MASTER FORMULA RECORD
Generic Name: Ofloxacin
& Ornidazole Tablets IP
1.0 PRODUCT
DETAILS:
|
Shelf life: 24 Months |
Batch Size: 1.0
Lac |
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Brand Name of
Product: |
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Generic Name of
Product: Ofloxacin
& Ornidazole Tablets IP |
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|
Label
Claim |
Each film coated tablet contains; Ofloxacin IP………….……...200 mg Ornidazole…………………...500mg Excipients…………………..……q.s. Colour :
Sunset Yellow FCF, Tartrazine & Titanium Dioxide IP |
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Market |
Domestic/Export/ Institutional
Supply |
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Marketed By |
|
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Dosage Form |
Oral dosage form - Tablets |
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|
Description |
Orange
coloured, Elongated Shaped, Biconvex, film coated tablets having scored line
on one side and plain other side. |
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|
Length &
Width |
15.8X 5.8 ± 0.2 mm |
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|
Average weight of
tablets |
Uncoated
tablets: |
850
mg |
Coated Tablets: |
866 mg |
|
|
Mfg. Lic. No.: |
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2.0 TABLE
OF CONTENT:
|
Sr. No. |
INDEX |
Page No. |
|
1. |
Product Details |
2 |
|
2. |
Table of Content |
3 |
|
3. |
Flow-chart for
formulation |
4 |
|
4. |
Bill of raw
Material |
5-8 |
|
5. |
List of equipment |
9 |
|
6. |
Manufacturing
Process |
10-14 |
|
7. |
Coating Process |
15 |
|
8. |
Batch
Reconciliation |
16 |
|
9. |
Revision history |
16 |
3.0 FLOW-CHART
FOR FORMULATION
4.0 BILL
OF MATERIAL (For
1,00,000 Tabs)
|
Sr. No. |
Ingredients |
Specification |
Quantity
Mg Per Tablet |
Overages % |
Batch Quantity In Kg (1.0 Lac) |
|
|
Active Ingredients |
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|
1.
|
Ofloxacin |
IP |
200 |
** |
20.000 |
|
|
2.
|
Ornidazole |
IP |
500 |
** |
50.000 |
|
|
Total Weight |
|
70.000 |
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|
Inactive Ingredients |
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|
1. |
Starch |
IP |
--- |
--- |
7.000 |
|
|
2. |
MCCP (Micro Crystalline Cellulose) |
IP |
--- |
--- |
2.000 |
|
|
3. |
Starch for Paste |
IP |
--- |
--- |
1.500 |
|
|
4. |
Gelatin |
IP |
--- |
--- |
0.600 |
|
|
5. |
Aerosil (Colloidal silicon dioxide) |
IP |
--- |
--- |
0.750 |
|
|
6. |
Talc Cross Carmellose sodium |
IP |
--- |
--- |
0.750 |
|
|
7. |
Cross Povidone XL-10 USP28/NF23 |
IP |
--- |
--- |
0.800 |
|
|
8. |
Magnesium Stearate |
IP |
--- |
--- |
1.000 |
|
|
9. |
Purified Water |
IP |
--- |
--- |
15.000 |
|
|
10. |
Talc |
IP |
--- |
--- |
2.000 |
|
|
11. |
Sodium Starch Glycolate |
IP |
--- |
--- |
0.750 |
|
|
12. |
HPMC E15 CPS(Hydroxy Propyl Methyl
Cellulose) |
IP |
--- |
--- |
1.000 |
|
|
13. |
Colour Titanium dioxide |
IP |
--- |
--- |
0.100 |
|
|
14. |
Colour Lake Sunset Yellow |
IP |
--- |
--- |
0.300 |
|
|
15. |
Talc |
IP |
--- |
--- |
2.500 |
|
|
Total Weight |
850 |
36.05 |
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**
Note: API Overages
depends upon Raw Material Assay.
(API-I) ACTUAL QUANTITY
OF OFLOXACIN IS TO BE TAKEN AS PER THE FORMULA GIVEN:
A. Calculation
for single AR No.:
AR.
