Veritas Pharmaceuticals limited Process Validation Analytical Report

Muradpur,Vannara,Mouchak,Gazipur VPL-PVAR-007
Rev. No. 00

VERITAS PHARMACEUTICALS LTD

Muradpur, Vannara, Mouchak, Kaliakoir, Gazipur

Document Title: Process Validation Analytical Report of

Ketofast 10 Tablet
Document Number : VPL-PVAR-007, Revision - 00

Product Name : Ketofast 10 Tablet (Ketorolac Tromethamine USP)

Batch Number :
Batch Size : 41.25 kg (2,75,000)

Prepared by Checked by Agreed by Approved by Date

Signature

Name Md. Shafayat Hossain Md. Tarikul Islam Bossunia H. M. Jahid Murad Md. Moniruzzaman
Sr. Executive, Product Quality Assurance
Designation Asst. Manager, QC Manager, Production
Development Manager

1.0 Qualification and training of personnel

Ketofast 10 Tablet COMPANY PROPRIETARY AND CONFIDENTIAL Page 1 of 20

Veritas Pharmaceuticals limited Process Validation Analytical Report
Muradpur,Vannara,Mouchak,Gazipur VPL-PVAR-007
Rev. No. 00

Signature of Signature of
Name Designation Department
Trainee Trainer

2.0 Calibration and qualification status of equipment and utility system

Batch No. Batch Size:

Last
Identification
Equipment Name qualification Ref. Doc. Remarks
No.
/Calibration date

3.0 Qualification of starting materials

Ketofast 10 Tablet COMPANY PROPRIETARY AND CONFIDENTIAL Page 2 of 20

Veritas Pharmaceuticals limited Process Validation Analytical Report
Muradpur,Vannara,Mouchak,Gazipur VPL-PVAR-007
Rev. No. 00

Name of the
QC Ref. No. Release status Remarks
materials

4.0 Details of reference / working standards

Sl. Strengt Exp. Date/
Name Source Ref. No.
No. h Retest test
01

02

03

04

05

5.1 Manufacturing formula for core tablet

Batch
Batch size 41.25 Kg 275000 Standard B/N.:
Qty
Qty
(Kg/Batch) Weigh Checked by
Ingredients Code No.
by (WH) (PO/QA)
Ketorolac Tromethamine 1111001 2.750*
Microcrystalline Cellulose (Avicel PH 102) 1113005 35.858*
Sodium Starch Glycolate 1119001 2.063
Colloidal Silicon Dioxide (Aerosil 200) 1103001 0.309
Magnesium Stearate 1113002 0.206
Green Lake 1103001 0.064
*The quantity will be calculated based on potency.

Ketofast 10 Tablet COMPANY PROPRIETARY AND CONFIDENTIAL Page 3 of 20

Veritas Pharmaceuticals limited Process Validation Analytical Report
Muradpur,Vannara,Mouchak,Gazipur VPL-PVAR-007
Rev. No. 00

5.2 List of Coating materials

Checked by
Code No. Description of Materials Standard Qty (Kg) Actual Qty Weighted by (WH)
(PO/QA)
1108001 Hydroxy propyl Methyl Cellulose (15cps) 2.550
1113006 Methylene Chloride 25.500
1113007 Methanol 25.500
1116003 Polyethylene Glycol (PEG-6000) 0.284
1120001 Titanium Dioxide 0.070
1120002 Purified Talc 0.378
1117003 Green Lake 0.005

5.3 List of packaging materials

Checked by
Code No. Description of Materials Standard Qty (Kg) Actual Qty Weighted by (WH)
(PO/QA)
120002 Printed Alu Foil for Ketofast 10 Tablet
120010 Alu Bottom foil 228 mm
030005 Leaflet for Ketofast 10 Tablet
040005 Inner Carton for Ketofast 10 Tablet (2X10s)
110001 Hollogram Sticker
060005 Master Carton Size # 1
070026 Master Carton Label for Ketofast 10 Tablet
100001 Gum Tape 2"
100002 Glue

