Sop-Qa-038-00-Stability Studies

SOLITAIRE PHARMACIA PVT. LTD.
RESTRICTED CIRCULATION
STANDARD OPERATING PROCEDURE AUTHORISED PERSONS ONLY
Title: Procedure for Stability Study of Finished Products SOP. No. : SPL/ SOP/QA/038
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Supersedes : New
Revision No. : 00
Prepared By Checked By Reviewed By Approved By Effective Date Review Date
Concerned Dept Concerned Dept QA QA-Head
1. Objective
To define the procedure for Stability Study of Finished Products.
2. Scope
This procedure is applicable to carry out the stability study of finished Products manufactured
at Solitaire Pharmacia Pvt. Ltd., Baddi.
3. Responsibility
Executive - Quality Assurance:
To provide the stability samples from production floor during packing operation.
To enter the stability samples details in “Sample Login Register”.
To charge the stability samples into required stability chambers, to withdraw samples as per
frequency, handling and analysis.
To prepare the “Stability Study Monthly Schedule” and planning for analysis.
To review the compiled stability data at each station.
To raise Out of Specification (OOS) wherever applicable.
To maintain all Stability Study records.
Executive- Quality Control
To prepare Stability Study Work Sheet and Protocol and carry out analysis.
Head – Quality Assurance, Head – Quality Control:
To approve the Stability Study Work Sheet Protocol.
To review and approve the stability study data.
To investigate the Out of Specification (OOS) results.
To authorize any deviation during Stability Study of Drug Product.
Format No.SPL/QA/001
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To investigate and approve Out of Specification report.
4. Accountability
Head QA and Head- QC.
5. Procedure
5.1 Purpose:
5.1.1 The purpose of stability study is to evaluate physical, chemical and microbiological
change(s) with time period under the influence of variety of temperature and humidity
to which drug products may be exposed during its shelf life.
5.1.2 To monitor the drug product throughout its shelf life to determine whether it remains
stable within the specification under the labelled storage condition.
5.1.3 To confirm that the drug product is assured for its efficacy and safety in marketed pack
throughout the cycle of warehousing, distribution, storage and use.
5.1.4 To monitor the stability of drug products for change(s) in manufacturing process or
active raw materials or primary packaging materials.
5.1.5 The results of stability studies shall be used in demonstrating that storage conditions,
retest period and expiration date given to products are justified.
5.2 General:
5.2.1 If product is manufactured under generic name or different brand names but the
formulation, strength, manufacturing process and primary packing remain same; the
samples of any one generic or brand name shall be subjected for stability study.
5.2.2 If manufacturing formula of the drug product is same but primary packaging materials
are different, product packed in each packaging shall be kept for stability studies.
5.2.3 The samples kept at different storage conditions shall be withdrawn from these
conditions at the stipulated time interval and analyzed within - 10 days and + 15 days.
5.2.4 In case of failure of stability chamber, it shall be repaired by in-house or vendor

representative.
5.3 Selection of Batches and Stability Commitment:
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5.3.1 Initially first three batches of drug product shall be subjected ("Initially" means the drug
product is subjected for stability for the first time at the location or new product) for
long term and accelerated stability.
5.3.2 Subsequently minimum one batch per year shall be subjected for long-term stability
study.
5.3.3 Subsequent stability studies are required due to various changes in the existing process
or critical equipment.
5.3.4 Stability study shall be carried out up to the shelf life of the drug product. This may be
extended further if necessary for extending the shelf life of the product for 2 to 3
batches. i.e. continue the stability study up to expiry plus 1 year or period up to which
the drug product is stable, whichever is more. During this 1-year or the period up to
which the drug product is stable, (whichever is more) extended period samples shall be
analyzed at 6 months interval.
5.3.5 Pack selected for stability studies shall be the marketed pack.
5.4 Procedure to provide the samples for stability studies to Stability Section:
5.4.1 Officer - Quality Assurance shall collect the stability samples from manufacturing
department during packing operation. Quantity of samples (1000 Tablets per batch for
both conditions. 700 Tablets for long term condition & 300 tablets for accelerated).
5.4.2 Officer- Quality Assurance shall verify the details of samples and sign the “Stability
Sample Log In Register” (refer Format no. SPL/QA/058)
5.5 Procedure for storage of samples into the Stability Chamber:

