VR Aslow 81tab Validation Report

Document # H.L.
X-0403-01
TITLE: Issue # 02
Effective Date 26-07-2019
ASL OW 81 TABL ETS Review Date 26-07-2023
(ASPIRIN) Supersede # 01
Page 1 of 31
ENTERIC COATED
REVIEWED BY:
PREPARED BY: APPROVED BY:
QA Officer Sr. Q.C Manager Sr. Q.A Manager Sr. Production Manager GM
Engineering G.M Quality
Operation
TABLE OF CONTENTS
Section Description PAGE

NO.
1.0 SCOPE 1
2.0 DOCUMENTATION 1
3.0 VALIDATION APPROACH 2
3.1 PROCESS VALIDATION 2-3
3.2 VALIDATION STRATEGY 3
4.0 PRODUCT DESCRIPTION 3
5.0 LIST OF MAJOR EQUIPMENT USED IN MANUFACTURING 4
6.0 PROCESS DETAILS 4
6.1 PROCESS SCALE 4
7.0 PROCESS FLOW DIAGRAM 5-7
7.1 MANUFACTURING PROCESS 7-11
8.0 CRITICAL QUALITY ATTRIBUTES 12-13
9.0 PROCESS PARAMETERS TO BE QUALIFIED 13-15
10.0 MANUFACTURING CONDITION-REQUIREMENTS & 15-30
RESULTS
11.0 PACKAGING 31
11.1 BLISTERING & PACKING 31
12.0 VALIDATION ACCEPTANCE CRITERIA 31
13.0 CONCLUSION 31
1.0 SCOPE: This protocol will document at least the critical steps and parameters of
manufacturing process, i.e. those that may have an impact on the quality of the product.Complete
manufacturing processes, including Drying, Blending, Compression, and Coating processes will be
validated.
2.0 DOCUMENTATION:
All batch documents should be in compliance with standard documents.
i) Mfg. Directions
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Document # H.L.X-0403-01
TITLE: Issue # 02
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ii) Manufacturing Order

iii) Standard Operating Procedure
iv) Standard Control Procedures
v) Standard Test Method
vi) Packaging Order
All of the above stated documents are understood by all responsible persons, as applicable.
All related operating procedures must be in compliance with the product requirement.
3.0 VALIDATION APPROACH:

3.1 Process Validation.
Rationale: Establishing documented evidence with a high degree of assurance, that a specific
process will consistently produce a product meeting its predetermined specifications and
quality characteristics, based on preplanned protocols, following are the pre-requisites: Initially
one to two lots will be manufactured using this batch size and direction, therefore it has been
planned to take this product on concurrent validation with single lot acceptance plan.
 Equipment, production environment and analytical testing methods – already fully

validated.
 appropriately trained personnel and batch manufacturing documentation prepared after
these critical parameters have been identified, and machine settings, component
specifications and environmental conditions have been determined and specified
 Data within the finally agreed parameters.
– from at least three consecutive batches, giving product of the desired quality
may be considered acceptable.
 Same size batches will be considered for validation.

 Commercial batch sizes will be considered.
– Validity of assumptions made should be demonstrated when commercial
production starts.
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 Extensive testing at various stages in the manufacturing process _ including on the final
product and its package.
3.2 VALIDATION STRATEGY:

Focuses on:
 Drying of materials
 Mixing
 Blending
 Slugging
 Compression
 Coating
 Blistering and packing
4.0 PRODUCT DESCRIPTION:

4.1 ACTIVE INGREDIENT:
Each Enteric coated tablet contains: Aspirin = 81.0 mg
INDICATION:
Aspirin is used to reduce myocardial infarction in patients with unstable angina or in
patients who have had a previous myocardial infarction.
5.0 LIST OF MAJOR EQUIPMENTS TO BE USED IN MANUFACTURING:
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Sr.No Equipment Description Asset Number Qualification