6.0 Process Description

Ketofast 10 Tablet COMPANY PROPRIETARY AND CONFIDENTIAL Page 4 of 20

Veritas Pharmaceuticals limited Process Validation Analytical Report
Muradpur,Vannara,Mouchak,Gazipur VPL-PVAR-007
Rev. No. 00

Follow process as per the BMR of Ketofast 10 Tablet

7.0 Sampling
7.1 Granulation stage (Dry mixing and blending)
Sampling Point Quantity collected Collected by Time Sign Date
Top 20 gm
Middle 20 gm

Bottom 20 gm

7.2 Compression
Sampling Point Quantity collected Collected by Time Sign Date
12 RPM & 3 Ton
100 Tablet
pressure
16 RPM & 3 Ton
100 Tablet
pressure
20 RPM & 3 Ton
100 Tablet
pressure
12 RPM & 4 Ton
100 Tablet
pressure
16 RPM & 4 Ton
100 Tablet
pressure
20 RPM & 4 Ton
100 Tablet
pressure

7.3 Coating
Sampling Point Quantity collected Collected by Time Sign Date
Top 100 Tablet
Middle 100 Tablet

Bottom 100 Tablet

7.4 Blistering

Ketofast 10 Tablet COMPANY PROPRIETARY AND CONFIDENTIAL Page 5 of 20

Veritas Pharmaceuticals limited Process Validation Analytical Report
Muradpur,Vannara,Mouchak,Gazipur VPL-PVAR-007
Rev. No. 00

Sampling Point Quantity collected Collected by Time Sign Date

Start 100 Tablet
Middle 100 Tablet
End 100 Tablet
7.5 Finish Product
Sampling Point Quantity collected Collected by Time Sign Date
Start of Operation 100 Tablet
Middle of Operation 100 Tablet
End of Operation 100 Tablet
8.0 Analysis
8.1 Granulation
8.1.1 After 30 minutes mixing Analytical method Ref. No.:
Testing
Test Acceptance
plan/sample Sample ID No. Result Range Pass/fail Remarks
parameters criteria
preparation plan
Top-1
Top
Top-2
Loss on Carry out tests on
Middle-1 Not more than
drying/Wate each sample ( 6 Middle
Middle-2 3.5%
r content samples)
Bottom-1
Bottom
Bottom-2
Top-1
Top 9.50mg
Top-2
Carry out tests on 10.50mg (95.0%
Middle-1
Assay each sample ( 6 Middle to 105.0% of the
Middle-2
samples) label claim)
Bottom-1 RSD: NMT 3%
Bottom
Bottom-2
Must be positive
Identificatio
for Ketorolac
n
Tromethamine
Done by (Sign & Date): ___________________ Checked by (Sign & Date): _____________
8.1.2 If needed extra 5 minutes mixing

Ketofast 10 Tablet COMPANY PROPRIETARY AND CONFIDENTIAL Page 6 of 20

Veritas Pharmaceuticals limited Process Validation Analytical Report
Muradpur,Vannara,Mouchak,Gazipur VPL-PVAR-007
Rev. No. 00

Testing plan/sample Acceptance

Test parameters Sample ID No. Result Range Pass/fail Remarks
preparation plan criteria
Top-1
Top
Top-2
Loss on Carry out tests on
Middle-1 Not more than
drying/Water each sample ( 6 Middle
Middle-2 3.5%
content samples)
Bottom-1
Bottom
Bottom-2
Top-1 9.50mg
Top
Top-2 10.50mg
Carry out tests on
Middle-1 (95.0% to
Assay each sample ( 6 Middle
Middle-2 105.0% of the
samples)
Bottom-1 label claim)
Bottom RSD: NMT 3%
Bottom-2
Must be
positive for
Identification
Ketorolac
Tromethamine

Done by (Sign & Date): ___________________ Checked by (Sign & Date): _____________

8.2 COMPRESSION STAGE

Ketofast 10 Tablet COMPANY PROPRIETARY AND CONFIDENTIAL Page 7 of 20

Veritas Pharmaceuticals limited Process Validation Analytical Report
Muradpur,Vannara,Mouchak,Gazipur VPL-PVAR-007
Rev. No. 00