No.________________, Assay on dried basis: __________, LOD: ________
Standard QTY.X 100 X 100
Quantity
of Ofloxacin to be dispensed =----------------------------------------------
= -------------------------------------
=
Assay on as dried basis X (100-LOD)
B. Calculation
for Multiple AR No.:
1st
AR No.: AR. No.________________, Assay on dried basis: __________ , LOD:
________
Q1 (Available Quantity) X Assay on as dried basis X
(100-LOD)
A1
= ----------------------------------------------
----------------------------------- =
----------------------------------------- =
100 X 100
2nd AR No.:
AR. No.________________, Assay
on dried basis: __________ , LOD: ________
Q2 (Available Quantity) X Assay on as dried basis X
(100-LOD)
A2
= ----------------------------------------------
----------------------------------- =
----------------------------------------- =
100 X 100
Final
AR No.: AR. No.________________, Assay on dried basis: __________, LOD:
________
Q3 (Std Qty-A1-A2) X 100 X100
A3
= ---------------------------------------------- ----------------- = ----------------------------------------- =
Assay on as dried basis X (100-LOD)
Total
Qty of API to be dispensed (A4) = A3+Q2+Q1) = ______________
Quantity of Starch is to be adjusted based on quantities of the above Active.
Quantity of Starch in kg = Standard Qty
of Starch – (A4 - Slandered Qty of API) =
(API-II) ACTUAL QUANTITY
OF ORNIDAZOLE IS TO BE TAKEN AS PER THE FORMULA GIVEN:
A. Calculation
for single AR No.:
AR.
No.________________, Assay on dried basis: __________, LOD: ________
Standard QTY.X 100 X 100
Quantity
of Ornidazole to be dispensed =----------------------------------------------
= -------------------------------------
=
Assay on as dried basis X (100-LOD)
B. Calculation
for Multiple AR No.:
1st
AR No.: AR. No.________________, Assay on dried basis: __________ , LOD:
________
Q1 (Available Quantity) X Assay on as dried basis X
(100-LOD)
A1
= ----------------------------------------------
----------------------------------- =
----------------------------------------- =
100 X 100
2nd AR No.:
AR. No.________________, Assay
on dried basis: __________ , LOD: ________
Q2 (Available Quantity) X Assay on as dried basis X
(100-LOD)
A2
= ----------------------------------------------
----------------------------------- =
----------------------------------------- =
100 X 100
Final
AR No.: AR. No.________________, Assay on dried basis: __________, LOD:
________
Q3 (Std Qty-A1-A2) X 100 X100
A3
= ---------------------------------------------- ----------------- = ----------------------------------------- =
Assay on as dried basis X (100-LOD)
Total
Qty of API to be dispensed (A4) = A3+Q2+Q1) =
______________
5.0 LIST
OF EQUIPMENT
|
Sr.
No. |
Name
of Equipment |
Equipment
ID No. |
|
1.
|
Vibro
Sifter |
PRL/TAB/EQ/002 |
|
2.
|
Rapid
mixer granulator (RMG) |
PRL/TAB/EQ/001 |
|
3.
|
Paste
kettle |
PRL/TAB/EQ/005 |
|
4.
|
Fluid
bed dryer (FBD) |
PRL/TAB/EQ/011 |
|
5.
|
FBD
Bag |
PRL/TAB/EQ/005 |
|
6.
|
Multi-mill
|
PRL/TAB/EQ/009 |
|
7.
|
Octagonal
blender |
PRL/TAB/EQ/004 |
|
8.
|
Weighing
Balance 300
KG |
PRL/TAB/IN/002 |
|
9.
|
SS
scoop |
PRL/TAB/EQ/008 |
|
10.
|
Compression
Machine (Forced
Feeder machine) |
PRL/TAB/EQ/006 |
|
11.
|
Disintegration
Tester |
PRL/TAB/DT/001 |
|
12.
|
Friability
Apparatus |
PRL/TAB/FA/001 |
|
13.
|
Vernier
caliper |
PRL/TAB/VC/001 |
|
14.
|
Hardness
Tester |
PRL/TAB/HT/001 |
|
15.
