PROCESS VALIDATION REPORT

FOR VOSTEM® PLUS ORANGE TABLET EFFERVESCENT

Document No. : VAL-PV/PVR/MB/086R

Date : 23 March 2015

I. Product description
Name : VOSTEM® PLUS ORANGE TABLET EFFERVESCENT
Code : 17026
Dosage forms : Tablet Effervescent
Batch Size : 129.25 kg for 27,500 tablets (Production Scale)
Manufacturing site : PT. CAPRIFARMINDO LABORATORIES
(Pharmaceutical Plant)
Jl. Industri Cimareme No. 8 Block H
Kabupaten Bandung Barat - Indonesia

Compiled by:

II. Prepared by:

Function Name/Title Signature Date
Novita Purwanti /
Production
Process Validation Coordinator
Giva Olviana Yudhista./
Validation
Process Validation Engineer

III. Reviewed & Approved by:

Function Name/Title Signature Date
Mukti Wibowo /
Validation
Site Validation Coordinator
Herwanto /
R&D
Reviewed R&D Corp. General Manager
Quality Riny Yunita H. /
Control QC Manager
Plant Khairudin /
Manager Plant Manager
Lutfi Febrina /
QA Manager
QA Manager
Approved
Head of Sumardi /
Quality Head of Quality
I. Objective
 Manufacturing mixing process validation of VOSTEM® Plus Orange Tablet Effervescent
by conducting observation on mass appearance (color, odor), moisture content,
identification and assay.
 Tablet compressing and tubing process validation by conducting the appearance (form,
color, odor, sign), diameter, thickness, hardness, weight, weight variaton, identification,
desintegration time, microbial enumeration, assay, and leakage test.

II. Scope
 Validation is conducted on three batches of VOSTEM® Plus Orange Tablet Effervescent
that is manufactured in PT. Caprifarmindo Laboratories.
 Inspection is performed on preparation and raw material mixing process.
 Inspection on the compressing and tubing process.
 Validation process includes:
1. Production process
2. Sampling process
a. Mixing Process
The process sampling were taken after mixing process is completed. The samples
were taken in the final mixing from Top, Middle and Bottom. The samples were
used for appearance (color, odor), moisture content, identification and assay.
Sampling point is shown below:

B C

D
E

b. Compressing Process
Samples are taken from 10 sampling points during filling process. The samples
were taken for appearance (form, color, odor, mark), diameter, thickness,
identification, weight, weight variaton, speed of solubility, hardness, assay, and
leakage test.
3. Operational data recording
4. Critical parameters test
5. Data collecting
6. Evaluation and report
 This validation is dedicated for VOSTEM® Plus Orange Tablet effervescent that produced
in PT. CAPRIFARMINDO Laboratories, Cimareme, Padalarang.

III. Formula
Batch size : 129.25 kg for 27,500 tablets
Starting Material Weight Vendor of Materials
Glucosamine Hydrochloride 20.625 kg Yantai Dongcheng, China
Chondroitin Sulfate Sodium 14.414 kg Bioberica, Spain
Methyl Sulphonyl Methane 7.013 kg Bio-gen Extracts, India
Sodium Selenite 1% 0.180704 kg Dr. Paul Lohmann,
Germany
Zinc Sulfate Monohydrate 0.377232 kg Dr. Paul Lohmann,
Germany
Manganese Sulfate Monohydrate 0.084602 kg Merck, Germany
Magnesium Hydroxide 80% Granule 1.649660 kg Tomita Pharmaceutical,
Jepang
Ascorbic Acid 1.375 kg Jiangsu Jiangshan, China
Sodium Hydrogen Carbonate 27.50 kg Penrice, Australia
Citric Acid Anhydrous 27.50 kg S.A. Citrique Belge
Polyethylene Glycol 6000 6.875 kg Nippon Oil, Japan
Sucralose 2.145 kg JK Sucralose, China
Orange Durarome 2.06250 kg Firmenich, Indonesia
Isomaltulose 10.00 kg Beneo - Platinit GmbH,
Germany
Isomaltulose qs ad 129.25 kg 7.448302 kg Beneo - Platinit GmbH,
Germany

IV. Description on Process

See attachment 1 Schematic Flow Process Table and Attachment 2 Schematic Flow Process
Diagram.

