details of training shall be recorded in the training attendance Annexure-I.
SUPERVISORY STAFF
S. Department Name of Designation Training on Signature Checked by
No. Trainee protocol is given of (Sign/Date)
(Yes/No) Trainee (QA)
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Name of the Trainer: _______________

7.0 SPECIFICATION AND TEST METHODOLOGY INFORMATION:

Details of the Specification and Test Methodology and MFR/BMR/BPR which will be used for the

analysis ------------------------------------

Reference Specification / STP No.:

Specification No.: ---------------------------

*Current Version of Specification / STP shall be used for Analysis.

Reference MFR No.: -----------------------

Reference BMR No.: -----------------------

Reference BPR No.: -----------------------

8.0 TYPES OF STUDIES:

TYPES OF
STORAGE CONDITION TESTING FREQUENCY IN MONTH
STUDIES

Accelerated 40oC ±2°C /

Initial, 01, 02, 03 & 06.
Condition 75%RH ± 5%

Long Term Storage 30ºC ± 2 ºC /

Initial, 03, 06, 09, 12, 18, 24, 30 & 36.
Condition 75 % RH ± 5%

Note: Finished Product Analysis results shall be considered as Initial Stability Study Results. In case the
batch is not charged into the stability chamber within 30 days from the date of initial analysis
result the testing of the test parameters and acceptance criteria test would be repeated for
considering it as time initial analysis.
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9.0 TEST RESULTS ACCEPTANCE CRITERIA:

The Test Parameters and Acceptance Criteria during Stability Studies for Testing of -----------------------as
below:
S. No. TEST ACCEPTANCE CRITERIA
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.

10.0 REFERENCE TO ANALYTICAL VALIDATION [STABILITY INDICATING]:

Validation of the test methodology used for the analysis of Stability Samples of ------------------------ will
be as per Protocol of Analytical Method Validation No. ---------------------------
/ Protocol of Analytical Method Verification No. --------------------------------
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11.0 STUDY DESIGN AND CONDITION:

11.1 Stability Study Sampling Schedule and Sample Distribution for drug product:

The Stability Study Sampling Schedule and Sample Distribution is as per the details provided in the table
below:
Storage Conditions
Sampling Accelerated Long Term
Intervals 40 C ±2°C / 75 %RH ± 5% RH
o
30 C ±2°C / 75 %RH ± 5% RH
o

01 - -
Months
02 - -
Months
03 - -
Months
06 - -
Months
09 - -
Months
12 - -
Months
18 - -
Months
24 - -
Months
30 - -
Months
36 - -
Months
Extra ----------- --------------
Samples
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Storage Conditions
Sampling Accelerated Long Term
Intervals 40 C ±2°C / 75 %RH ± 5% RH
o
30 C ±2°C / 75 %RH ± 5% RH
o

Total -------------- No’s -------------- No’s

Note: Extra Samples kept in Stability Chamber for one time analysis of Chemical and Micro Analysis.

11.2 Total quantity of samples charged per batch and per pack for Stability Study and Chambers
Identification:
STABILITY SAMPLE QTY.
STUDY STORAGE CONDITIONS
CHAMBER ID NO.
Accelerated 40oC ±2°C / 75%RH ± 5% RH SYS/STBC/02 ------ No's
Long Term 30 C ±2°C / 75 %RH ± 5% RH
o
SYS/STBC/03 ------ No's
Total ------ No's

The samples shall be loaded or charged into the stability chambers and labeled as per SOP No.
SYS/SOP/QAD/049 Titled “Stability Study”.
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12.0 STABILITY TESTING MATRIX:

Stability Time Points Testing parameter ------------------------ BET,

Study ----------------------- (Visual Inspection) Sterility
Conditions
(0) Initial √ √ √
03 months √ √ X
Long Term
06 months √ √ X
(30 C ±2°C /
o

75 %RH ± 09 months √ √ X
5% RH)
12 months √ √ √

18 months √ √ X

24 months √ √ √

30 months √ √ √

36 months √ √ √

48 months

60 months

01 months √ √ X
Accelerated
02 months √ √ X
(40oC ±2°C
75% RH ± 03 months √ √ X
5% RH)
06 months √ √ √
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(√) Analysis Required (X) Analysis not required

13.0 STABILITY STUDY REPORT:

A Stability Study Report shall be prepared as per the Stability Study Sampling and Analysis Plan
mentioned in the Stability Study Protocol by Quality Control Department.

14.0 OUT OF SPECIFICATIONS:

The stability sample with Out-of-specifications (OOS) & Out Of Trend results shall be investigated
adequately as per SOP No. SYS/SOP/QC/039 of “Handling of Out of Specification Results”&
SYS/SOP/QAD/041 of Out Of Trend” Decision on the continuation of stability studies (after getting
OOS & OOT results) shall be taken by Head QC and Head QA with proper supporting rationale. Stability
Studies, if required, can be aborted after getting the test results of next consecutive testing interval,
provided the sample is again failing in the same parameter. At this stage there shall be no need to
investigate the OOS & OOT results.

15.0 DEVIATIONS:

Any deviation, if observed, shall be handled as per SOP No. SYS/SOP/QAD/009 & SOP/QAD/010 of
“Handling of Deviations” and same shall be a part of Stability Study Report.

16.0 CHANGE CONTROL:

Any Change if required, shall be handled as per SOP No. SYS/SOP/QAD/008 of “Change Control” and
same shall be a part of Stability Study Report.
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17.0 EQUIPMENT AND STORAGE MALFUNCTION:

To be handled As per SOP No. SYS/SOP/QAD/049“Stability Study”.

18.0 COMMITMENT:

All studies shall be carried out and report shall be complied as per plan outlined in this Stability Study
Protocol.

19.0 CONCLUSION:

The Stability report shall be reviewed for the following significant changes.

a) A Reduction in the Assay Value by more than 5% with respect to Initial Value of Product

b) Failure to Meet the Acceptance Criterion for pH.

c) Failure to Meet Specifications for Appearance & Physical Properties e.g. Colour, Phase Separation,

Sedimentation/Precipitation, Turbidity etc.

d) Failure to meet the acceptance criteria for any other test.

e) Conclusion shall be drawn based on the results of the test parameter at each interval. The conclusion
shall define the packing material, storage conditions and shelf life of the product.

20.0 REFERENCE DOCUMENTS:

 ICH Guideline (Q1AR2, Step 4), Stability Testing of New Drug Substances and Products.

 SOP No. SYS/SOP/QAD/049 of “Stability Study”.

 SOP No. SYS/SOP/QC/039 of “Handling of Out-of-Specification Results”.

 SOP No. SYS/SOP/QAD/009 & SOP/QA/010 of “Handling of Deviations”.

 SOP No. SYS/SOP/QAD/008 of “Change Control”.

 SOP No. SYS/SOP/QAD/041 of “Out of Trained”.

 Finished Product Standard Test Specification & Procedure .

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21.0 ABBREVIATIONS:

SOP : Standard Operating Procedure

ICH : International Conference on Harmonization

QA : Quality Assurance

QC : Quality Control

OOS : Out of Specification

RH : Relative Humidity

STP : Standard Test Procedure

ID No. : Identification Number

w/v : Weight / Volume

IP : Indian Pharmacopoeia

NA : Not Applicable