|
Weighing
Balance 300 gm |
PRL/TAB/IN/001 |
6.0 MANUFACTURING
PROCESS:
|
Step No. |
Manufacturing Instruction |
|
6.1 |
Binder Preparation |
|
|
Stap-1 Take Purified water in 15 Kg
in paste kettle and Heat up to 90°C now add Gelatin (0.600 Kg). Stap-2 Take Purified water 5.0 Kg in
SS container and add Starch (1.500 kg) with stirring for 5
minutes. Stap-3 Then Mixing Step-2
in Step-1 |
|
6.2 |
Dry Mixing |
|
|
Take
sifted material for dry mixing and mix all the material with slow speed of
impeller/chopper Off for 10.0 minutes Ofloxacin__________20.000___________Kg Ornidazole__________50.000___________Kg Starch__________7.000___________Kg Sodium
Starch Glycolate __________0.375___________Kg Aerosil
(COLLAIDAL SILICON DIOXIDE)_____0.375____Kg MCCP
(Micro Crystalline Cellulose) __________2.000___________Kg |
|
Impeller
Speed (Slow/Fast): __ Slow___ then
__Fast__ Chopper Speed(Off):__Off___
Then___ Slow |
|
|
6.3 |
Wet granulation |
|
6.3.1 |
Star
RMG at impeller Slow speed and add binder to dry mixed material with fast
impeller and slow chopper speed. Binder addition time shall be 1 to 3
minutes. Continue the process for 15 minutes after complete addition of
binder. Add additional purified water if required |
|
Binder
addition time_______ min. (Limit: About 1 to 3 min.) Wet
Mixing time___________ min(Limit: 15 min) Total
Time:___________ min |
|
|
6.3.3 |
Additional
purified water Qty. ___________L Water addition
time:_________ in Wet mixing time:
_________ min Total time __________
min Impeller Speed
(Slow/Fast)________ Chopper
Speed (Slow/Fast)______ |
|
|
Unload
the granules into FBD bowls with impeller
slow and chopper slow. |
|
Step.
No. |
Manufacturing
Instruction |
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|
6.4 |
Drying |
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|
Air
Dry the granules for 10 minutes. |
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|
Shaking of Bag & put out
the bowls and raking for 1 minutes |
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|
Drying
Instruction: Dry
the granules at 70°C ± 5°C inlet temperature till the outlet temperature
reached at 45°C ±5°C or the composite sample of dried granules meets the LOD
limit (NMT 2.0% ) of IPQC specs. The indicative parameter for drying process
end point is LOD limit achievement and outlet temperature of about 45°C ±5°C
in drying time of approximately 120 minutes including the raking time. Drying
follows step wise process in FBD. The drying process can be stopped in any
step if the LOD or appropriate outlet temperature is achieved. |
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|
Collect
the granules and check loss on drying. |
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|
LOD.
_________________________________%w/w (Limit NMT 2.0 % w/w) |
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|
|
Unload
the FBD bowl. |
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|
6.5 |
Milling & sizing |
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|
|
Sift
the dried granules through Vibro sifter fitted with 40# mesh. The over sized
granules retained on the 40# mesh should be passed through 8.0 mm screen. Now
pass the sifted granules form multi-mill
fitted with 1.5 mm screen with knife forward direction operated medium speed. |
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|
Mesh
40# |
Screen
1.5 mm |
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|
Before Use |
After Use |
Before Use |
After Use |
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|
Rusted : Yes / No |
Rusted : Yes / No |
Rusted : Yes / No |
Rusted : Yes / No |
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|
Broken : Yes / No |
Broken : Yes / No |
Broken : Yes / No |
Broken : Yes / No |
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Clean : Yes / No |
NA |
Clean : Yes / No |
NA |
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6.6 |
Blending &
Lubrication |
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|
|
Transfer
the milled and sized dried granules to blender and add pre-sifted blending
material and blend the materials for 45 minutes at __14__ RPM (to be
reported) Dried
granules after… (Milling & sizing )……………….....................Kg Aerosil
(COLLAIDAL SILICON DIOXIDE)_____0.375 Kg Cross
Povidone XL-10 USP28/NF23____0.800 Kg Sodium
Starch Glycolate____0.375 Kg Talc____2.000
Kg |
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|
Lubrication |
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|
Add
pre-sifted magnesium state in blender and blend the material for 5 minutes at
14 RPM (To be reported) Magnesium
Stearate 1.000 Kg |
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|
IPQA Shall collect
the sample and send it to QC for analysis |
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|
Unload
the material in HDPE container with double lined poly bag. |
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6.7
COMPRESSION:
D-Tooling,
Double Rotary compression machine.
Punch Description: 15.8 X 5.6 mm.
Upper Punch: 15.8 X 5.6 mm, elongated shape,
biconvex and break-line.
Lower Punch: 15.8 X 5.6 mm, elongated shape,
biconvex and plain.
6.8
STANDARD SPECIFICATIONS OF
COMPRESSED TABLATE:
|
Sr.