V. Room Monitoring
See attachment 3 Room Monitoring Result.

VI. Equipment Qualification

See attachment 4 Equipment Qualification.

VII. Manufacturing Process

Stage 1. Mixture A Preparation
 1st Sieving
Sieve Glucosamine Hydrochloride (20.625 kg), Chondroitin Sulfaate Sodium (14.414 kg),
Methyl Sulphonyl Methane (7.013 kg), Magnesium Hydroxide 80% Granule (1.64966
kg), and Ascorbic Acid (1.375 kg) using Powder Siever Lou Soung mesh 20.

 1st Mixing
Mix manually materials from step 1st Sieving with Sodium salenite 1% (0.180704 kg),
Zinc Sulfate Monohydrate (0.377232 kg), Manganase Sulfate Monohydrate (0.084602
kg), and Isomaltulose (10.0 kg) in plastic bag 25 kg during 5 minutes until completely
homogeneous.
  2nd Sieving
Sieve materials from step 1st Mixing using Powder Siever Lou Soung Mesh 20 into
container I.

 3rd Sieving
Sieve Isomaltulose (7,448302 kg), Sodium Hydrogen Carbonate (27.5000 kg), Citric Acid
Anhydrous (27.5000 kg), Polyethylene Glycol 6000 (6.875000 kg), Sucralose (2.14500
kg), and Orang Durarome (2.062500 kg) using Powder Siever Lou Soung Mesh 12 into
container I. Move all of materials in Bohle.

 Final Mixing
Mix all of materials in Bohle with machine speed 6 rpm during 90 minutes.

Stage 3. Compressing Process

Compress the final mixing material using Manesty D4. Write down the process data in
attachment 5, Critical Parameter Result During Process.

Stage 4. Tubing Process

Fill the tablet of VOSTEM® Plus Orange Tablet effervescent into empty tube. Write down the
process data in attachment 5, Critical Parameter Result During Process.

VIII. Acceptance criteria

 Validation is considered to be accepted and valid if all the obtained evaluation result
complies with the compendia or internal specification.
 All evaluation parameters mentioned in the attachment is conducted.

IX. Evaluation Failure

If one or more obtained evaluation result does not comply with acceptance criteria, further
action should be proposed by the protocol makers to the production department and
validation executors and approved by the officers who have signed the protocol.

X. Revalidation Review
Revalidation is performed if there is a change of:
1. Formulation
2. Batch size (if more than 25% of previous batch)
3. Manufacturing process
4. Equipment
5. Primary Packaging Materials
 ATTACHMENT 1
SCHEMATIC FLOW PROCESS TABLE
IN MANUFACTURING OF VOSTEM® PLUS ORANGE
TABLET EFFERVESCENT (112.8 kg for 24,000 tablets)

