XXXX PHARMA LIMITED

Standard Operating Procedure

Quality Control Department
Title: Stability studies of active pharmaceutical ingredients
SOP Number: Revision No.
Effective date: Review date: Page 1 of 6

1.0 Objective: To provide Guidance how stability studies conducted under different
environmental conditions such as temperature, light and humidity and to assign
retest/expiry date as per the stability data.

2.0 Scope: This standard operating procedure is applicable all the drug substances
manufactured at Active pharmaceutical ingredients division of Lee Pharma limited.

3.0 Responsibility: Quality Control Chemist.

4.0 Accountability: HOD - Quality Control.

5.0 Procedure: The procedure shall be as follows

5.1 Introduction
5.1.1 To provide guidance on how to conduct stability studies under various
environmental conditions such as temperature and humidity in container
closure system simulated to dispatch containers.

5.2 Selection of batches

5.2.1 Stability studies shall be conducted on at least three primary batches of the
drug substance. The batches shall be manufactured to a minimum of pilot
scale by the same synthetic route or commercially produced batches.
5.2.2 One commercial batch shall be added to the long term stability on every
year [add on batch].
5.2.3 Reprocessing or reworking batches shall be kept for stability studies.
5.2.4 Materials which undergo physical modification such as micronization
should be kept for stability studies.
5.2.5 If the batch uses recovery solvents in the manufacturing process one batch
should be kept for stability study inorder to evaluate their effect on stability
of the drug substance.
5.2.6 Enter the details of batches selected in Stability Programme Register in
format number - 01

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 XXXX PHARMA LIMITED
Standard Operating Procedure
Quality Control Department
Title: Stability studies of active pharmaceutical ingredients
SOP Number: Revision No.
Effective date: Review date: Page 2 of 6

5.3 Container closure system

5.3.1 The stability studies shall be conducted on the drug substance packed in a
container closure system which simulates the market containers.
5.3.2 Label the container with details given in format number-06

5.4 Testing frequency

5.4.1 Testing frequency shall be determined based on condition at which stability
is performed.
5.4.2 Accelerated:
5.4.2.1 Accelerated stability shall be conducted at 0,1,2,3 and 6
months.
5.4.3 Long term:
5.4.3.1Long-term stability studies shall be carried out at the intervals
of every three months on first year and every six months on
second year and every year on third year on words.Eg:
0,3,6,9,12,18,24,36,48 and 60 months.
5.4.4 Intermediate:
5.4.4.1 Intermediate stability studies shall be carried out at 0,3,6,9 and
12 months, or upto 60 months.

5.4.5 The time periods shall be determined prior to carrying out the long-term
stability studies and prepare the stability schedule as per format number- 04
5.4.6 For add on batch use long term stability testing frequency and prepare
schedule as per the format number-04

5.5 Storage conditions:

5.5.1 Identify the storage conditions based on the pharmacopeal data or literature
information or R&D information. For add on batch use long term storage
conditions.
5.5.1.1 For general case
5.5.1.1.1 Accelerated stability:

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 XXXX PHARMA LIMITED
Standard Operating Procedure
Quality Control Department
Title: Stability studies of active pharmaceutical ingredients
SOP Number: Revision No.
Effective date: Review date: Page 3 of 6
5.5.1.1.1.1 Temperature : 40C 2C
5.5.1.1.1.2 Humidity : 75% 5% RH
5.5.1.1.2 Long term Stability
5.5.1.1.2.1 Temperature : 25C 2 C
5.5.1.1.2.2 Humidity : 60 % 5% RH.
5.5.1.2 For drug substances stored in Refrigerator

5.5.1.2.1 Accelerated stability:

5.5.1.2.1.1 Temperature : 25C 2C
5.5.1.2.1.2 Humidity : 60% 5% RH
5.5.1.2.2 Long term Stability
5.5.1.2.2.1 Temperature : 5C 3 C
5.5.1.3 For drug substances stored in freezer
5.5.1.3.1 Long term stability
5.5.1.3.1.1 Temperature : -20C 5C

