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Sunday, September 7, 2008

Validation Master Plan Product Validation format

In todays post I will like to provide you information on Product Validation for who gmp with respect to who gmp guidelines .a master validation plan is prepared before actual doing a validation of a product and here I am giving you a sample of a validation ,master plan as it is followed by my who gmp approved company in UK.

MASTER VALIDATION PLAN
Objective
The purpose of this plan is to cover validation process for manufacturing filling , cleaning and filling of “YOUR PRODUCT NAME” manufactured at “your company name and address”
Scope
This validation exercise covers Performance Qualification [ PQ ] of manufacturing, filling , cleaning and packing operations for “YOUR PRODUCT NAME”
Responsibility
Following personnel would execute the Pharmaceutical Validation plan .
a) QA Executive and Production Executive are the validation co-ordinators for the exercise.
b) Manufacturing of the product will be performed in presence of Production Executive , Quality Assurance Executive.
c) Quality Control chemist will draw samples for analysis.

Analysis of the samples drawn will be performed as directed by QA Executive and Manager, Quality Assurance.
Approach
The approach for this exercise is to validate the manufacturing, filling, cleaning and packing process of “YOUR PRODUCT NAME”.

Process parameters which affect final product quality are considered as Critical with respect to
the Performance Qualification.

Following aspects are considered as critical parameters
a. Manufacturing process
i. Line clearance for manufacturing
ii. Preparation of carbopol phase
iii. Preparation of drug dispersion
iv. Distribution of active in the bulk
v. Mixing of bulk.
vi. Transfer to Storage vessels

b. Analytical parameters – pH , Identification for Active ingradient Name and Assay for Active ingradient Name Content for bulk sample from the top level, middle level and bottom level of the storage vessel.

c. Filling process
i. Line clearance for filling
ii. Fill weight
iii. Weight variation
iv. Quality of Crimping and coding
v. Rejection during filling process

d. Packing activity
i. Line Clearance for packing activity
ii. Legibility and correct batch details on the inner carton
iii. Packing of tubes into cartons along with inserts
iv. Legibility and correct batch details on the outer carton
v. Packing of correct number of inner cartons in the outer cartons
vi. Packing of correct number of outer cartons in the shippers.

e. Cleaning of equipments
i. cleaning validation ( traces pf previous product ingredients. )

Subject for Validation :
Three batches of “YOUR PRODUCT NAME” have been selected as the subject for performance validation.

Validation Review :
Revalidation will be carried out every five years or when there is a major change in the manufacturing process, manufacturing equipment or a new pack is introduced.
Validation review will be performed every two years.

The Validation batches will be released to the market only after

1 Validation plan and protocols are signed off.
2 All the acceptance criteria as per the protocol are met.

Validation plan

Prepared by :_______________Date___________
(QA Executive )

Checked by :_______________Date ___________
(Production Executive )

Verifed by :________________Date ____________
( QC Executive )

Approved by :______________Date ____________
( QA Manager )

Authorised by :_____________Date ____________
( Partner of Company)



ReF No : “YOUR COMPANY NAME”/VP/ALE/01
VALIDATION PROTOCOL

ABSTRACT

The validation of the three production batches of “YOUR PRODUCT NAME” is the subject of this validation exercise.

This protocol discusses the pharmaceutical aspects of the validation exercise. A description of the process and its critical and non-critical stages is included with a rationale for the testing programme. The formula and process flow sheets for the exercise are included in the appendices to this protocol.

Three batches of “YOUR PRODUCT NAME” have been selected as the subject for the Performance Qualification exercise.

The Batch numbers for validation exercise are :

Batch Nos Mfg Date Exp Date Batch Size


OBJECTIVE :

The objective of this Performance qualification exercise is to demonstrate that “YOUR PRODUCT NAME” can be manufactured as per the manufacturing process described in the manufacturing guide Ref No :
After final mixing , the bulk will be tested for Identification , Description , Active ingradient Name content and pH. The finished product filled in aluminium collapsible tubes will be tested again for Identification , Description , Active ingradient Name content and pH. The finished goods will be analysed fully as per the specification No “YOUR COMPANY NAME” QC FP R 00

INTRODUCTION :

It was decided to conduct a Performance Qualification Exercise to validate the processing
parameters of the three batches of “YOUR PRODUCT NAME” using the production facilities at address

Each stage of the manufacturing process has been considered for potential effect on the variability in quality of the finished product.