5.5.1 Divide the sample quantity as follows;
Qty in units
Study Condition
Cap Tab Liq
Accelerated 40 OC ± 2 OC, 75% ± 5% RH 300 300 3
Long Term 30 OC ± 2 OC, 65% ± 5% RH 700 700 7
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Samples are considered for repeat analysis and shelf life of 5 years.
5.5.2 Stability Section officer shall prepare “Stability Sample Label” and affix on the sample
container indicating (a) Product Name (b) Batch No. (c) Pack Style (d) Storage
Condition (e) Stability Start Date. Samples shall be charged as per the required storage
condition and entries shall be made in the “Stability Sample Log In Register” (refer
Format no. SPL/QA/058).
5.5.3 Samples shall be charged into the stability chamber within + 2 day after receipt of
sample.
5.5.4 Samples shall be incorporated into the stability program at all storage conditions on
same date.
5.5.5 Stability start date shall be the date of charging of samples into Stability Chamber.
Subsequent time intervals shallCondition
Study be counted on the basis of "Date
Applicable of charging
Frequency into the
(Months)
Stability Chamber".
5.5.6 ASampleLong
shallTerm 30 OinC Stability
be charged ± 2 OC, 65% ± 5% within
Chamber RH 0,one
3, 6, 9, 12,of18,
month the24, 36, 48,
batch 60 by
release
Quality Control. In case, the samples are not charged into the Stability Chamber within
one month, the samples subjected for stability studies shall be reanalyzed. This result
O
Bshall be
Accelerated
considered as 40 2 OC, 75% ± 5% RH 0, 3 & 6
C ±analysis.
initial
5.6 Storage Conditions and Testing Frequency for Drug Product:
5.6.1 The storage condition and testing frequency for the samples subjected for stability
studies are :
As long term condition taken as 30°C ± 2°C, 65%±5% RH there will be no intermediate
condition.
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5.6.2 Analysis at the time of release (Finished Product analysis), is considered as initial or “0”
month analysis and if finished product analysis date and sample charging date differs by
more than one month, 0 month’s analysis shall be done at the time of charging of samples
to stability chamber.
5.6.3 If sufficient stability data for 3 batches are available and product is stable, some
frequencies in the yearly batch samples may not be analyzed. But samples of next
frequency shall be analyzed.
5.6.4 Stability batches, which are kept for various changes, shall be analyzed as per frequency
mentioned in table or as indicated in Validation Protocol.
5.6.5 If it is not possible to analyze the samples at specified storage conditions within the time
interval specified, samples shall be analyzed for that specified condition at next time
interval indicating justification for the same. e.g. If analysis of sample at 30 OC / 75 %
RH at 12 months is not possible within 30 days of time interval, it shall be analyzed at
18 months.
5.7 Procedure for withdrawal of samples from Stability Chamber:
5.7.1 The withdrawal of samples shall be carried out within -15 and +15 days from stipulated
date at Accelerated, and Long term storage condition.
5.7.2 The samples withdrawn from the chamber shall be stored in QC laboratory at ambient
condition.
5.7.3 The sample shall have all details like Product Name, Batch Number, Storage Condition,
and Frequency in months and Pack style.
5.7.4 According to the “Stability Monthly Planner ” (Stability sample analysis due register
format No. SPL/QA/062) Stability Section In-charge shall schedule the plan and give the
instruction to the analyst to analyse the sample.
5.8 Procedure for analysis and review the data:
5.8.1 Stability Section In-charge shall plan the analysis of stability samples to analyst on the basis
of analyst training and experience.
5.8.2 Stability In-charge shall issue the worksheet.
5.8.3 Analyst shall perform the analysis as per the respective standard testing procedure.
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All raw data shall be recorded into the respective worksheet at the time of analysis.
5.8.4 The samples shall be analyzed for the parameters like Appearance / Description, Colour,
Hardness, Friability, Moisture content / Loss on Drying, Disintegration test, Dissolution
rate, Related substances, Assay and Microbiological test as per finished product
specifications except Identification, Diameter, Thickness, Uniformity of content,
Uniformity of weight. If the parameters are not the part of specification, it shall not be
tested.
5.8.5 If stability data is required to be sent to Analytical Development Laboratory (ADL), R & D,
or Regulatory authorities, the compiled data shall be approved by Head - Quality Assurance
and Unit Head and forwarded to Managing Director for further approval. A Photostate copy
of the same shall be kept in Stability Section.
5.9 Investigation on Stability Data:
5.9.1 If stability data shows significant change for critical parameters as mentioned below, the
results shall be investigated.
Assay : More than 5 % change from initial value.
5.9.2 Any result, which is found out of specification (OOS), Section In-charge shall intimate to
Head - Quality Assurance.
5.9.3 Head - Quality Assurance and Section In-charge shall investigate the OOS results within
three days according to the current version of SOP on OOS and prepare the laboratory
investigation report.
5.9.4 In an event of stability failure, Head - Quality Assurance shall approve the Out of
Specification report and forward to Managing director.
5.10 Discontinuation Of Stability Study
5.10.1 Decision of discontinuation of stability studies shall be taken on the basis of response
received from Head- Quality Assurance on Non-conformity report.
5.10.2 End of shelf life or study is over and extension of shelf life is not required.
5.10.3 Stability Study of condition 40 OC /75 % RH shall be discontinued at the end of 6 months.
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5.11 Procedure for preparation of Stability Study Work Sheet Protocol:

5.11.1 Stability study Work Sheet protocol shall be product specific and prepared for:
 New Drug Product

 On going stability studies for all existing Drug Products
 Validation batches
5.11.2 Stability study Work Sheet and protocol shall be prepared by the Officer – Quality
Assurance
5.11.3 Stability Study Protocol (New Product) number shall have 14 characters as given
below
XXX / XXX / XXX / XX

th th th th th th th
First 4 5 ,6 8 9 , 10 12 13th and
three character and 7th character and 11th character 14th
characters character character character
SSP Slash Product Slash Sequential Slash Revision
Code Number No.
A. 1st three characters are letters of alphabet denoting the “SSP” (Stability Study
Protocol) for New Product.
B. 4th character denotes “/” (Slash).
C. 5th, 6th and 7th characters are letters of alphabet denoting the “Product Code”. If
product code is not of three letters, directly write whatever product code is there. If
product code is of 2 digits then 0 will be prefixed.
D. 8th character denotes “/” (Slash).
E. 9th , 10th and 11th characters are denoting the “Sequential Number” for the
protocol Number of that particular code.
F. 12th character denotes “/” (Slash).

G. 13th and 14th characters are denoting the revision number.
5.11.4 Stability study protocol shall be reviewed by the Stability Section In-charge /
Executive – Quality Assurance.
5.11.5 Head - Quality Assurance shall approve the protocol.
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6. Records/Formats:
SPL/QA/058 - Stability Sample Log In Register

SPL/QA/059 - Format for Reporting Stability Study Data
SPL/QA/060 - Stability Parameters For Different Dosage Forms
SPL/QA/061 - Nonconformity Report of Stability Study
SPL/QA/062 - Monthly stability schedule
7. Annexure:
NA
8. Reference:
NA
9. Abbreviations:
SOP - Standard Operating Procedure
No. - Number
NMT - Not More Than

O
C - Degree Centigrade
RH - Relative Humidity
QA - Quality Assurance
QC - Quality Control
R&D - Research and Development (Formulation)
ADL - Analytical Development Laboratory
LOD - Loss on Drying
OOS - Out of Specification
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10. Revision History:
Revision No Effective date Reason for Revision

00 New Document
Title: Procedure for Stability Study of Finished Products
SOP. No. : SPL/ SOP/QA/038
Prepared By Checked By Reviewed By Approved By

Stability Sample Login Register
Format No: SPL/QA/058
Name of Drug Product
Sr. Batch Mfg Exp. Batch Pack Qty. of Total Stability start date Sign Chkd
No. No. Date Date size Style sample at Quantity Date by
of
sample
40°C 30°C 0 3 6 12 18 24 36 48 60
75% 60% M M M M M M M M M
RH RH









Format for Reporting Stability Study Data

Sample Stored At :
Product :
Label Claim :
Stability Started on :
Specification Ref. No. :
Batch No. :
Mfg. Date :
Exp. Date :
Batch Size :
Test Specification Batch No. Initial Stability Station
Compiled By Approved By Approved Approved By (Corporate Division)

By
Signature
Date
Name
Designation Stability -Officer Head Quality Head Quality Unit Head
Control Assurance