8.2.1 Compression at 12 RPM & 3 ton pressure

Record
Parameter Specification Minimum Maximum Average Deviation (if any) Remarks
A green colored, round tablet
Appearance with one side engraved V and
other side break line
Average weight 150.0mg (142.50 157.50) mg
Thickness 3.45mm 3.81 mm
Hardness Not less than 5.0 kg
Friability less than 1.0%
Disintegration
Not more than 15 min
Time
NMT 2 of the individual weight
of 20 tablets deviate from
Uniformity of
average weight by more than
weight
7.5% and none deviate by
more than 15%

Done by (Sign & Date): ___________________ Checked by (Sign & Date): _____________

8.2.2 Compression at 16 RPM & 3 ton pressure

Record
Parameter Specification Minimum Maximum Average Deviation (if any) Remarks

Ketofast 10 Tablet COMPANY PROPRIETARY AND CONFIDENTIAL Page 8 of 20

Veritas Pharmaceuticals limited Process Validation Analytical Report
Muradpur,Vannara,Mouchak,Gazipur VPL-PVAR-007
Rev. No. 00

A green colored, round tablet

Appearance with one side engraved V and
other side break line
Average weight 150.0mg (142.50 157.50) mg
Thickness 3.45mm 3.81 mm
Hardness Not less than 5.0 kg
Friability less than 1.0%
Disintegration
Not more than 15 min
Time
NMT 2 of the individual weight
of 20 tablets deviate from
Uniformity of
average weight by more than
weight
7.5% and none deviate by
more than 15%

Done by (Sign & Date): ___________________ Checked by (Sign & Date): _____________

8.2.3 Compression at 20 RPM & 3 ton pressure

Record
Parameter Specification Minimum Maximum Average Deviation (if any) Remarks

Ketofast 10 Tablet COMPANY PROPRIETARY AND CONFIDENTIAL Page 9 of 20

Veritas Pharmaceuticals limited Process Validation Analytical Report
Muradpur,Vannara,Mouchak,Gazipur VPL-PVAR-007
Rev. No. 00

A green colored, round tablet

Appearance with one side engraved V and
other side break line
Average weight 150.0mg (142.50 157.50) mg
Thickness 3.45mm 3.81 mm
Hardness Not less than 5.0 kg
Friability less than 1.0%
Disintegration
Not more than 15 min
Time
NMT 2 of the individual weight
of 20 tablets deviate from
Uniformity of
average weight by more than
weight
7.5% and none deviate by
more than 15%

Done by (Sign & Date): ___________________ Checked by (Sign & Date): _____________

8.2.4 Compression at 12 RPM & 4 ton pressure

Record
Parameter Specification Minimum Maximum Average Deviation (if any) Remarks

Ketofast 10 Tablet COMPANY PROPRIETARY AND CONFIDENTIAL Page 10 of 20

Veritas Pharmaceuticals limited Process Validation Analytical Report
Muradpur,Vannara,Mouchak,Gazipur VPL-PVAR-007
Rev. No. 00

A green colored, round tablet

Appearance with one side engraved V and
other side break line
Average weight 150.0mg (142.50 157.50) mg
Thickness 3.45mm 3.81 mm
Hardness Not less than 5.0 kg
Friability less than 1.0%
Disintegration
Not more than 15 min
Time
NMT 2 of the individual weight
of 20 tablets deviate from
Uniformity of
average weight by more than
weight
7.5% and none deviate by
more than 15%

Done by (Sign & Date): ___________________ Checked by (Sign & Date): _____________

8.2.5 Compression at 16 RPM & 4 ton pressure

Record
Parameter Specification Minimum Maximum Average Deviation (if any) Remarks

Ketofast 10 Tablet COMPANY PROPRIETARY AND CONFIDENTIAL Page 11 of 20

Veritas Pharmaceuticals limited Process Validation Analytical Report
Muradpur,Vannara,Mouchak,Gazipur VPL-PVAR-007
Rev. No. 00