. Status
1. Mass Mixer,300 kg 1-01-03-25-0006 Qualified
2. Fitz Mill with 16 mesh screen 1-01-03-28-0001 Qualified
3. Tray Dryer 1-01-03-34-0001 Qualified
4. No.18,20 and 40 mesh Screen - Qualified
5. Tablet Compression Machine,ZP33 1-01-03-48-0002 Qualified
6. Accela Cota 1-01-03-32-0001 Qualified
7. Blister Machine- China 1 1-01-03-02-0003 Qualified
6.0 PROCESS DETAILS:
6.1 PROCESS SCALE
Sr.No. Scale Material Name Drug Code No. Unit of Quantity: 75.00 kg
mg/tab. Measure /500,000 Tablets
1. 82.000 Aspirin (40mesh) RM-API-0130 kg 41.000
2. 62.200 * Avicel 102 RM-XCP-0105 kg 32.580
3. 5.000 * Crosscarmellose Sodium RM-XCP-0125 kg 2.663
4. 0.400 Stearic acid (Powder) RM-XCP-0072 kg 0.200
5. 0.400 Stearic acid (Powder) RM-XCP-0072 kg 0.200
6. - Opadry enteric coating RM-XCP-0191 kg 7.300

system, 94O630008, Orange
7. - Isopropyl Alcohol RM-XCP-0131 kg 75.000
Compliance to Specification of all (new & already in use) codes used will be checked.
I - Verify the material is received from the approved source.

II - Successful completion of shelf life of the product will confirm the validation of the raw materials.
7.0 Process Flow Diagram:
Process Flow Diagram of Aslow 81Tablet

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- AVICEL PH 102 Dry the materials in tray

- CROSSCARMELLOSE dryer at 80-90 C for 8-to 10 Tray Dryer
hrs. Moisture become less
than 2.0 %
All process carried out in controlled Temperature 25 C

humidity and temperature
Humidity less than
40%
Pass the dried and cooled above
- AVICEL PH 102 materials following through mesh 16 Mesh sieve
Add Additional
- CROSSCARMELLOSE 16 and collect in a mixer and mix
Distilled Water (if
- ASPIRIN
required). for 60 minutes
Add the following material in blender

Stearic Acid Sieve 40 mesh
and mix for 5 minutes.
Collect the blended granules in S.S

container and slug 100% using19 m.m 16 mesh screen
Crush the above slug through
punches.
fitz mill using sieve 16 mesh.
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Transfer the materials in to Blender, 300 kg

the blender
Blender, 300 kg
Stearic Acid- Add the following material
Sieved through 40 mesh
through sieve 40 and mix for 5
screen- minutes. Blend for 05 minutes.
Submit sample to Blended granules transfer to Polyethylene lined

Q.C. for analysis Polyethylene lined Plastic plastic Containers
Containers.
Release for Compression
Compression
Compression, Weight /tablet Machine, ZP33
Submit sample to
QC for analysis =150 mg
Mix following items in Distilled

Water:
OPADRY TABCOAT (Orange) Release for Coating Accela Cota 48”
940630008
Mix for 45 minutes and filter

through 100 mesh screen
Coating Application COATING OF TABLETS
Accela Cota 48” 6

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Submit sample to QC BLISTERING

for analysis
China Star Blister

Packing 3 X 10’S
Machine ALU PVC
7.1 MANUFACTURING PROCESS:

Batch No.1: N001 Mfg. started on: 09/01/2019 Mfg. completed on:25/01/2019
Batch No 2:N002 Mfg. started on: 14/02/2019 Mfg. completed on:07/03/2019
Batch No.3: N003 Mfg. started on: 07/2019 Mfg. completed on:07-2019
Step # 1: Dry the following materials in tray dryer at 80 - 90oC for 8 – 10 hours or till the moisture
becomes less than NMT 2.0 %.
AVICEL PH 102 32.580 Kg