Critical Analysis
Starting Material Mfg Step Equipment Testing Point
Parameter Method
 Glucosamine Weighing Electronic Quantity  Calibration N/A
Hydrochloride Process (1) Balance Accuracy: label/certificate
20.625 kg
Mettler  Balance checking
Toledo Calibration  The weighing
 Chondroitin Sulfate  Actual result
Sodium 14.414 kg Weight verification by
 Methyl Sulphonyl second person
Methane 7.013 kg
 Sodium Selenite 1%
0.180704 kg
 Zinc Sulfate
Monohydrate
0.377232 kg
 Manganese Sulfate
Monohydrate
0.084602 kg
 Magnesium
Hydroxide 80%
Granule
1.649660 kg
 Ascorbic Acid 1.375
kg
 Sodium Hydrogen
Carbonate 27.500 kg
 Citric Acid
Anhydrous
27.500 kg
 Polyethylene Glycol
6000 6.875 kg
 Sucralose 2.145 kg
 Orange Durarome
2.062500 kg
 Isomaltulose 10 kg
 Isomaltulose qs ad
129.25 kg
7.448302 kg
 Critical Analysis
Starting Material Mfg Step Equipment Testing Point
Parameter Method
 Glucosamine Sieving (2A) Powder Mesh 20 Homogeneity Visually
Hydrochloride Siever Lou
Soung
20.625 kg
 Chondroitin Sulfate
Sodium 14.414 kg
 Methyl Sulphonyl
Methane 7.013 kg
 Magnesium
Hydroxide 80%
Granule
1.649660 kg
 Ascorbic Acid 1.375
kg
 Sodium Selenite 1% Mixing and Mix 3 Minutes Homogeneity Visually
0.180704 kg Sieving (2B) Manually
 Zinc Sulfate
Monohydrate Powder Mesh 20
0.377232 kg Siever Lou
 Manganese Sulfate Soung
Monohydrate
0.084602 kg
 Isomaltulose 10 kg
 Isomaltulose qs ad Sieving (2C) Powder Mesh 12 Homogeneity Visually
129.25 kg 7.448302 Siever Lou
Soung
kg
 Sodium Hydrogen
Carbonate 27.500 kg
 Citric Acid
Anhydrous
27.500 kg
 Polyethylene Glycol
6000 6.875 kg
 Sucralose 2.145 kg
 Orange Durarome
2.062500 kg
 Sieved Mixing (3) BOHLE Speed Color Visual
Materials from step machine: 6 Moisture
rpm Moisture content determination
2A
Mixing time : balance
90 minutes Odor Organoleptic
 Critical Analysis
Starting Material Mfg Step Equipment Testing Point
Parameter Method
 Sieved Assay of
Materials from step - Glucosami
2B ne HCL HPLC
- Chondroiti
 Sieved n SO4
Materials from step
- Methylsulp
2C
hony-lmethane GC
(MSM)
- Zinc
- Manganase
- Magnesiu AAS
m
- Ascorbic
Titration
acid
 Mixed material Compressing Tablet Press Machine Appearance Visual
step 3 (4) Manesty D4 speed Diameter Visual
Compressing
Force Odor Organoleptic
Color Visually
Sign Visually
Weight of tablet Balance
Thickness Thickness tester
Weight variation Balance
Hardness Hardness tester
Disintegration Disintegration
time tester
Heavy metal AAS
Identification of
- Glucosamine HCl HPLC
- Chondroitin SO4
-Methylsulphonyl
methane (MSM) GC
- Selenium
- Zinc
Qualitative
- Manganese
method
- Magnesium
- Ascorbic acid
Assay of
- Glucosamine HCl HPLC
- Chondroitin SO4
-Methylsulphonyl GC
methane (MSM)
 Critical Analysis
Starting Material Mfg Step Equipment Testing Point
Parameter Method
- Zinc
- Manganese AAS
- Magnesium
- Ascorbic
Titration
acid

 Effervescent Tablet Tubbing and Selective Microbial Microbial Microbiological

from step 4 Capping (5) Media contaminant enumeration testing

 Tubed and capped Finished

effervescent tablet product
from step 5 testing Described in : SP-OJ-701, Rev.02
 ATTACHMENT 2
SCHEMATIC FLOW PROCESS DIAGRAM
 ATTACHMENT 3
ROOM MONITORING RESULT

BATCH 1 : PK9015

Relative Temperature Inspection

Room Note
Humidity 15-35% 18-26°C by/Date

Giva
Weighing 23.1 % 23.3°C N/A
03/10/2014

Relative Temperature Inspection

Room Note
Humidity 15-35% 18-26°C by/Date

Giva
Mixing 25.4 % 22.6°C N/A
09/10/2014
Relative Temperature Inspection
Room Note
Humidity 15-35% 18-26°C by/Date
Giva
Compressing 25.9 % 24.8°C N/A
09/10/2014
Relative Temperature Inspection
Room Note
Humidity 15-35% 18-26°C by/Date
Giva
Tubing 26.0 % 23.4°C N/A
09/10/2014