No. |
Parameters |
Requirement |
|
1. |
Description/ Appearance |
Orange
coloured, Elongated Shaped, Biconvex, Film coated tablets having scored line
on one side and plain other side. |
|
2. |
Punch Size |
15.8
X 5.6 mm ± 0.2 mm |
|
3. |
Weight
of 20 tablets |
17.000 ± 2.0% (16.66 gm to 17.34 gm) |
|
4. |
Avg. weight |
850 mg
± 5.00% (807.5 mg to 892.5 mg) |
|
5. |
Individual weight variation |
850 mg
± 5% |
|
6. |
Thickness |
5.6 mm ± 0.2 mm (5.4 mm to 5.8
mm) |
|
7. |
Hardness |
NLT 4.0 kg/cm2 |
|
8. |
Friability |
NMT 1.0% |
|
9. |
Disintegration Time |
NMT 15 minutes |
|
10. |
Machine Speed |
Optimum |
|
11. |
Temperature |
NMT
25±2 ºC |
|
12. |
RH |
NMT
45±5% |
6.9
Batch Reconciliation
|
|
Average weight of tablets
(A)=: mg |
|
|
Standard Yield (B) = Lac |
|
|
Total weight of compressed
tablets (C) =
Kg. |
|
|
C Quantity
of compressed tablet in Number (D)= ------------X 1000 X1000 = A |
|
|
No. of Tablets rejected during
Metal detection (X): Nos. |
|
|
No. of Tablets rejected during
Visual Inspection (Y): Nos. |
|
|
No. of tablet rejected (Z):=
(X+Y)
Nos. |
|
|
No. of tablet sampled Samples
(E)=
Nos. |
|
|
(D+E)-Z
Yield=------------------------
x 100=
(Yield NLT: 98.50%) Std. batch Size |
Note:-
·
Use
Metal detector during compression process.
·
Collect
the compressed tablets in HDPE plastic containers lined with double poly-bags.
·
Label
the all containers properly and maximum 20 Kg tablets can be kept in a
container.
7.0 COATING
PROCESS:
Equipment to be
used for coating: Auto-Coater,
Type
of Coating: Film
Coating.
7.1 Coating
Solution Preparation Procedure
Take
purified water 4.000 kg in a SS vessel. Stir with Propeller stirrer to form
vortex.
Add HPMC E15 CPS (Hydroxy Propyl Methyl Cellulose) 1.000 Kg and Colour
Titanium dioxide, Colour Lake Sunset Yellow, Talc to above vortex under
continuous stirring for 45 min. Stop stirring and Filter the solution through
(100#).
7.2 Process
Parameter:
Inlet temp: 60 ± 5°C
Outlet temp.: 50 ± 5°C
Bed temp.: 45 ± 5°C
Pan RPM: 2.0 to 6.0
Atomization Air: 2.0 to 3.5 Kg/cm2
Peristaltic pump RPM: 8 to 14
All
coating process parameter are interred related with each other, so can be
adjusting as per requirement.
7.3
STANDARD SPECIFICATION OF COATED
TABLET:
|
Sr.
No. |
Parameters |
Requirement |
|
1. |
Description/ Appearance |
Orange
coloured, Elongated Shaped, Biconvex, Film coated tablets having scored line
on one side and plain other side. |
|
2. |
Weight
of 20 tablets |
17.000 ± 2.0% (16.66 gm to 17.34 gm) |
|
3. |
Avg. weight |
866 mg
± 5.00% (822.7 mg to 909.3 mg) |
|
4. |
Thickness |
5.80 mm ± 0.2 mm (5.60 mm to 6.00 mm) |
|
5. |
Wt. Build up |
1.5 to 2.0% w/w |
|
6. |
Disintegration Time |
NMT 30 minutes |
7.4 Send the coated tablet sample for
QC analysis with intimation.
8.0 BATCH
RECONCILITAION:
Calculate the % yield at various
stages. In case actual yield is out of limit, Officer / Executive /Manager of
production/Packing department shall be fill the deviation form and get it
approved by QA Head
|
Sr. No. |
Stage of
Operation |
Input (kg) A |
Actual Wt. (kg) B |
Percentage (%)
B/A x 100 |
Permissible Yield
(%) |
|
|
Lower |
Higher |
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|
1. |
Dried granules |
|
|
|
|
|
|
2. |
Lubricated granules |
|
|
|
|
|
|
3. |
Compressed tablets |
|
|
|
|
|
|
Actual Wt. of the stage (B)
output / Actual Wt. of stage input (A) x 100 =(B/A)
/ 100= Y% %
ACCOUNTABILITY = to be established % |
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9.0 REVISION
HISTORY:
|
Effective Date |
Version No. |
Change History |
Change Control No. |
|
15/01/2018 |
00 |
New
Document |
NA |
END OF
DOCUMENT
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