-

CROSSCARMELLOSE SODIUM 2.663 Kg
All process must be carried out in controlled humidity and Temperature Area
Limit: Temperatures (25°C ± 2°C) and RH below 40%.
All equipment & utensils used must be completely dried.
Step #02:
If required, pass the dried and cooled materials from Step #1 and the following through sieve # 16,
collect in mixer and mix for 60 minutes.
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AVICEL PH 102 (DRIED) kg
CROSSCARMELLOSE SODIUM (DRIED) kg
ASPIRIN 41.000 kg
Step #03: Then add the following material through sieve # 40 in Blender and blend for 5 minutes.
STEARIC ACID 0.200 Kg
Step #04: Collect the blended granules in S.S. Container and slug 100% by using 19 m.m. punches.
Step #05: Pass the dried granules through 16 mesh screen. Crush through Fitz Mill and after crushing,
the granules collect in Blender.
Step# 06: Then add the following material through sieve # 40 in Blender and blend for 5 minutes.
STEARIC ACID 0.200 Kg
Step # 07: Collect the blended granules in the container with double polythene lined bag and send the
sample to QC for Analysis.
Sr. No. Location Assay (%) Acceptance Criteria

Aspirin
1 Top
2 Middle 76.95 mg/tab – 85.05 mg/tab
3 Bottom 95 – 105 % of L.C
4 composite
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Step # 08: Weigh the granules and record the yield.
Theoretical weight of Granules: 75.0 kg / 500,000 tablets.

Net Weight of Granules: __________ kg
% Yield: __________ %.
Step # 09: COMPRESSION: Check compression of tablets with product specifications:
- Compression Machine: ZP33
- Upper Punch: Round Concave - Lower Punch: Round concave
- Appearance: White round biconvex
- Hardness: 30-60 N - Thickness: 3.0-3.6 m.m.
- Friability: NMT 1%
- Average Weight: 150.0 mg ± 5.0% (142.5 – 157.5 mg)
- Disintegration: NMT 15 min in Water at 37°C.
Check and record weight after completion of compression.
Step # 10: Check actual yield after completion of compression.
Step # 11: COATING SOLUTION PREPARATION: Check mixing of following material in Distilled Water,
and then filtration through mesh # 100.
- OPADRY TABCOAT (ORANGE) 940630008 : 7.300 Kg

- ISOPROPYL ALCOHOL : 75.000 liters
Step # 12: APPLICATION OF COATING SOLUTION:

Equipment: Accela Cota 48”
Check application of Coating solution on core tablets in Coating Pan according to process parameters:
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-No. of spray guns. 03

-Distance between spray guns 6”
-Distance of guns to tablets bed. 8”
-Gun nozzle bore size. 1.5 mm
-Pan Speed. 2 - 10 rpm
-Inlet Air Temp. 50 - 60 oC
-Bed Temp 40-50 oC
-Exhaust Air Temp. 30-40 oC
-Atomizing Pressure. 4-8 bar
-Solution Flow Rate 40-150 ml/min.
Step #13: Apply coating solution using the following conditions, with maintaining agitation through out
Spraying.
- Pan Speed. 02 - 10rpm
-Inlet Air Temp. 50- 60 oC
-Bed Temp 45 - 50 oC
-Exhaust Air Temperature 30 - 40 oC
-Solution Flow Rate 40-150 ml/min
Step # 14: APPLICATION OF COATING SOLUTION:

Equipment: Accela Cota 48”
Check application of Coating solution on core tablets in Coating Pan according to process parameters:
-No. of spray guns. 03
-Distance between spray guns 6”
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-Distance of guns to tablets bed. 8”

-Gun nozzle bore size. 1.5 mm
-Pan Speed. 2 - 8 rpm
-Inlet Air Temp. 50 - 60 oC
-Bed Temp 45-50 oC
-Exhaust Air Temp. 30-40 oC
-Solution Flow Rate 40-150 ml/min.
Step #15: Take 10 samples of 20 tablets each, at 10 equally distributed time intervals to cover whole
coating process and record. On completion of the coating run, take samples of coated tablets for testing.
Step # 16: Check actual yield after completion of coating.
8.0 CRITICAL QUALITY ATTRIBUTES

Critical Quality Attribute How Measured Rationale/Reference
Blending:
Assay : Collect sample after blending As Per STM