Dat
Prepared by : :
e
Dat
Checked by : :
e
BATCH 2 : PK9016

Relative Temperature Inspection

Room Note
Humidity 15-35% 18-26°C by/Date

Giva /
Weighing 22.4 22.1 N/A
08/10/2014

Relative Temperature Inspection

Room Note
Humidity 15-35% 18-26°C by/Date

Giva /
Mixing 26.5 22.5 N/A
09/10/2014
Relative Temperature Inspection
Room Note
Humidity 15-35% 18-26°C by/Date
Giva /
Compressing 26.2 23.1 N/A
09/10/2014
Relative Temperature Inspection
Room Note
Humidity 15-35% 18-26°C by/Date
Giva /
Tubing 23.4 23.0 N/A
09/10/2014

Dat
Prepared by : :
e
Dat
Checked by : :
e
BATCH 3 : PM8669

Relative Temperature Inspection

Room Note
Humidity 15-35% 18-26°C by/Date

Giva /
Weighing 21.4 23.1 N/A
09/12/2014

Relative Temperature Inspection

Room Note
Humidity 15-35% 18-26°C by/Date

Giva /
Mixing 21.7 26.3 N/A
09/12/2014
Relative Temperature Inspection
Room Note
Humidity 15-35% 18-26°C by/Date
Giva /
Compressing 26.3 21.7 N/A
09/12/2014
Relative Temperature Inspection
Room Note
Humidity 15-35% 18-26°C by/Date
Giva /
Tubing 25.3 23.6 N/A
09/12/2014

Dat
Prepared by : :
e
Dat
Checked by : :
e
 ATTACHMENT 4
CALIBRATION AND QUALIFICATION OF EQUIPMENTS

QUALIFIACTION OR CALIBRATION CHECK BY &

NO EQUIPMENTS BRAND & TYPE REMARKS
NUMBER DATE DATE
Electronic Balance METTLER TOLEDO – Giva
1 CLXWB046 04/08/2014 N/A
cap. 6 kg BBK422-6XS 09/12/2014
Electronic Balance Giva
2 METTLER TOLEDO – ID7 CLXWB047 04/08/2014 N/A
cap. 150 kg 09/12/2014
Electronic Balance METTLER TOLEDO – Giva
3 2948517 04.08.2014 N/A
cap. 150 kg IND690 03/10/2014
N/A N/A
VAL-EV/OQR/MB/192 01/02/12 Giva
4 Powder Sifter Lao Soung N/A
10/12/2014
N/A N/A
VAL-EV/IQR/MB/154 21/11/2008
Giva
5 Mixer Bohle VAL-EV/OQR/MB/154 26/11/2008 N/A
10/12/2014
VAL-EV/PQR/MB/154 24/06/14
VAL-EV/IQR/MB/045 Rev.01 10/09/2007
Giva
6 Tablet Press Manesty D4D VAL-EV/OQR/MB/045 Rev.01 13/09/2007 N/A
10/12/2014
VAL-EV/PQR/MB/045-R6 19/12/13

Prepared by : Date :
Checked by : Date :
 ATTACHMENT 5
CRITICAL PARAMETER RESULT DURING PROCESS

Acceptance Actual Actual Actual

Mfg. Stage Critical Parameter Pass/Fail
Criteria BN : PK9015 BN : PK9016 BN : PM8669
Mix until completely Completely Completely Completely Completely
Pass
Sieving I homogeneous homogeneous homogeneous homogeneous homogeneous
Mesh size Mesh 20 Mesh 20 Mesh 20 Mesh 20 Pass
Mixing time 5 minutes 5 minutes 5 minutes 5 minutes Pass
Mixing I Mix until completely Completely Completely Completely Completely
Pass
homogeneous homogeneous homogeneous homogeneous homogeneous
Sieving II Mesh size Mesh 20 Mesh 20 Mesh 20 Mesh 20 Pass
Sieving III Mesh Size Mesh 20 Mesh 20 Mesh 20 Mesh 20 Pass
Machine Speed 6 rpm 6 rpm 6 rpm 6 rpm Pass
Final Mixing
Time 90 minutes 90 minutes 90 minutes 90 minutes Pass
Machine speed As info 300 tab/minute 300 tab/minute 270 tab/minutes Pass
Compressing
Compression force As info 4 tons 4 tons 4 tons Pass
Tubing Tube Leakage No Leakage No Leakage No Leakage No Leakage Pass

