PHARMA DEVILS

QUALITY ASSURANCE

PROCESS VALIDATION PROTOCOL OF UN-COATED TABLET

Batch Size: 1000000 Tablets BMR No.: XXX/PRO/BMR/ZZ-00
Protocol No.: XXX/BBB/PPV/ZZ-00 Page No.: 1 of 19

PROCESS VALIDATION
DRAFT TEMPLATES
PROTOCOL
FOR
UN-COATED TABLETS
 PHARMA DEVILS
QUALITY ASSURANCE

PROCESS VALIDATION PROTOCOL OF UN-COATED TABLET

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TABLE OF CONTENTS
SR. NO. SUBJECT PAGE NO.
1. PROTOCOL APPROVAL 3

2. INTRODUCTION 4

3. OBJECTIVE 4

4. SCOPE 4

5. VALIDATION CRITERIA 4

6. REVALIDATION CRITERIA 4

7. REASON FOR VALIDATION 4

8. PRODUCT PROFILE 5

9. MASTER FORMULA 5

10. RISK ANALYSIS 7

11. SAMPLING PROCEDURE 8

12. FLOW DIAGRAM (PROCESS) 9

13. MANUFACTURING PROCEDURE 10

14. CALIBRATION / QUALIFICATION 12

15. SAMPLE SUMMARY 13

16. RAW MATERIALS RATIONALE 15

17. SPECIFICATIONS 15

18. DESTRUCTION OF REMAINING VALIDATION SAMPLES 21

19. SUMMARY, CONCLUSION AND APPROVAL 21

20. ABBREVIATIONS 21
 PHARMA DEVILS
QUALITY ASSURANCE

PROCESS VALIDATION PROTOCOL OF UN-COATED TABLET

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1.0 PROTOCOL APPROVAL:

Department Name Signature Date

Quality Assurance
Prepared By

Production

Quality Control
Reviewed By

Engineering

Approved By Head-QA
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QUALITY ASSURANCE

PROCESS VALIDATION PROTOCOL OF UN-COATED TABLET

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2.0 INTRODUCTION:
Product shall be manufactured using the Wet Granulation Technology. The batches manufactured
during the validation shall be setup for the stability study and other parameters monitored periodically
and shall be reviewed by the validation Team.

3.0 OBJECTIVE:
The objective of this exercise is to develop a PROCESS VALIDATION PROTOCOL to validate the
process and have documented evidence to ensure that critical process variables are checked during
validation. Also to demonstrate the process capability of the product meets its predetermined
specifications and quality attributes.

4.0 SCOPE:
This protocol for the Process validation of product name formulation defines the procedural aspects to
be followed while carrying out Process validation activity that includes prerequisites before
commencing the actual work like, Master formula and process, approved vendors and characteristics of
raw materials. Also it defines the acceptance criteria, re-validation criteria and justification for critical
process parameters.

5.0 VALIDATION CRITERIA:

 Process validation batch shall be manufactured as per process steps given in the Master
Manufacturing Formula.
 The batches manufactured during process validation shall meet the criteria defined in product
specification.

6.0 REVALIDATION CRITERIA:

The process shall be revalidated whenever there shall be changes in:
 Manufacturing process and the product formula.
 Manufacturing site or location.
 Change in critical equipment in manufacturing process
 Change in batch size
 PHARMA DEVILS
QUALITY ASSURANCE

PROCESS VALIDATION PROTOCOL OF UN-COATED TABLET

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7.0 REASON FOR VALIDATION:

 The product Name will be manufactured as validation batch due to new product in Plant,
 Transferred/change in facility from another location of Pharmadevils Pvt. Ltd.

8.0 PRODUCT PROFILE:

Name of the product : ………………………………
Label Claim : Each un-coated tablet contains:
API-1 (BP) .......................................... 12 mg
API-2 (IP) …................................…… 90 mg
API-3 (BP) ........................................ 100 mg
Shelf Life : 24 Months
Appearance : Biconvex, un- coated tablets having plain surface on both sides.
Storage Condition : Store in cool and dry place. Protect from light.