Aspirin process. (Top Mid and Bottom
of the blend)
Compression:
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Physical characteristics (Shape, 20 tablets collected each from As Per STM

Color, Marking) the beginning, middle and end
of Compression Process.
Weight variation In‐process control chart used As Per STM
to monitor weight variation.
Hardness , Thickness & In‐process control chart used As Per STM
Friability of core tablets to monitor Hardness, Thickness
and Friability.
Assay : 20 tablets collected each from As Per STM
Aspirin the beginning, middle and end
of compression process.
Disintegration Time 18 tablets collected each from As Per STM
the beginning,
middle and end of compression
process
Coating:
Physical characteristics 20 coated tablets (composite As Per STM

(Appearance, Color, Shape, sample) collected from each
Markings) coating run.
Inspection of Attributes 200 coated tablets (composite As Per STM
sample) collected from each
coating run.
Disintegration Time 18 tablets (composite sample) As Per STM
collected from
each coating run.
Coating process & parameters Coating process and As Per STM
parameters noted during
each coating run
Assay : 20 tablets collected each from As Per STM
Aspirin the composite sample.
9.0 PROCESS PARAMETERS TO BE QUALIFIED:

Process Parameter Process Operating How Monitored Rationale/
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Range Reference
DRYING:
Drying of 80-90 C for 8- 10 hrs Drying of materials As per Mfg. Direction

-AVICEL PH 102 moisture becomes
CROSSCARMELLOS less than 2.0%
SODIUM
In a tray dryer.
Pass the dried granules 16 Mesh Sieve Uniform mixing of As per process
through 16 mesh screen and granules. requirement
add the following materials
and mix for 60 minutes
transfer in blender.
AVICEL PH 102
CROSSCARMELLOS
SODIUM
ASPIRIN
Blending :
Add the following Pass through 40 mesh & Uniform size material As per Mfg. Direction
material through sieve add it to blender .Blend for and blending time of
40. 05 minutes. 05 minutes.
Stearic Acid
Slugging : Slugging of whole batch. As per Mfg. Direction

100 % Slug using 19
mm punches
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Pass the dried granules 16 mesh size .Transfer the Uniform size material As per Mfg. Direction
through 16 mesh material into blender.
screen. Crush through
Fitz Mill.
Add the following Pass through 40 mesh & Uniform size bending As per Mfg. Direction
material through sieve # add it to blender .Blend for and blending time of
40 in Blender and blend 05 minutes. 05 minutes.
for 5 minutes
Stearic acid
Compression:
Compression of tablets Wt. /tablet =150.0 mg,+, - In-process inspection As per Mfg. Direction
5.0% at a given time
interval.
Coating :
Coating solution Mix for 45 minutes and then Uniform mixing of As per Mfg. Direction
Preparation: pass through 100 mesh coating solution.
Dissolve : sieve.
- OPADRY
TABCOAT(ORANGE)
940630008 in
-ISOPROPYL ALCOHOL
Coating Application : 2-10 rpm Check actual rpm As per Mfg. Direction
Pan speed used
Inlet air temperature 50-60 C Check actual As per Mfg. Direction
temperature used.
Atomizing Pressure 4 - 8 Bar Check actual As per Mfg. Direction
pressure used
Exhaust temperature 30 - 40oC Check actual As per Mfg. Direction
during Coating temperature used
Solution Flow Rate. 40-150 ml/min Check actual Flow As per Mfg. Direction
rate used
10.0 MANUFACTURING CONDITION-REQUIREMENTS & RESULTS
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S.No. Section
10.1 Blending :
 Blend uniformity of lubricated bulk granules
10.2 Compression:
 Physical Characteristics of core tablets.
10.3 Compression:
 Average weight and Weight Variation, %Friability, Hardness, Thickness,
Disintegration Test of core tablets.
10.4 Assay of Aspirin on Core Tablet (% of L.C. per Tab.)
10.5 Coating:
 Physical characteristics of coated tablets.
10.6 Coating:
 Inspection of attributes for coated tablets
10.7 Disintegration Test:
 Disintegration Time of coated tablets
10.8 Assay & Dissolution of Aspirin on Coated Tablet (% of L.C. per Tab.).
10.1 Blend uniformity of lubricated bulk granules:
Sr. Section
No.
10.1. Blending :
 Blend uniformity of lubricated bulk granules
A. OBJECTIVE :
To verify the blend uniformity of the lubricated bulk granules.
B. TEST AND SAMPLING PLAN :