A flow diagram for the manufacturing process at each stage including details of the formulation and equipment for “YOUR PRODUCT NAME” is shown in page 10

Process stages where the performance of the process affects the final product quality were
considered CRITICAL and a Performance Qualification Protocol (PQP) has been defined.

Performance Qualification Protocol :

The Performance Qualification Protocol for CRITICAL process operations give as follows :

a. Process parameters to be validated
b. The Experimental program to be performed including sampling
procedure
c. The acceptance criteria .


Three batches of “YOUR PRODUCT NAME” (Batch size: 400 Kg and Kg respsctively )
will be manufactured as per the manufacturing guide

Permanent amendment to Manufacturing Guides and Batch Manufacturing Records will be made on successful completion of the validation exercise.

DESCRIPTION OF CRITICAL AND NON CRITICAL PARTS OF THE MANUFACTURING PROCESS:

RAW MATERIAL
Non- Actives
The excipient raw materials used in “YOUR PRODUCT NAME” are purchased from approved suppliers and
are individually assessed by the Quality Assurance Dept. Hence the non-actives are
considered NON-CRITICAL with respect to this Performance Qualification exercise.

Active

The active raw materials used in “YOUR PRODUCT NAME” are purchased from approved suppliers and are
individually assessed by the Quality Assurance Dept. Hence the actives are considered NON-
CRITICAL with respect to this Performance Qualification exercise.


DISPENSING OF RAW MATERIALS

Dispensing of raw materials is carried out according to the manufacturing guide {Ref.: } and
the SOP specified in the stores and is therefore considered as a NON-CRITICAL with respect
to Performance Qualification.



MANUFACTURING:
PREPARATION OF THE BULK SUSPENSION
1. Line clearance for manufacturing
The line clearance procedure is followed by the manufacturing process for the new product.
During Line clearance the equipments used for manufacturing process is checked for following
parameters.
a. Cleaning of the manufacturing equipment with suitable solution such as raw water with detergent solution followed by Demineralised water.
b. In-process QC checks for the traces of the previous product by suitable analytical methods.
c. Cleanliness of the area for manufacturing.
d. Status labeling of the area of manufacturing.

2. Preparation of carbopol phase
The carbopol phase is the important stage in the manufacturing process. This stage is
involved in formation of gel base for the product. This stage is considered CRITICAL with respect to Performance validation.

3. Preparation of drug dispersion
A uniform dispersion of the drug is prepared in the mixing tank with high speed stirrer ( Turbo disperser) and transferred to the main vessel. Air entrapment is avoided during stirring and it is ensured that the dispersion is free from lumps before addition to the final mixing tank.
The mixing time and RPM of the stirrer used for achieving uniform dispersion are noted.
This step is considered as CRITICAL with respect to Performance Qualification.

4. Distribution of active in the bulk
The drug dispersion is transferred in the main mixing tank slowly to get uniform distribution in
the carbopol phase. The mixing time and RPM of the stirrer used for achieving uniform
distribution are noted. This step is considered as CRITICAL with respect to Performance
Qualification.

5. Mixing of bulk.
After addition of all the ingredients, the gel is stirred to achieve uniformity of bulk gel.
Inadequate mixing would result in content non-uniformity of the bulk gel. This step is
considered as CRITICAL with respect to Performance Qualification.

6. Transfer to Storage vessels
The batch is transferred to the cleaned storage SS vessel. This step is considered as NON-
CRITICAL with respect to Performance Qualification.

Analytical parameters
The analysis defined for the bulk gel will be carried out on three batches as per the specification method : “YOUR COMPANY NAME” QC IP R 00 for Description , Identification for Active ingradient Name , pH ad content of Active ingradient Name to demonstrate the consistency of the process.


Filling process

1. Line clearance for filling
The line clearance procedure is followed by the filling process for the new product.
During Line clearance the machines used for filling process is checked for following parameters.
a. Cleaning of the filling machines with suitable solution such as raw water with detergent solution followed by Demineralised water.
b. In-process QC checks for the traces of the previous product by suitable analytical methods.
c. Cleanliness of the filling area .
d. Status labeling of the filling area .

2. Fill weight
The manufactured gel is filled in the collapsible aluminium tubes. Dosage of particular weight is given in the tube say 5 gm / 15 gm. The machine is so adjusted that the fill weight falls within the range specified in the batch manufacturing record. The fill weight is checked when the filling machine hopper is full, half filled and at the 3/4th level of the product in the hopper.

3.Weight variation
The weight variation of the filled tubes are checked at a frequency of 30 minutes and checked
for adjusted fill weight. 500 filled tubes are checked for fill weight and weight variation
checked.