9.0 MASTER FORMULA

Batch size: 1000000 Tablets MMF No.: XX/YY/ZZ/AA-01
Sr. No. Components Specification Weight/Tablet in mg
Uncoated Tablets
Dry mixing
1. API-1 BP BP 100.00
2. Croscarmellose sodium IP IP 51.00
3. Microcrystalline cellulose IP (PH 112) IP 20.00
4. Colloidal silicon dioxide IP IP 9.00
Binder Preparation
5. Povidone IP (K-30) IP 7.20
6. Isopropyl alcohol IHS * IHS 210.00
Pre-Lubrication
7. API-3 BP BP 79.44
8. API-2 IP IHS 62.7
9. Croscarmellose sodium IP IP 34.00
10. Colloidal silicon dioxide IP IP 1.00
11. Polacrilin potassium USP USP-NF 23.70
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PROCESS VALIDATION PROTOCOL OF UN-COATED TABLET

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Lubrication
12. Magnesium Stearate IP IP 4.40
Weight of uncoated tablet XXX.00
* Not considered in final weight of tablet.

10.0 RISK ANALYSIS:

The product shall be manufactured in General block with batch size of 1000000 Tablets as a validation
batch. product shall be manufacturing by using wet granulation. Raw materials of approved vendor
source shall be sifted, dry mixed, granulated using binder solution and dried at 50 OC ± 5 OC. Dried
granules are sized (Sifted and milled) and lubricated using Magnesium stearate. An Approved
lubricated granules will be compressed by using 11.5 mm diameter circular standard concave punches
having plain surface on upper and lower punch.

 Dispensing:
Dispensing of all raw material is done by using calibrated balance, all raw material are procured from
approved vendor, there is no critical parameter identified for validation during dispensing stage.

 Granulation:

 Sifting of raw material: Sifting of raw material is done by specified sieve under supervision of the
trained personnel. Sieve integrity is verified before and after processing.
 Dry Mixing: Dry mixing of the material is performed by laid down procedure and dry mixing
uniformity was established during optimization of product, at dry mixing stage critical parameters are
mixing time and speed of mixer is to be monitored. At the end of 10 minutes Samples from various
locations shall be withdrawn and evaluated for mixing uniformity. Composite sample shall be
withdrawn and evaluated for untapped bulk density, tapped bulk density, for record purpose as part of
validation.
 Binding: At the time of binding manual monitoring is to be done for the defined mixing speed of
agitator and chopper and end point of the granulation to be monitored by checking the mass
intermittently for consistency and amperage load monitoring.
 Drying: At the Drying stage of the granules Inlet temperature to be monitored and sample to be
withdrawn during drying and tested for LOD till the end of drying to find out rate of drying and at end
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PROCESS VALIDATION PROTOCOL OF UN-COATED TABLET

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of drying sample withdrawn from seven location of bowl for checking of drying uniformity for specified
LOD by using IR moisture balance.

 Sizing of Granules: Sizing of granules is to be milled by using Multimill, Speed of the Multimill and
direction of shafts is to be monitored and sample to be withdrawn at the end of the sizing operation for
the monitoring of particle size distribution, untapped bulk density, tapped bulk density and LOD at 105
ºC on IRMB for record as part of validation.

 Lubrication: Critical Process variable to be monitor about speed of blender and mixing time of
granules and sample to be withdrawn from ten location for verification of blend uniformity and also
composite sample to be withdrawn for analysis particle size distribution, untapped bulk density, tapped
bulk density and for complete analysis as per QC in process specification.

 Compression:
During compression stages physical parameter, assay and dissolution as per sample summary of tablet to
be checked at different challenges, at maximum/minimum speed, at maximum/minimum hardness, at
optimum speed and optimum hardness during – initial/ full of hopper stage, middle stage and end/ half
of hopper stage of compression process. This process will cover critical process variables such as effect
of speed and compression force. After completion of compression process composite sample to be
withdrawn for analysis as per QC in-process specification.