Take sample of the blender after blending process.
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C. TEST METHOD:
Take bulk powder quantity according to tablet weight and proceeded as per
Test method: HP/QC/SPFG-139
D. ACCEPTANCE CRITERIA:
Assay of Aspirin 76.95 mg/tab – 85.05mg/tab,
95 – 105% of L.C.
E. DATA :
Product: Aslow 81 tablets
Batch Nos. ASSAY mg/150mg Acceptance

Criteria
76.95 mg/tab –
85.05mg/tab,
95 – 105% of L.C.
Top Middle Bottom Comp.sample. Avg

N001 80.980 81.009 81.154 81.652 81.198
N002 80.746 80.44 80.666 80.764 80.654
N003 81.524 81.250 81.666 81.544 81.496
Conclusion: Results found within specification.
Performed S.M. Shahid
By:
Verified By: Shakeel Ahmed
F. CALIBRATION
Test Instrument Instrument I.D. Calibration Status

Description Number
Spectrophotometer Q.C.D.-035 Calibrated
10.2 Physical Characteristics of core Tablet:

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Sr. Section
No.
10.2 Compression:
 Physical Characteristics of core tablets.
A. OBJECTIVE :
To verify physical characteristics of core tablets during compression process

Collected 20 tablets each sample from the beginning, middle and end of compression
Process.
C. TEST METHOD:
As per Std. Test Method: HP/QC/SPFG-139
Appearance: White round biconvex tablet
Color: White.
Shape: Round Biconvex

E. DATA :
Aslow 81Tablet Batch No. N001
No. Of Top Middle Bottom

Sample
Appearance Color Shape Appearance Color Shape Appearance Color Shape
20 tablets White White Round White White Round White White Round
Round Biconvex Round Biconvex Round Biconvex
Biconvex Biconvex Biconvex
core tablets core tablets core tablets
Conclusion Results Comply acceptance criteria
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Performed Mehmeen
By
Verified By Aamir Zaidi

No. Of Beginning Middle End
Sample
Performed Mehmeen
By
No. Of Beginning Middle End

Sample
Performed Mehmeen
By
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F. CALIBRATION:

Description Number
N/A N/A N/A
10.3 Compression:
Sr. Section
No.
Compression:
10.3  Average weight , Weight Variation of core tablets, % Friability
,Hardness ,Thickness, Disintegration Time
A. OBJECTIVE :
To verify Average weight and Weight Variation, % Friability, Hardness, Thickness &
disintegration time of core tablets.

Collected 100 tablets each sample from the beginning, middle and end of compression
Process.
C. TEST METHOD:
-Theoretical Weight: 150 mg per tablet core.

Variation from theoretical weight: The average weight shall not differ from the theoretical
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Weight by more than 5%.

Weight Variation: 145.20 mg /tab. – 157.50 mg/tab.
-% Friability: NMT 1% -Hardness: 30N – 60 N
-Thickness: 3.0mm. – 3.6 mm. -Disintegration Time: N.M.T. 15 minutes.
E. DATA
Product: Aslow 81Tablet Batch No. N001
Sample Weigh Individual Hardness Thicknes %Friability Disintegration

(Start of t/10 weight per (N) s (m.m.) Test
compression) tablets tablet
(gm)
1 1.50 154 60 3.35 0.1% 40 sec
2 1.52 150 57 3.40
3 1.49 147 59 3.39
4 147 60 3.38
5 145 54 3.34
6 158 52 3.30
7 140 55 3.49
8 149 59 3.45
9 147 57 3.41
10 155 60 3.36
Conclusion: Results meet acceptance Criteria.
Performed By: Rashid Mukhtar / S.M. Shahid
Verified By: Aamir Zaidi / Shakeel Ahmed

