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Tablet Process Validation
Tablet Process Validation
Tablet Process Validation
PROCESS
VALIDATION
PROTOCOL FOR TABLETS
TABLE OF CONTENTS
Page
S.NO. SECTION
No
1. Protocol approval
2. Purpose
3. Responsibilities
4. Requirements
5. Personnel Responsibilities
6. Validation parameters
7. Limits
8. Conclusion report
1. PROTOCOL APPROVAL
This document is prepared by the validation and the GMP compliance (QA) team of
xxxxxxxxxxxxxxxxx under the authority of Manager QC & A. Hence this document before being
effective shall be approved by xxxxxxxxxxxxxxx QA team.
Manager production
Manager Engineering
Manager QA
2. PURPOSE
Process validation is establishing documented evidence which provides a high degree of assurance
that a specific process (such as manufacturer of pharmaceutical dosages forms) will consistently
produce a product meeting its predetermined specifications and quantity characteristics.
3. RESPONSIBILITIES
5. PERSONNEL RESPONSIBILITIES:
The perfect validation program necessitates various departments involvement mainly to balance the
total system functioning for its effective utilization for success criteria compliance on regular basis.
Quality assurance department initiates validation program with protocol, specified procedure and
success criteria. Quality control personnel are responsible for the validation run as per the protocol
and during validation maintenance departments have to cooperate to the quality control personnel.
6. VALIDATION PARAMETERS:
6 Tablet coating
7 Tablet packing
Formulation:
Batch Size:
Sr Ingredients/Excipients Unit per Std. Overages Dispensed Weight Checked
No Tablet Qty. Quantity by by
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
FLOW SHEET:
Prepare production order and according RM dispensing as per Bill of material
to that issue the BPR
Drying
Dry milling Slugging, Milling (if required)
Mixing
Tablet packing
Sampling point
A detailed list of equipment used for validation together with the cleaning status will be provided in the
manufacturing documents.
Binder Quantity
Binder addition rate
Binder addition time
Temperature of binder
Mixing time after binder addition /Total granulation time
Uniformity of granulated mass (Visual Checking)
3. Drying Dryer outlet temperature
Dryer inlet temperature
Drying load
Total drying time
Weight of the Dried granules
4. Milling Speed of machine
Direction of knives
5. Lubrication Load size
Occupancy
Speed of equipment (RPM)
Total time of mixing
Assay - (individual sample)
6. Compression Temperature of area
Humidity of area
Machine Details
Weight variation of 20 tablets
Average weight of tablet
Disintegration time
Friability
Diameter (Length)
Thickness
Hardness
Assay
Content uniformity
Dissolution
Prepared By Reviewed by Approved by
Machine setting
Sr. No Process / Variable Remarks
( Control Variables)
1 Blend Manufacturing
PREMIXING:
MIXING:
Sampling Qty.: -Depends on quantity required for analysis.
Sampling Time: - (bracketing the time between 2 to 3 intervals of total mixing time)
While mixing is on: -
After ____ minutes,
After ___ minutes,
After _____ minutes
______ minutes _______ minutes ______ minutes
(Top , Middle & Bottom) (Top , Middle & Bottom) (Top , Middle & Bottom)
Total samples: 9 Samples
DRYING:
T2
Top View Sampling
Top B2
B3
TOP VIEW
T1 T3
B1
Front side Bottom
T2
Loading Valve
Sampling Points
B3
B3
B2
T3
T2 T1
M
T4 T3
T1
T
1 B1
B4
Prepared By Reviewed by Approved by
B2 B3
B1
Sampling points T1, T2, T3 for top T4 B4 for middle, B1, B2, B3 for bottom sampling.
COMPRESSION:
Sampling Qty.: -Depends on quantity required for analysis.
Sampling Time: - (bracketing the time between 2 to 3 intervals of total compression time)
After ____ minutes,
After ___ minutes,
After _____ minutes
______ minutes _______ minutes ______ minutes
COATING:
Sampling Qty.: -Depends on quantity required for analysis.
Sampling Time: - (Bracketing the time between 2 to 3 intervals of total coating time)
While coating is on: -
After ____ minutes,
After ___ minutes,
After _____ minutes
______ minutes _______ minutes ______ minutes
Sampling:
Stage / Test Parameter Equipment Acceptance Criteria
(Size, Location & Time)
Premixing Stage Variation between the results of Assay shall
not be more than 2%
Mixing
Drying Loss on drying Between 2.0 to 4.0%
Mixing
Lubrication Variation between the results of assay shall
not be more than 2%
Tablet compression Physical Parameter (I.P.Q.C)
Tablet coating Weight Gain
Tablet packing Leak Test
Mean
Standard Deviation
% Relative standard deviation
Mean
Standard Deviation
% Relative standard deviation
Mean
Standard Deviation
% Relative standard deviation
Analyst: Date
Remarks:
Checked By: _________________________ Date: ____________________
Drying Load :
Total Drying time : Minutes
Weight of the dried granules :
Remarks:
Plan: Samples to be drawn at of blender from 3 different locations (Top, Middle & Bottom)
Mean
Standard Deviation
% Relative standard deviation
Prepared By Reviewed by Approved by
Mean
Standard Deviation
% Relative standard deviation
Mean
Standard Deviation
% Relative standard deviation
Remarks:
Plan: Compressed tablets to be analyzed for: Average weight, Weight variation and Physical parameter
at an interval of 2 hours
Requirement RPM: RPM: RPM:
Time
Average weight
Thickness mm
Hardness in kg./sq. cm2
Friability in %
DT in min.
Weight variation after validated RPM __________
Weight variation:
Time Time Time Time Time
Remarks:
Plan: Coated tablets to be analyzed for Weight gain, weight variation and DT. At an interval of __ hours
Weight variation:
Time
Weight variation
Remark:
5.2
5.3
5.4
Remark:
Result: The sample referred above complies / does not comply with the standard prescribed as per In
house Specification.
28
Utilities:
1 AHU System
2 Water System
3 Compressed Air
4 Steam
5 Lightning
6 Drain
Remark:
Analytical Method Validation protocol attached
Conclusion
Analysis By Approved By
Date Date
8. CONCLUSION REPORT
Summary report will contain discussion and conclusion , which clearly states the successful
achievement of objective of validation studies and recommended concentrations required for
sanitization, disinfections and equipment sanitization.