11.0 SAMPLING PROCEDURE:

 All validation samples except unit dose blend samples shall be placed in clean container and labeled.
 Unit dose blend sample shall be taken in accordance with SOP for “Procedure for cleaning and
operation of sampling thief”. The samples shall be placed in container or sampling poly bag and
labeled.
 PHARMA DEVILS
QUALITY ASSURANCE

PROCESS VALIDATION PROTOCOL OF UN-COATED TABLET

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12.0 FLOW DIAGRAM (PROCESS):

13.0 MANUFACTURING PROCEDURE:

13.1 Sifting of raw material:
 Sift API-1 through s.s. sieve # 60 ASTM (250 µ) on a vibro sifter.
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PROCESS VALIDATION PROTOCOL OF UN-COATED TABLET

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 Co-sift Microcrystalline cellulose (PH 112) and Colloidal silicon dioxide through s.s. sieve # 40
ASTM (425 µ) on a vibro sifter.
 Sift Lactose Monohydrate through s.s. sieve # 40 ASTM (425 µ) on a vibro sifter.
13.2 Dry Mixing:
 Transfer the material of step 10.1 to RMG and mix for 10 minutes at slow speed.
13.3 Binder Preparation:
 Dissolve Povidone (K-30) in Isopropyl alcohol under stirring to form a clear solution.
13.4 Granulation:
 Add the binder solution obtained in step 10.3 to the dry mix of step 10.2 and granulate to obtain
dough mass of required consistency. Continue mixing till the desired dough mass is obtained. If
required add additional quantity of Isopropyl alcohol to get the desired dough mass and note down
the same.
13.5 Drying:
 Air-dry the granules in FBD for 30 minutes. Reshuffle the granules.
 Air-dry the granules in FBD for 10 minutes. Reshuffle the granules.
 Dry the granules at an inlet temperature of 50 OC ± 5 OC, till the desired LOD (Limit: 3.0 % -
4.0 % w/w at 105 OC on IRMB) is achieved.
13.6 Sifting and Milling:
 Sift the dried granules through sieve # 24 on a vibro sifter.
 Mill the granules retained on # 24 through 1.5 mm screen fitted on multimill; at medium speed
knives forward direction and pass the granules through # 24.
13.7 Pre-Lubrication:
 Co-sift API-2 and API-3 geometrically through s.s. sieve # 40 ASTM (425 µ) on a vibro sifter.
 Co-sift the materials of step 10.7.1 with the dried granules of step 10.6 geometrically through s.s.
sieve # 24 on a vibro sifter.
 Sift Croscarmellose sodium through s.s. sieve # 40 ASTM (425 µ) on a vibro sifter.
 Sift Colloidal silicon dioxide through s.s. sieve # 40 ASTM (425 µ) on a vibro sifter.
 Sift Polacrilin potassium through s.s. sieve # 40 ASTM (425 µ) on a vibro sifter.
 Transfer the sifted materials of step 10.7.2, 10.7.3, 10.7.4 and 10.7.5 into the blender and mix for
15 minutes.
13.8 Lubrication:
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PROCESS VALIDATION PROTOCOL OF UN-COATED TABLET

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 Sift Magnesium stearate through s.s. sieve # 60 ASTM (250 µ) on a vibro sifter.
 Transfer the sifted Magnesium stearate to the blender and mix for 3 minutes.
13.9 Blend Analysis:
 Intimate the Quality Control department for analysis of blend as per current in process
specifications.
13.10 Compression:
 Compress the approved blend on rotary compression machine as per in process specification.
13.11 Finished Product Analysis:
 Intimate the Q.C. for analysis of finished product as per current Finished Product Specifications.