Prepared by : Date :
Checked by : Date :

ATTACHMENT 6
 PROCESS VALIDATION RESULT
Results
Manufacturing Acceptance
Operation Critical Parameter BN : PK9015 BN : PK9016 BN : PM8669 Pass/
Stage Criteria
MD : 03/10/2014 MD : 08/10/2014 MD : 09/12/2014 Fail
Appearance : White with yellow White with White with White with
Pass
Color spot yellow spot yellow spot yellow spot
Odor Orange Orange Orange Orange
Loss on drying:
Top (A) 0.4 % 0.2 % 0.1 %
Top (B) 0.2 % 0.2 % 0.1 %
Middle (C) <1% 0.2 % 0.3 % 0.1 % Pass
Middle (D) 0.2 % 0.2 % 0.1 %
Bottom (E) 0.2 % 0.1 % 0.1 %
Bottom (F) 0.2 % 0.2 % 0.1 %
Assay of Glucosamine HCl
Mixing Process Mixing Top (A) 100.7 % 102.6 % 96.8 %
Top (B) 99.9 % 104.7 % 97.2 %
Middle (C) 95.0 % - 120.0 % 101.9 % 106.4 % 104.5% Pass
Middle (D) 104.0 % 104.1 % 97.3%
Bottom (E) 99.6 % 105.7 % 99.6 %
Bottom (F) 98.0 % 103.2 % 96.0 %
Assay of Chondroitin SO4
Top (A) 101.9 % 116.2 % 115.8 %
Top (B) 104.7 % 113.9 % 115.4 %
Middle (C) 95.0 % - 120.0 % 102.5 % 112.6 % 106.8 %
Pass
Middle (D) 101.1 % 112.6 % 105.4 %
Bottom (E) 105.9 % 106.9 % 102.5 %
Bottom (F) 103.4 % 106.8 % 110.1%
 Results
Manufacturing Acceptance
Operation Critical Parameter BN : PK9015 BN : PK9016 BN : PM8669 Pass/
Stage Criteria
MD : 03/10/2014 MD : 08/10/2014 MD : 09/12/2014 Fail
Appearance : White with yellow White with White with White with
Pass
Color spot yellow spot yellow spot yellow spot
Mixing Process Mixing Assay of Methylsulphonyl
methane (MSM)
Top (A) 97.2 % 103.6 % 104.0 %
Top (B) 95.8 % 103.6 % 100.8 %
95.0 % - 110.0 % Pass
Middle (C) 95.5 % 103.4 % 108.0 %
Mixing Process Mixing
Middle (D) 95.7 % 102.0 % 105.0 %
Bottom (E) 95.0 % 96.2 % 109.7 %
Bottom (F) 95.7 % 100.1 % 103.8 %
Assay of Zinc
Top (A) 104.0 % 106.5 % 106.8 %
Top (B) 104.2 % 105.1 % 109.3 %
Middle (C) 95.0 % - 125.0 % 100.7 % 102.8 % 109.3 % Pass
Middle (D) 101.4 % 103.2 % 109.2 %
Bottom (E) 104.2 % 101.3 % 114.0 %
Bottom (F) 105.1 % 105.0 % 109.9 %
Assay of Manganase 95.0 % - 125.0 % Pass
Top (A) 105.1 % 102.8 % 104.9 %
Top (B) 105.0 % 103.3 % 106.1 %
Middle (C) 103.1 % 101.2 % 103.7 %
Middle (D) 104.3 % 102.0 % 105.8 %
Bottom (E) 102.7 % 102.5 % 106.4 %
Bottom (F) 102.3 % 102.9 % 105.5 %
 Results
Manufacturing Acceptance
Operation Critical Parameter BN : PK9015 BN : PK9016 BN : PM8669 Pass/
Stage Criteria
MD : 03/10/2014 MD : 08/10/2014 MD : 09/12/2014 Fail