A green colored, round tablet

Appearance with one side engraved V and
other side break line
Average weight 150.0mg (142.50 157.50) mg
Thickness 3.45mm 3.81 mm
Hardness Not less than 5.0 kg
Friability less than 1.0%
Disintegration
Not more than 15 min
Time
NMT 2 of the individual weight
of 20 tablets deviate from
Uniformity of
average weight by more than
weight
7.5% and none deviate by
more than 15%

Done by (Sign & Date): ___________________ Checked by (Sign & Date): _____________

8.2.6 Compression at 20 RPM & 4 ton pressure

Record
Parameter Specification Minimum Maximum Average Deviation (if any) Remarks

Ketofast 10 Tablet COMPANY PROPRIETARY AND CONFIDENTIAL Page 12 of 20

Veritas Pharmaceuticals limited Process Validation Analytical Report
Muradpur,Vannara,Mouchak,Gazipur VPL-PVAR-007
Rev. No. 00

A green colored, round tablet

Appearance with one side engraved V and
other side break line
Average weight 150.0mg (142.50 157.50) mg
Thickness 3.45mm 3.81 mm
Hardness Not less than 5.0 kg
Friability less than 1.0%
Disintegration
Not more than 15 min
Time
NMT 2 of the individual weight
of 20 tablets deviate from
Uniformity of
average weight by more than
weight
7.5% and none deviate by
more than 15%

Done by (Sign & Date): ___________________ Checked by (Sign & Date): _____________

8.3 Justify the machine speed from above result. Run the machine with suitable speed. (Speed: __________rpm & Pressure: __________ton)
Test Testing plan/sample Sample ID Acceptance
Result Average Range Pass/fail Remarks
parameters preparation plan No. criteria
Start Ch.-1

Ketofast 10 Tablet COMPANY PROPRIETARY AND CONFIDENTIAL Page 13 of 20

Veritas Pharmaceuticals limited Process Validation Analytical Report
Muradpur,Vannara,Mouchak,Gazipur VPL-PVAR-007
Rev. No. 00

Ch.-2 A green colored,

Middl Ch.-1 round shaped,
e Ch.-2 one side
Physical Check at each sampling
Ch.-1 engraved with
appearance stage & each channel
V and other
End side break line
Ch.-2
tablet
Ch.-1
Start
Ch.-2
Check at each sampling Middl Ch.-1
Hardness NLT 5 kg
stage & each channel e Ch.-2
Ch.-1
End
Ch.-2
Ch.-1
Start
Ch.-2
3.45mm 3.81
Check at each sampling Middl Ch.-1
Thickness mm (3.63mm
stage & each channel e Ch.-2
5%)
Ch.-1
End
Ch.-2
Channel-1 142.50mg
Average Weight 10 tabs at each
157.50 mg
weight stage from each channel Channel-2
(150.0mg5%)
NMT 2 of the
Channel-1 individual
weight of 20
tablets deviate
Weight Sample from each stage at
from average
variation each channel with 20 tabs.
weight by more
Channel-2 than 7.5% and
none deviate by
more than 15%

Test Testing plan/sample Sample ID Acceptance

Result Average Range Pass/fail Remarks
parameters preparation plan No. criteria
Start Ch.-1

Ketofast 10 Tablet COMPANY PROPRIETARY AND CONFIDENTIAL Page 14 of 20

Veritas Pharmaceuticals limited Process Validation Analytical Report
Muradpur,Vannara,Mouchak,Gazipur VPL-PVAR-007
Rev. No. 00

Ch.-2

Middl Ch.-1
Disintegratio 6 samples from each stage e Not more than 15
Ch.-2
n test at each channel minutes
Ch.-1
End
Ch.-2
9.50mg
Composite of 20 tablets Channel-1 10.50mg (95.0%
Assay from each stage and to 105.0% of the
channel Channel-2 label claim)
RSD: NMT 3%
Individual: 85%
- 115% (10
dosage units).If
one unit is
outside the limit
but within 75%
-125% then test
another 20 units
Select 10 tablets from
individually.
Content composite sample collected
30 units: None
Uniformity from different steps &
should be outside
carryout assay of each unit.
of 75% - 125% of
average content
(30 units) and
maximum one
can be outside
85% -115% of
average content
(30 units).
*Ch.-1: Left hopper; Ch.-2: Right hopper