14.0 CALIBRATION/QUALIFICATION:
All equipment utilized in conducting the Validation activity shall be within calibration / qualification.
Calibration/qualification shall be conducted in-house in accordance with approved SOPs or by an
external body. All standards used in calibration shall be traceable to a national standard and shall
remain within calibration for the duration of the Validation exercise.
 PHARMA DEVILS
QUALITY ASSURANCE

PROCESS VALIDATION PROTOCOL OF UN-COATED TABLET

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15.0 SAMPLE SUMMARY:

Sample Acceptance
Stage Location Sample Size Frequency Tests
Type Criteria
Draw samples equivalent to
10 position from Unit dose
between 1-3 unit dose (XX Mixing Uniformity**
RMG sample
mg to XX mg)* After 10 As per
$Dry
Composite sample minutes of dry specification /
Mixing Untapped bulk density
from the Top, Composite mixing To record
Approximately 20 gm * Tapped bulk density
middle and bottom sample
level of RMG
Till the desired
Composite During drying LOD at 105º C/ IR
Approximately 2 gm LOD achieved
sample operation Balance
$Drying Fluid bed drier as per BMR
At the end of
Approximately 2 gm each 6 locations LOD As per BMR
drying
LOD As per BMR
Particle Size To record
Distribution To record
At the end of
$ Milled (20#,40#,60#,80#and To record
Blender Approximately 50 g * Composite milling
granules 100#)
operation
Untapped Bulk
Density
Tapped Bulk Density
Draw samples equivalent to Unit dose After 10 As per
Pre- 10 position from between 1-3 unit dose (XX sample minutes of pre- Blend Uniformity** specification /
lubrication Blender mg to XX mg) * lubrication To record
10 position from Draw samples equivalent to Unit dose
As per
Blender between 1-3 unit dose (XX sample Blend Uniformity
specification
mg to XX mg) *
lubrication Composite 1) Particle size
sample from the 50 g* Composite distribution* For record
top, middle and After 3 (20,40,60,80 & 100#) For record
bottom level of minutes of 2) Untapped bulk For record
Blender lubrication density*,
3) Tapped bulk
density*
4) LOD*
5) For complete As per blend
analysis specification
Average weight during lubrication : 400.0 mg
* Sample shall be withdrawn and sent to QC along with test requisition.
** Duplicate sample to be retained by QA for reference purpose till testing.
$ Sample from each lot.
For unit dose sampling during Lubrication stage use 1.0 CC covette.
Sample shall be withdrawn at the depth of Approx 20 % from top layer of blend using sampling thief and
about Approx .0.6 feet from wall of the Bin Blender.
Sample shall be withdrawn at the depth of Approx 50 % from top layer of blend using sampling thief and
about Approx. 0.6 feet from wall of the Bin Blender.
Sample shall be withdrawn at the depth of Approx 80 % from top layer of blend using sampling thief and
about approx. 0.6 feet from wall of the Bin Blender.
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PROCESS VALIDATION PROTOCOL OF UN-COATED TABLET

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Stage Location Sample Sample Frequency Tests Acceptance

Size Type Criteria
1) Appearance*
2) Group Weight
3) Avg. Weight
4) Uniformity of
1) At maximum
weight
100** hardness As per
5) Thickness
Tablets 2) At minimum Specification
6) Hardness
hardness
7) Disintegration
time
8) Friability
Capability index NLT 1.33
Individual 1) Appearance*
Tablets 2) Group Weight
3) At maximum speed 3) Avg. Weight
4) At minimum speed 4) Uniformity of
Direct from 5) At optimum speed & weight
Compression hardness 5) Thickness As per
100+(20*)**
Compression # Machine a) Initial stage/ 6) Hardness Specification
Tablets
Full Hopper 7) Disintegration
b) Middle stage time
c) End stage/ Half 8) Friability
Hopper 9) Assay*
Capability index NLT 1.33
1) Appearance
2) Group Weight
3) Avg. Weight
As per
4) Uniformity of
Specification
Individual At regular interval as weight
100 Tablets (To be
Tablets per BMR 5) Thickness
recorded in
6) Hardness
BMR)
7) Disintegration
time
8) Friability
Pooled Tablet Composite End of For complete As per QC
100 Tablets*
Container sample Compression analysis* specification
* Sample shall be withdrawn and sent to QC along with test requisition.
** Duplicate sample to be retained by QA for reference purpose till testing.
*** Results to be recorded in PVR.
@ For Microbial analysis.
# Samples to be collected from L.H.S and R.H.S separately and sent to QC as per sample summery.