Appearance : White with yellow White with White with White with
Pass
Color spot yellow spot yellow spot yellow spot
Assay of Magnesium
Top (A) 103.3 % 101.9 % 107.0 %
Top (B) 101.0 % 101.8 % 109.6 %
Middle (C) 101.0 % 101.5 % 110.6 % Pass
95.0 % - 125.0 %
Middle (D) 101.4 % 100.7 % 112.9 %
Bottom (E) 101.6 % 101.2 % 109.7 %
Bottom (F) 101.2 % 101.4 % 113.0 %
Assay of Ascorbic acid
Top (A) 99.0 % 99.6 % 104.1 %
Mixing Process Mixing Top (B) 99.1 % 99.6 % 104.1 %
Miing Process Mixing Middle (C) 95.0 % - 150.0 % 99.5 % 103.2 % 102.5 % Pass
Middle (D) 99.5 % 103.2 % 102.5 %
Bottom (E) 99.1 % 99.6 % 102.5 %
Bottom (F) 99.0 % 99.6 % 102.5 %
Compressing Compressing Appearance:
Process - Form - Flat round tablet - Flat round tablet - Flat round tablet - Flat round tablet
- Color - White with yellow - White with - White with - White with
spot yellow spot yellow spot yellow spot Pass
- Sign - Plain - Plain - Plain - Plain
- Odor - Orange - Orange - Orange - Orange
Diameter 25 mm 25 mm 25 mm 25 mm Pass
Thickness 7.0 + 0.4 mm Pass
Beginning 6.9 mm 6.8 mm 6.7 mm
Middle 7.2 mm 6.6 mm 6.7 mm
End 6.9 mm 7.0 mm 6.7 mm
 Results
Manufacturing Acceptance
Operation Critical Parameter BN : PK9015 BN : PK9016 BN : PM8669 Pass/
Stage Criteria
MD : 03/10/2014 MD : 08/10/2014 MD : 09/12/2014 Fail
Appearance : White with yellow White with White with White with
Pass
Color spot yellow spot yellow spot yellow spot
Hardness
6 kg/cm2 7 kg/cm2 7 kg/cm2
Beginning 2
5 - 8 kg/cm 6 kg/cm2 6 kg/cm2 6 kg/cm2 Pass
Middle
Mixing Process Mixing 7 kg/cm2 6 kg/cm2 7 kg/cm2
End
Weight:
Beginning 4728 mg 4749 mg 4675mg
Middle 4,700 mg + 3% 4701 mg 4736 mg 4741 mg Pass
End 4741 mg 4715 mg 4684 mg
Compressing Compressing Not more than 2 Not more than 2 Not more than 2
Not more than 2 of
Process of individual of individual of individual
individual masses
masses tablets masses tablets masses tablets
tablets deviate from
deviate from the deviate from the deviate from the
the average mass by
Weight variation average mass by average mass by average mass by Pass
more than
more than 5.0 % more than 5.0 % more than 5.0 %
5.0 % and none
and none deviates and none deviates and none deviates
deviates by more
by more than 10.0 by more than 10.0 by more than 10.0
than 10.0 %.
%. %. %.
Identification Glucosamine
HCl Positive Positive Positive Positive Pass