Done by (Sign & Date): ___________________ Checked by (Sign & Date): _____________

9.0 COATING STAGE

9.1 Compressed tablets are coated in PAM GLATT Coating machine by maintaining following Procedure:
Inlet Pan speed Duration Spray RPM Test parameter Result Checked by Remarks

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Veritas Pharmaceuticals limited Process Validation Analytical Report
Muradpur,Vannara,Mouchak,Gazipur VPL-PVAR-007
Rev. No. 00

Temperature
400c 3 rpm 60 minutes 20 rpm
430c 4 rpm 30 minutes 25 rpm Appear uniform color
450c 5 rpm 30 minutes 30 rpm
500c 6 rpm 60 minutes 35 rpm Appearance, weight gain
weight gain & other
550c 1 rpm 15 minutes Off
parameter as specification

9.2 Coating result Batch No.:

Testing
Test Sample
plan/sample Result Average Range Acceptance criteria Pass/fail Remarks
parameters ID No.
preparation plan
Top A green colored round
shaped film coated
Physical Check at each Middle tablet with one sides
appearance sampling stage
engraved V and other
End side break line
Top
Average Weight 20 tabs at 152.0 mg 168.0 mg
Middle
weight each stage (160.0 mg 5 %)
End
Top
Sample from each
Hardness Middle Not less than 6 kg
stage with 20 tablets
End
Top
Sample from each 3.55 mm 3.93 mm
Thickness Middle
stage with 10 tablets (3.74 mm 5%)
End
Top Not more than two of
Middle the individual weight of
20 tablets deviate from
Weight Sample from each
average weight by
variation stage with 20 tablets
End more than 7.5% and
none deviate by more
than 15%
Top
Disintegratio 6 samples from Not more than 30
Middle
n test each stage minutes
End

Testing
Test Sample
plan/sample Result Average Range Acceptance criteria Pass/fail Remarks
parameters ID No.
preparation plan

Ketofast 10 Tablet COMPANY PROPRIETARY AND CONFIDENTIAL Page 16 of 20

Veritas Pharmaceuticals limited Process Validation Analytical Report
Muradpur,Vannara,Mouchak,Gazipur VPL-PVAR-007
Rev. No. 00

9.50mg 10.50mg
Composite of 20
Composit (95.0% to 105.0% of
Assay tablets from each
e the label claim)
stage
RSD: NMT 3%
5 min.
Composite of 10 min.
sample from each
15 min. Not less than 75%
Dissolution stage (at 5, 10, 15,
30 min. within 45 minutes
30, 45 & 60
minutes) 45 min.
60 min.

Done by (Sign & Date): ___________________ Checked by (Sign & Date): _____________

10.0 Blistering

Verify Embossing on the blister

Batch Number Only Batch Digits

Expiry Date. E MM YY (M= Month, Y= Year)

Embossed statement on the blister

Testing plan/sample
Test Parameter Sample ID No. Result Remarks
preparation plan
Start
Start, Middle & end of
Pocket Formation Middle
operation
End
Start
Start, Middle & end of
Leak test Middle
operation
End

Done by (Sign & Date): ___________________ Checked by (Sign & Date): _____________

11.0 Summary of test result of individual batch Batch No.:

Stage Test Parameter Result Acceptance criteria Pass/Fail Remarks Deviation (if any)
Granulation Loss on drying/Water Not more than 3.5%
content

Ketofast 10 Tablet COMPANY PROPRIETARY AND CONFIDENTIAL Page 17 of 20

Veritas Pharmaceuticals limited Process Validation Analytical Report
Muradpur,Vannara,Mouchak,Gazipur VPL-PVAR-007
Rev. No. 00