16.0 RAW MATERIALS RATIONALE:

The raw materials shall be tested to ensure that the materials are of the acceptable quality prior to their
use in the manufacturing. All the API and excipients shall be tested as per the respective
Pharmacopoeial monograph. The details of reference monographs, vendor and analytical reference
number are to be written in validation report.
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17.0 SPECIFICATIONS:
Specifications for Uncoated Tablets: (As per BMR/MMF*)
Sr. No. Parameter Specification
1. Light yellow circular, biconvex uncoated tablet having plain
Appearance
surface on both sides.
2. Weight of 20 tablets 8.0 g + 2.5%
3. Average weight 400.0 mg + 2.5 %
4. Uniformity of weight 400.0 mg + 5.0 %
5. Thickness 4.4 + 0.30 mm
6. Hardness NLT 6 kg/cm2
7. Friability NMT 1.0 % w/w
8. Disintegration time NMT 15 minutes

Specifications for Coated Tablets: (As per BMR/MMF*)

Sr. No. Parameter Specification
1. Reddish orange coloured, circular, biconvex, enteric coated
Appearance
tablets having plain surface on both sides.
2. Weight of 20 tablets 9.020 g 2.5 %
3. Average weight 451.0 mg ± 2.5 %
4. Uniformity of weight 451.0 mg 5.0 %
7. Thickness 4.6 + 0.30 mm
8. Disintegration time As per IP monograph for enteric coated tablets.

Note:-
 Uncontrolled Copy of Raw material specification attached*:________________
 Uncontrolled Copy of Inprocess specification for Lubricated blend and core tablets attached*:_________
 Uncontrolled Copy of Finished product specification attached*:_____________
*Current version shall be followed
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 DRY MIXING:
As specified in the BMR, dry mix the material for 10 minutes. Withdraw about 20 gm of sample after
10 minutes of dry mixing as specified in BMR, from the centre position of Top, middle and bottom
layer of dry mixed granules in rapid mixer granulator for determination as test given in sample
summary.
DIAGRAM AND SAMPLING LOCATION FOR R.M.G :

T1 = Top left T2 = Top middle T3 = Top right

M1 = Middle left M2 = Middle centre M3 = Middle right
B1 = Bottom left B2 = Bottom middle B3 = Bottom right
B4 = Discharge chute
 PHARMA DEVILS
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PROCESS VALIDATION PROTOCOL OF UN-COATED TABLET

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 DRYING:
Dry the granules at inlet temperature defined in BMR. Withdraw the composite sample during drying to
till the end of drying to get the desired LOD and after the completion of drying withdraw samples from
seven locations to determine the uniformity of drying in FBD as defined in sample summary.

DIAGRAM OF FLUID BED DRYER BOWL WITH SAMPLING POINTS:

T1 T2

M1 M2

B1 B2

Where,
T1 = Top Left M2 = Middle Right
T2 = Top Right B1 = Bottom Left
M1 = Middle Left B2 = Bottom Right
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 LUBRICATION:

As specified in the BMR, blend the material for 20 minutes for pre-lubrication. Withdraw the samples
equivalent to between 1 – 3 unit dose (395.60 – 1216.80) mg, in duplicate separately from 10 locations
as per defined sampling location; determine the blend uniformity of granules.
As specified in the BMR, blend the material for 03 minutes for lubrication. Withdraw the samples
equivalent to between 1 – 3 unit dose (400.0 – 1230.0) mg, in duplicate separately from 10 locations as
per defined sampling location; determine the blend uniformity of granules.
Withdraw about 50 gm of sample after 03 minutes of blending as specified in BMR, from the centre
position of Top, middle and bottom layer of blend in Bin bender for determination of test given in
sample summary.
DIAGRAM OF BIN BLENDER WITH SAMPLING LOCATIONS:

Top Layer

Middle Layer

Bottom Layer

Side View

Where,
T1 = Top Left M2 = Middle Front
T2 = Top Front M3 = Middle Rear
T3 = Top Rear M4 = Middle Right
T4 = Top Right B1 = Bottom Left
M1 = Middle Left B2 = Bottom Right
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 COMPRESSION:
On release of the lubricated granules by QA, the granules are taken up for compression. During tablet
compression stage, the homogeneous granules are compressed on a tableting machine. To validate the
tableting process for product, the compression machine is run on maximum / minimum hardness,
maximum / minimum speed and on optimum hardness / speed - at initial run, middle run, end of the
run. Samples are collected for analysis as defined in the sample summary. The in-process testing shall
be carried out at regular intervals during the machine run. These validation samples shall be tested as
per the sample summary, to meet the acceptance criteria specified therein.
 PROCEDURE
Appropriately label the sample containers and collect samples as follows:
Set the machine, and adjust the compression parameters. After stabilization of the compression
machine, the parameters mentioned below are checked and recorded in the respective BMR and report.
Parameters of Evaluation
1. Appearance 5. Disintegration Time
2. Hardness 6 Group Weight
3. Thickness 7. Average Weight
4. Friability 8. Uniformity of Weight

After the start of compression operation, set the compression machine -

AT OPTIMUM HARDNESS AND MAXIMUM SPEED:
Set the compression machine at optimum hardness and maximum limit of speed and collect the tablets
as per the sample summary. Maximum speed to be recorded in validation report.
AT OPTIMUM HARDNESS AND MINIMUM SPEED:
Set the compression machine at optimum hardness and minimum limit of speed and collect the tablets
as per the sample summary. Minimum speed to be recorded in validation report.
AT OPTIMUM SPEED AND MAXIMUM HARDNESS:
Set the compression machine at optimum speed and higher limit of hardness range and collect the
tablets as per the sample summary. Target hardness and thickness to be recorded in validation report.
AT OPTIMUM SPEED AND MINIMUM HARDNESS:
Set the compression machine at optimum speed and lower limit of hardness range and collect the
tablets as per the sample summary. Target hardness and thickness to be recorded in validation report.
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OPTIMUM RUN:
Set the compression machine at optimum speed / hardness and collect the tablets as per the sample
summary Optimum speed to be recorded in validation report.
AT INITIAL /FULL HOPPER RUN
MIDDLE RUN
END/HALF HOPPER OF RUN
Collect tablets at regular intervals till the end of the compression cycle as per the Batch Manufacturing
Record and sample summary. Record the sample details in validation report and Batch Manufacturing
Record. About 100 tablets in a container labelled, as ‘POOLED SAMPLE’ shall be collected
throughout the compression operation. The tablet for Inprocess analysis shall be taken from the pooled
sample for Inprocess Product Analysis as per specification.

18.0 DESTRUCTION OF REMAINING VALIDATION SAMPLES:

All remaining samples of the validation batch shall be destroyed as per respective SOP, details to be
recorded in validation report.

19.0 SUMMARY, CONCLUSION AND APPROVAL:

Record the summary of the validation study with special emphasis on physical parameter, chemical
parameter and evaluation of data obtained in validation report. Details of out of specification /
deviation if any should be recorded in validation report. Record the recommendations or suggestions
based on the implementations of the results in validation report. It should include the approval of
quality assurance, quality control and production head.
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20.0 ABBREVIATIONS:
QA : Quality Assurance
QC : Quality Control
OOS : Out of Specification
SOP : Standard Operating Procedure
LOD : Loss on Drying
BMR : Batch Manufacturing Record
MMF : Master Manufacturing Formula
A.R. No. : Analytical Report Number
NLT : Not Less Than
NMT : Not More Than
FBD : Fluid Bed Dryer
RMG : Rapid Mixer Granulator
PVR : Process validation report
ASTM : American Society for Testing and Materials
IRMB : Infra Red Moisture Balance
API : Active Pharmaceutical Ingredient

REVISION CARD

Sr. Reason for Change

PPV No. RPV No.
No. Revision Control No.

1 New -----