4.Quality of Crimping and coding
The filled tubes are checked for quality of crimp and the coding for batch details.

5. Rejection during filling process
The rejections arising during the filling process are checked and analysed at various stages such as fill weight, crimping and coding. The total rejections should not exceed 1 % .

6. The sampling and testing at this stage is designed to demonstrate that throughout the filling
operation the filled product in tubes is consistently uniform in content and fill weight .


Packing activity

1. Line Clearance for packing activity
The line clearance procedure is followed by the packing activity for the new product.
During Line clearance the machines used for packing activity is checked for following parameters.
a. In-process QC checks for the extraneous matter , previous product materials.
b. Cleanliness of the packing area.
c. Status labeling of the packing area .

2.Legibility and correct batch details on the inner carton
The batch details on the inner cartons are checked for correctness and legibility by the
supervisors and cross checked by the QC department.

3.Packing of tubes into cartons along with inserts
The operators are trained to carryout packing activity. The individual tubes are packed in the
overprinted inner cartons along with the insert literature.

4. Legibility and correct batch details on the outer carton
The batch details on the outer cartons are checked for correctness and legibility by the
supervisors and cross checked by the QC department.

5.Packing of correct number of inner cartons in the outer cartons
The operators are trained to carryout packing activity. The inner cartons are packed in the
overprinted outer cartons.

6. Packing of correct number of outer cartons in the shippers.
The packed outer cartons are then packed in the printed shippers .

Cleaning of equipments

1. Cleaning validation ( traces pf previous product ingredients. )
After the completion of the batch, when the new product is manufactured the cleaning
procedure is employed for manufacturing, filling process.

All the above process is considered as CRITICAL with respect to Performance
Qualification.

The testing defined for the final mixing and filling / packing of the suspension will be carried out on three batches as per the specification method : to demonstrate the consistency of the process.

All analytical instruments used for the analysis must be in a valid calibrated state.
REPORT FOR VALIDATION OF MANUFACTURING PROCESS AND FILLING OF “YOUR PRODUCT NAME”

Introduction:
“YOUR PRODUCT NAME” contains Active ingradient Name as active ingredient. In order to establish the uniformity of distribution and uniformity of filling of the batch this validation exercise was performed.

Study:
Process of manufacturing, filling, packing and cleaning of the product were studied for the validation exercise.
Each stage of the manufacturing process has been considered for potential effect on the
variability in quality of the final product.

A flow diagram for the manufacturing process at each stage including details of the formulation, plant and equipment for “YOUR PRODUCT NAME” is given in page 9 & 10 respectively.

Process stages where the performance of the process affects the final product quality were
considered CRITICAL and a Performance Qualification Protocol (PQP) has been defined.
The stages which are well controlled when performed in accordance with the defined operating
procedures, if test data is available or previously generated validation data is available are
considered NON -CRITICAL with respect to this Performance Qualification Protocol (PQP).

Following were considered as critical and non-critical parameters for the study and observations on the same were recorded accordingly.

Following are considered as critical parameters :
i) pH of the water used for the manufacture
ii) Preparation of carbopol phase
iii) Preparation of drug dispersion
iv) Distribution of active in the bulk
v) Mixing of bulk


Conclusion:
From the studies performed it was observed that in order to achieve uniform distribution of Active ingradient Name , it requires mixing for 30 minutes. The process of manufacturing and filing of “YOUR PRODUCT NAME” is well under control and the parameters studied indicate satisfactory uniformity of contents in the bulk. Filling of the gel was also observed to be satisfactory in terms of fill weight crimping and coding quality.

A copy of Protocol, Observations and Supplementary Data are appended to this report.

FOR YOUR REFERANCE I AM GIVING HERE A LINK TO WORD FILE OF A ACTUAL
PRODUCT VALIDATION DOCUMENT . YOU CAN REFER THIS FOR YOU OR MODIFY , TAKE GUIDANCE AND DO YOUR SELF CHANGES.


Email this to your colleague friend or who is working with pharmaceutical manufacturing firm
good manufacturing practice guide for pharmaceuticals manufacturing
pharmaceuticals manufacturing guide
Quality assuarance guide for pharmaceuticals

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2 comments:

Rogelio Reyla said...

Please send me A copy of Protocol, Observations and Supplementary Data since the file does not exist in the hyperlink.

Thank you.

Rogelio Reyla said...

Please send me a A copy of Protocol, Observations and Supplementary Data since the file does not exist anymore in the google docs link page.
thank you.

My email add is rjreyla@jmtolmannlab.com

Posted by: Martin

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