Identification Chondroitin
Positive Positive Positive Positive Pass
SO4
Identification Positive Positive Positive Positive Pass
Methylsulphonyl-methane
(MSM)
 Results
Manufacturing Acceptance
Operation Critical Parameter BN : PK9015 BN : PK9016 BN : PM8669 Pass/
Stage Criteria
MD : 03/10/2014 MD : 08/10/2014 MD : 09/12/2014 Fail
Appearance : White with yellow White with White with White with
Pass
Color spot yellow spot yellow spot yellow spot
Identification Selenium Positive Positive Positive Positive Pass
Mixing Process Mixing
Identification Zinc Positive Positive Positive Positive Pass

Identification Manganese Positive Positive Positive Positive Pass

Identification Magnesium Positive Positive Positive Positive Pass

Identification Ascorbic acid Positive Positive Positive Positive Pass

Compressing Compressing Disintegration time
Process Beginning Not more than 5 04’06” 03’53” 03’59”
Middle 03’47” 03’43” 04’07” Pass
minutes
End 03’50” 03’49” 04’02”

Pb: Not more than Pb : Not more Pb : Not more Pb : Not more
10ppm than 10 ppm than 10 ppm than 10 ppm
As : Not more than As : Not more As : Not more As : Not more
Heavy metal Pass
5ppm than 5 ppm than 5 ppm than 5 ppm
Hg : Not more than Hg : Not more Hg : Not more Hg : Not more
0.5ppm than 0.5 ppm than 0.5 ppm than 0.5 ppm
Assay of Glucosamine HCl Pass
Beginning 95.0 % - 120.0 % 102.3 % 98.8 % 96.7 %
Middle 101.3 % 99.2 % 99.1 %
End 101.4 % 100.4 % 102.6 %
 Results
Manufacturing Acceptance
Operation Critical Parameter BN : PK9015 BN : PK9016 BN : PM8669 Pass/
Stage Criteria
MD : 03/10/2014 MD : 08/10/2014 MD : 09/12/2014 Fail
Appearance : White with yellow White with White with White with
Pass
Color spot yellow spot yellow spot yellow spot
Assay of :
Chondroitin SO4
Beginning 95.0 % - 120.0 % 103.9 % 106.8 % 106.5 % Pass
Middle 105.5 % 105.5 % 106.9 %
End 103.6 % 109.8 % 106.9 %
Mixing Process Mixing Assay of Zinc
Beginning 101.5 % 105,9 % 107.9 %
95.0 % - 125.0 % 115.6 % 103.0 % 108.5 % Pass
Middle
End 114.7 % 102.1 % 108.9 %

Assay of Manganese
Beginning 112.3 % 100.1 % 104.9 %
Middle 95.0 % - 125.0 % 115.4 % 106.0 % 108.0 % Pass
End 108.3 % 96.1 % 159.7 %
Compressing Compressing Assay of Methylsulphonyl-
Process methane (MSM)
Beginning 95.0 % - 110.0 % 98.5 % 96.5 % 100.6 % Pass
Middle 97.2 % 98.6 % 97.2 %
End 100.2 % 99.7 % 100.2 %
Assay of Magnesium 95.0 % - 125.0 % Pass
Beginning 104.5 % 105.5 % 109.3 %
Middle 100.5 % 106.2 % 106.5 %
End 99.2 % 108.9 % 106.1 %
 Results
Manufacturing Acceptance
Operation Critical Parameter BN : PK9015 BN : PK9016 BN : PM8669 Pass/
Stage Criteria
MD : 03/10/2014 MD : 08/10/2014 MD : 09/12/2014 Fail
Appearance : White with yellow White with White with White with
Pass
Color spot yellow spot yellow spot yellow spot
Assay of Ascorbic acid
99.6 % 100.5 % 99.1 %
Beginning
95.0 % - 150.0 % 98.2 % 101.7 % 101.5 % Pass
Middle
Mixing Process Mixing 98.2 % 100.0 % 101.7 %
End
- Total aerobic - Not detected - Not detected - Not detected
microbial count:
Not more than
1,000 cfu/gram
- Total combined - Not detected - Not detected - Not detected
Yeast and mold: not
more than 100
Tubing
Tube Filling Microbial enumeration cfu/gram Pass
Process
- Absence of - Negative - Negative - Negative
Salmonella spp,
Pseudomonas
aeruginosa,
Escherichia coli,
and Staphylococcus
aureus in 10 gram
Tubing
Tubing Tube Leakage No leakage No leakage No leakage No leakage Pass
Process
actual yield Theoretical yield Theoretical yield Theoretical yield
product is = 27,287 tablets = 27,287 tablets = 27,287 tablets
To be defined
counted and Actual yield = Actual yield = Actual yield =
Reconciliation %Yield (theoretical yield Pass
compare with 26,680 tablets 25.610 tablets 25,260 tablets
27,287 tablets)
theoretical % Yield = % Yield = % Yield =
yield 97.78 % 93.85 % 92.57 %
 Note : BN = Batch Number
MD = Manufacturing Date

Prepared by : Date :

Checked by : Date :