9.50mg 10.50mg (95.0% to 105.0% of the label

Assay
claim. RSD: NMT 3%
A green colored, round shaped, one side engraved
Physical appearance
with V and other side break line tablet
Hardness NLT 5 kg
Thickness 3.45mm 3.81 mm (3.63mm 5%)
Compression Average Weight 142.50mg 157.50 mg (150.0mg 5%)
Not more than two of the individual weight of 20
Weight variation tablets deviate from average weight by more than
7.5% and none deviate by more than 15%
Disintegration test Not more than 15 minutes
9.50mg 10.50mg (95.0% to 105.0% of the label
Assay
claim) RSD: NMT 3%
Individual: 85% - 115% (10 dosage units)
If one unit is outside the limit but within 75% -125%
Compression then test another 20 units individually.
Content Uniformity 30 units: None should be outside of 75% - 125%
of average content (30 units) and maximum one
can be outside 85% -115% of average content (30
units).
A green colored round shaped film coated tablet
Physical appearance with one sides engraved V and other side break
line
Average weight 152.0 mg 168.0 mg (160.0 mg 5 %)
Hardness Not less than 6 kg
Thickness 3.55 mm 3.93 mm (3.74 mm 5%)
Coating Not more than two of the individual weight of 20
Weight variation tablets deviate from average weight by more than
7.5% and none deviate by more than 15%
Disintegration test Not more than 30 minutes
9.50mg 10.50mg (95.0% to 105.0% of the label
Assay
claim) RSD: NMT 3%
Dissolution Not less than 75% within 45 minutes
Pocket Formation Must be OK
Blistering
Leak test Must be leak proof.

Stage Test Parameter Result Acceptance criteria Pass/Fail Remarks Deviation (if any)
Finish Physical A green colored round shaped film coated tablet with
Product appearance one sides engraved V and other side break line
Average weight 152.0 mg 168.0 mg (160.0 mg 5 %)

Ketofast 10 Tablet COMPANY PROPRIETARY AND CONFIDENTIAL Page 18 of 20

Veritas Pharmaceuticals limited Process Validation Analytical Report
Muradpur,Vannara,Mouchak,Gazipur VPL-PVAR-007
Rev. No. 00

Hardness Not less than 6 kg

Thickness 3.55 mm 3.93 mm (3.74 mm 5%)
Not more than two of the individual weight of 20
Weight variation tablets deviate from average weight by more than
7.5% and none deviate by more than 15%
Disintegration
Not more than 30 minutes
test
9.50mg 10.50mg (95.0% to 105.0% of the label
Assay
claim) RSD: NMT 3%
Dissolution Not less than 75% within 45 minutes
Individual: 85% - 115% (10 dosage units)
If one unit is outside the limit but within 75% -125%
Content then test another 20 units individually.
Uniformity 30 units: None should be outside of 75% - 125% of
average content (30 units) and maximum one can be
outside 85% -115% of average content (30 units).

Done by (Sign & Date): ___________________ Checked by (Sign & Date): _____________

12. YIELD SUMMARIES

Sl. No. Stage Specification Actual yield Pass/Fail Remarks
01 Granulation 96.0 -101.0%
02 Compression 95.0 101.0%
03 Coating 95.0 101.0%
04 Finish product 95.0 101.0%

Ketofast 10 Tablet COMPANY PROPRIETARY AND CONFIDENTIAL Page 19 of 20

Veritas Pharmaceuticals limited Process Validation Analytical Report
Muradpur,Vannara,Mouchak,Gazipur VPL-PVAR-007
Rev. No. 00

13. Reference documents

1) Raw data
2) Certificate of analysis for Granules, Core, Coated & Finish Product
3) Attachments
4) Analytical note book reference No.
5) Analytical note book No.
14. Deviation

Deviation Type Problem Investigation Conclusion

Analytical

Process

15. Final Approval

CERTIFICATE OF APPROVAL
Product : Ketofast 10 Tablet
Process : Granulation, Compression, Coating & Packing of Ketofast 10 mg
Tablet
Reference : VPL-PVP-007

Prepared by:
Signature:________________
Sr. Executive, Product Development Date :________________

Checked by:
Assistant Manager, Quality Control Signature:________________
Date :________________

Agreed by:
Manager, Production Signature:________________
Date :________________
Approved by:
Quality Assurance Manager Signature:________________
Date :________________

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