Sample Weight/10 Individual Hardness Thickness %Friability Disintegration
tablets weight per (N) (m.m.) Test
(gm) tablet
1 1.50 145 55 3.30 0.4% 01 minute
2 1.51 146 54 3.41
3 1.49 148 52 3.49
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4 148 59 3.47
5 147 57 3.39
6 152 56 3.45
7 150 58 3.29
8 149 54 3.51
9 151 52 3.39
10 157 53 3.32
Performed By: Mehmeen/S.M. Shahid

Sample Weigh Individual Hardness Thicknes %Friability Disintegration
(Start of t/10 weight per (N) s (m.m.) Test
compression) tablets tablet
(gm)
1 1.53 149 59 3.40 0.3% 30 sec
2 1.51 153 60 3.39
3 1.51 154 55 3.50
4 152 54 3.47
5 153 49 3.56
6 147 57 3.51
7 149 51 3.50
8 150 52 3.49
9 151 48 3.41
10 153 56 3.55
Performed By: Mehmeen / S.M. Shahid
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F. CALIBRATION:

Description Number
Hardness Tester: Q.C.D.-031 Calibrated
Friabilator Q.C.D.-011 Calibrated
D.T. Apparatus Q.C.D.-010 Calibrated
10.4 Assay of Aspirin on Core Tablet (% of L.C. per Tab.)
Sr. Section
No.
10.4  Assay of Aspirin on Core Tablet (% of L.C. per Tab.)
A. OBJECTIVE :
To verify the Assay of Aspirin on core Tablet.

For Assay, 20 tablets were collected each from the beginning, middle and end of the
compression process.
C. TEST METHOD:
Carry out the test as per current method: HP/QC/SPFG-139
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Assay of Aspirin 76.95mg/tablet – 85.05mg/tablet, 95 – 105% of L.C
E. DATA : Product: Aslow 81Tablet
Batch Nos. Top(mg/tab) Mid(mg/tab) Bot(mg/tab) Composite(mg/tab) Acceptance

95-105% of L.C 95-105% of L.C 95-105%of 95-105% of L.C Criteria
L.C
N001 81.08mg/tab 80.73mg/tab 81.56mg/tab 81.36mg/tab 76.95mg

100.09% 99.667% 100.69% 100.44% -85.05mg
N002 80.66mg/tab 80.07mg/tab 80.50mg/tab 81.71mg/tab per tab
99.58% 98.85% 99.38% 100.88% 95-105 % of
N003 80.994mg/tab 80.565mg/tab 80.97mg/tab 80.656mg/tab L.C
99.99% 99.46% 99.96% 99.58%
Conclusio
n
By:
Verified by Shakeel Ahmed
F. CALIBRATION:
Description Number
Spectrophotometer. Q.C.D.-035 Calibrated
10.5 Coating:
Sr. Section
No.
10.5 Coating:
 Physical characteristics of coated tablets.
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A. OBJECTIVE :
To verify the physical characteristics of coated tablets.

20 coated tablets (composite sample) collected from each coating run.
C. TEST METHOD:
Appearance: Round, orange, Biconvex enteric coated Tablet.
Coating : Smooth coating
Color : Orange
E. DATA :
Product: Aslow 81Tablet
Sample Appearance Coating Color

20 Tablets Round, orange, Smooth coating Orange
Batch N001 Biconvex enteric
coated Tablet.

coated Tablet.
coated Tablet.
Conclusion: Comply with specifications.
Performed By: Mehmeen

Verified By: Aamir Zaidi
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F. CALIBRATION:

Description Number
N/A N/A N/A
10.6 Coating
Sr. Section
No.
10.6 Coating:
 Inspection of attributes for coated tablets
A. OBJECTIVE :
To inspect the attributes of coated tablets.
200 coated tablets (composite sample) were collected from each coating run.
C. TEST METHOD:
As per Std. Test Method.
Defects Acceptance Limit