5.6 Test(s) to be performed

5.6.1 Identify the test(s) to be performed in the stability studies under accelerated
and long term stability based on the drug substance specification.
5.6.2 Stability indicating test procedures which are validated should be used for
analysis of the stability samples.
5.7 Sampling Quantity, sampling and Analysis time window
5.7.1 Identify the quantity of samples to be taken for stability study for both
accelerated and long term and record in the stability register format no-01
5.7.2 Remove the samples from the stability chambers on due date of analysis as
given in the stability schedule. If this is not possible follow this procedure
5.7.2.1 Remove the accelerated samples within 2 days of due date of
analysis

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 XXXX PHARMA LIMITED
Standard Operating Procedure
Quality Control Department
Title: Stability studies of active pharmaceutical ingredients
SOP Number: Revision No.
Effective date: Review date: Page 4 of 6
5.7.2.2 Remove the Long term samples within 4 days of due date of
analysis.
5.7.3 Store the samples below 25C in a dessicator dedicated for stability samples
ir in refrigerator between 2-8C until analysis of the samples are performed.
5.7.4 Perform the sampling as per the standard operting procedure of quality
control.
5.7.5 Analysis of the sample shall be performed on the due date or if not possible,
follow this procedure.
5.7.5.1 Analyze the accelerated samples within 3 days of due date.
5.7.5.2 Analyze the Long term samples which are having below 12
months stability shall be analyzed within 2 weeks of due date.
5.7.5.3 Analyze the Long term samples which are having above 12
months stability shall be analyzed within 4 weeks of due date

5.8 Stability Protocol

5.8.1 Prepare stability protocol after entering the details in Stability Programme-
Register with format number -02.
5.8.2 Protocol numbering shall be given as per following format
5.8.2.1 PSOMFP01
5.8.2.2 PS : stability protocol
5.8.2.3 OM : two letter code for product ( OM for Omeprazole)
5.8.2.4 FP : Finished Product
5.8.2.5 01 : Procedure Number
5.9 Stability summary
5.9.1 Compile the stability report as per format number -03 at the end of the
stability studies.
5.9.2 Numbering for stability report shall be
5.9.2.1 RSOMFP01
5.9.2.2 RS : stability report
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 XXXX PHARMA LIMITED
Standard Operating Procedure
Quality Control Department
Title: Stability studies of active pharmaceutical ingredients
SOP Number: Revision No.
Effective date: Review date: Page 5 of 6
5.9.2.3 OM : two letter code for product ( OM for Omeprazole)
5.9.2.4 FP : Finished Product
5.9.2.5 01 : Procedure Number
5.10 Storage statement(s)
5.10.1 Storage statements shall be concluded based on the evaluation of stability
data.
5.11 Evaluation of stability data:
5.11.1 Evaluate the stability data after analysis. Record the data in the stability data
format number-05.
5.11.2 Compile the data in the format numbe-05 at each time point and sign off
this document.
5.11.3 If there is any out of specification result or falure to meet
specification(significant change) in stability analysis, follow OOS standard
operating procedure.
5.12 Destruction of leftover samples
5.12.1 Destroy the sample leftovers after analysis. Follow the written procedure
from the quality control department.
5.13 In case of Changes in the manufacturing process or site
5.13.1 If minor changes done in the manufacturing process, Sample from batches
produced under each change shall be added to stability program (one
batch).
5.13.2 If major changes done in the manufacturing process, collect the samples
from the new batches (three batches) and perform the stability like new
product. In such a case the protocol and report procedure number shall be
changed.
5.13.3 In case of manufacturing site change, evaluate the affect on stability of the
drug substance by keeping one batch for stability.

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 XXXX PHARMA LIMITED
Standard Operating Procedure
Quality Control Department
Title: Stability studies of active pharmaceutical ingredients
SOP Number: Revision No.
Effective date: Review date: Page 6 of 6

6.0 Documents:

6.1 Stability Programme- Register --- 01

6.2 Stability Protocol --- 02

6.3 Stability Report --- 03

6.4 Stability schedule --- 04

6.5 Stability Data --- 05

6.6 Stabiliy Label --- 06

7.0 History

Superseded Rev. Change Reasons for

Effective Date
SOP. No No. revision
New Not
Not applicable Not applicable Not applicable
Document applicable

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