Stability Parameters for Different Dosage Forms

Characteristic Tests Tablets Capsules Oral liquids Dry Powder

Appearance
Colour
Odour
Shape
Hardness
Friability
Moisture
Dispersion Time
Disintegration
Dissolution
Related Substances
Assay
Total Bacterial Count
Mould & Yeast
Pathogens

Nonconformity Report of Stability Study

Name of product :
Product code :
Defining of Nonconformity:
Batch Number ;
Results of accelerated study :
Results of real time condition :
Additional information (if
any):
Course of Action Finalized by Technical Team
Disposition
Corrective Action
Preventive Action
Head – R&D (F) Head -ADL Head – Manufacturing Head – QC

Sign /
Date
Closure by Head-QA
The reference documents enclosed are checked with reference to above mentioned action plan
and found satisfactorily.
1.
2.
3.
4.
Hence the non-conformity report shall be considered as closed.
Reviewed by Approved by
Head- QA

Monthly Stability Schedule

Month:-
Sr. Date Product Batch Mfg. Exp. Stability Stability COA Remark Head - QA
No. No. Date Date station analysis Submitted Sign /Date
Due on Done on on

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SOLITAIRE PHARMACIA PVT. LTD.

To enter the stability samples details in “Sample Login Register”.

To review the compiled stability data at each station.

To raise Out of Specification (OOS) wherever applicable.

To maintain all Stability Study records.

Executive- Quality Control

Head – Quality Assurance, Head – Quality Control:

To approve the Stability Study Work Sheet Protocol.

To review and approve the stability study data.

To investigate the Out of Specification (OOS) results.

To authorize any deviation during Stability Study of Drug Product.

To investigate and approve Out of Specification report.

5.2.4 In case of failure of stability chamber, it shall be repaired by in-house or vendor

5.3 Selection of Batches and Stability Commitment:

5.5 Procedure for storage of samples into the Stability Chamber:

Accelerated 40 OC ± 2 OC, 75% ± 5% RH 300 300 3

Long Term 30 OC ± 2 OC, 65% ± 5% RH 700 700 7

5.6 Storage Conditions and Testing Frequency for Drug Product:

5.7 Procedure for withdrawal of samples from Stability Chamber:

5.8 Procedure for analysis and review the data:

5.8.2 Stability In-charge shall issue the worksheet.

5.9 Investigation on Stability Data:

Assay : More than 5 % change from initial value.

5.10 Discontinuation Of Stability Study

5.11 Procedure for preparation of Stability Study Work Sheet Protocol:

 New Drug Product

XXX / XXX / XXX / XX

D. 8th character denotes “/” (Slash).

F. 12th character denotes “/” (Slash).

5.11.5 Head - Quality Assurance shall approve the protocol.

SPL/QA/058 - Stability Sample Log In Register

SOP - Standard Operating Procedure

NMT - Not More Than

R&D - Research and Development (Formulation)

ADL - Analytical Development Laboratory

LOD - Loss on Drying

OOS - Out of Specification

10. Revision History:

Revision No Effective date Reason for Revision

Title: Procedure for Stability Study of Finished Products

SOP. No. : SPL/ SOP/QA/038

Prepared By Checked By Reviewed By Approved By

Title: Procedure for Stability Study of Finished Products

SOP. No. : SPL/ SOP/QA/038

Prepared By Checked By Reviewed By Approved By

Title: Procedure for Stability Study of Finished Products

SOP. No. : SPL/ SOP/QA/038

Prepared By Checked By Reviewed By Approved By

Title: Procedure for Stability Study of Finished Products

SOP. No. : SPL/ SOP/QA/038

Prepared By Checked By Reviewed By Approved By

Title: Procedure for Stability Study of Finished Products

SOP. No. : SPL/ SOP/QA/038

Prepared By Checked By Reviewed By Approved By

Title: Procedure for Stability Study of Finished Products

SOP. No. : SPL/ SOP/QA/038

Prepared By Checked By Reviewed By Approved By

Title: Procedure for Stability Study of Finished Products

SOP. No. : SPL/ SOP/QA/038

Prepared By Checked By Reviewed By Approved By

Title: Procedure for Stability Study of Finished Products

SOP. No. : SPL/ SOP/QA/038

Prepared By Checked By Reviewed By Approved By