1. Critical 0.0%
 Odd tablets (wrong product)
 Thin or thick tablets
 Foreign matter
2. Major 1.0%
 Cracked or broken tablets
 Color variation
 Chipped coating
 Capped
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 Sticking together
3. Minor 2.5%
 Small specks
 Bumpy rough coating
 Chipped coating (small chip)
E.DATA :
Product: Aslow 81Tablet
Batch Nos. Sampl Sample Sample Conclusion

e Defect Defect
Defect Major Minor
Critical
N001 0.0% 0.13% 0.22% Meet acceptance
Limit
N002 0.0% 0.16% 0.28%
N003 0.0% 0.12% 0.25%

Performed by: Mehmeen
Verified by: Aamir Zaidi
F. CALIBRATION:

Description Number
N/A N/A N/A
10.7 Disintegration test
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Sr. Section
No.
10.7 Disintegration Test :
 Disintegration Time of coated tablets
A. OBJECTIVE :
To verify the Disintegration Time of coated tablets.

Collected 18 coated tablets composite sample after completion of coating from different
locations of the coating pan.
C. TEST METHOD:
As per Test Method: HP/QC/SPFG-139
D. ACCEPTANCE CRITERIA
In 0.1N HCl : Tablets should not shows sign of crack in first 2 hrs.
In pH 6.8 Phosphate Buffer :NMT 1 Hour
E. DATA: Product: Aslow 81Tablet
Batch Nos. Disintegration Time in 0.1N In pH 6.8 Phosphate Acceptance Criteria

HCl Buffer
(Coated Tablets)
Tablets should not shows NMT 1 Hour
sign of crack in first 2 hrs
N001 Complies 27 minutes
Conclusion: Results meet acceptance criteria

Performed By: S.M. Shahid
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F. CALIBRATION:

Description Number
Disintegration Test Q.C.D.- 010 Calibrated
Apparatus
10.8 Assay & Dissolution test of Coated Tablets:
Sr. Section
No.
10.8  Assay of Aspirin on Coated Tablet (% of L.C. per Tab.)
 Dissolution
A. OBJECTIVE :
To verify the Assay of Aspirin on coated tablets.

Collected 24 coated tablets composite sample after completion of coating from different
locations of the coating pan.
C. TEST METHOD:
As per Test Method: HP/QC/SPFG-139
Assay of Aspirin : 76.95mg/tablet – 85.05mg/tablet ,
95%– 105% of L.C
E. DATA:
Product: Aslow 81Tablet (Assay)
28
TITLE: Issue # 02
Page 29 of 31
ENTERIC COATED
REVIEWED BY:
Operation
Batch Nos. Assay –Coated tablets Acceptance Criteria

N001 81.6520mg/tablet
100.80% 76.95mg/tablet –
N002 80.66mg/tablet 85.05mg/tablet , 95 – 105% of
99.58% L.C
N003 80.99mg/tab
99.98%
By:
(Dissolution)
Batch Nos. %Dissolved in %Dissolved in Acceptance Criteria

0.1 N HCl pH 6.8
(1) Phosphate buffer
(2)
N001 6.89% 97.20% 1- NMT 10% of
Label Claim.
N002 5.63% 93.65%
2- NLT 75% of
N003 5.78% 95.18% Label Claim

By:
29
TITLE: Issue # 02
Page 30 of 31
ENTERIC COATED
REVIEWED BY:
Operation
F. CALIBRATION:

Description Number
H.P.L.C. Q.C.D.-033 Calibrated
Dissolution Q.C.D.-033
11.0 PACKAGING:
11.1 BLISTERING AND PACKING:
Tablets are blistered by using tablet blistering machine in Aluminium Foil Printed, Aslow 81
Tablets, 152 mm, 20 µ and PVC BLUE Foil 152mm and then packed in printed cartons as
3 x 10’s pack.
Batch Nos Name of Equipment No. Blister Sealing

Blistering Checks
Machine
N001 China star blister NA Satisfactory
N002 machine Satisfactory
N003 Satisfactory
30
TITLE: Issue # 02
Page 31 of 31
ENTERIC COATED
REVIEWED BY:
Operation
12.0 ACCEPTANCE CRITERIA:

Each validation batch of Aslow 81 tablets will be released for marketing on the basis of
acceptance criteria of product specification limits.
13.0 CONCLUSION:
 Process validation of three batches of Aslow 81 tablets (Batch No.N001, N002, &
N003), Product Code No.0403 was performed as per Concurrent validation approach
with single lot acceptance criteria.
 All Physical and Chemical tests were performed and were found within specification
limit.
 Assay was performed on all of three batches as per approved test method and results
were found within specification limit.
31

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Section Description PAGE

ii) Manufacturing Order

3.0 VALIDATION APPROACH:

 Equipment, production environment and analytical testing methods – already fully

 Same size batches will be considered for validation.

3.2 VALIDATION STRATEGY:

4.0 PRODUCT DESCRIPTION:

Each Enteric coated tablet contains: Aspirin = 81.0 mg

5.0 LIST OF MAJOR EQUIPMENTS TO BE USED IN MANUFACTURING:

Sr.No Equipment Description Asset Number Qualification

2. 62.200 * Avicel 102 RM-XCP-0105 kg 32.580

3. 5.000 * Crosscarmellose Sodium RM-XCP-0125 kg 2.663

4. 0.400 Stearic acid (Powder) RM-XCP-0072 kg 0.200

5. 0.400 Stearic acid (Powder) RM-XCP-0072 kg 0.200

6. - Opadry enteric coating RM-XCP-0191 kg 7.300

I - Verify the material is received from the approved source.

7.0 Process Flow Diagram:

Process Flow Diagram of Aslow 81Tablet

- AVICEL PH 102 Dry the materials in tray

All process carried out in controlled Temperature 25 C

Add the following material in blender

Collect the blended granules in S.S

Transfer the materials in to Blender, 300 kg

Submit sample to Blended granules transfer to Polyethylene lined

Release for Compression

Mix following items in Distilled

Mix for 45 minutes and filter

Coating Application COATING OF TABLETS

Accela Cota 48” 6

Submit sample to QC BLISTERING

China Star Blister

7.1 MANUFACTURING PROCESS:

Batch No 2:N002 Mfg. started on: 14/02/2019 Mfg. completed on:07/03/2019

AVICEL PH 102 32.580 Kg

AVICEL PH 102 (DRIED) kg

CROSSCARMELLOSE SODIUM (DRIED) kg

STEARIC ACID 0.200 Kg

STEARIC ACID 0.200 Kg

Sr. No. Location Assay (%) Acceptance Criteria

Step # 08: Weigh the granules and record the yield.

Theoretical weight of Granules: 75.0 kg / 500,000 tablets.

- Compression Machine: ZP33

- Upper Punch: Round Concave - Lower Punch: Round concave

- Appearance: White round biconvex

- Hardness: 30-60 N - Thickness: 3.0-3.6 m.m.

- Average Weight: 150.0 mg ± 5.0% (142.5 – 157.5 mg)

- Disintegration: NMT 15 min in Water at 37°C.

Check and record weight after completion of compression.

Step # 10: Check actual yield after completion of compression.

- OPADRY TABCOAT (ORANGE) 940630008 : 7.300 Kg

Step # 12: APPLICATION OF COATING SOLUTION:

-No. of spray guns. 03

Step # 14: APPLICATION OF COATING SOLUTION:

-Distance of guns to tablets bed. 8”

8.0 CRITICAL QUALITY ATTRIBUTES

Assay : Collect sample after blending As Per STM

Physical characteristics (Shape, 20 tablets collected each from As Per STM

Physical characteristics 20 coated tablets (composite As Per STM

9.0 PROCESS PARAMETERS TO BE QUALIFIED:

Drying of 80-90 C for 8- 10 hrs Drying of materials As per Mfg. Direction

Slugging : Slugging of whole batch. As per Mfg. Direction

10.0 MANUFACTURING CONDITION-REQUIREMENTS & RESULTS