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DOCUMENT TITLE PROCESS VALIDATION REPORT

DOCUMENT NO. PRVR-TG-221003 PRODUCT CODE PR-20-22403

PRODUCT NAME LamaVet Tick Grease MANUFACTURER Adherechem (Pvt) Ltd

ISSUE NUMBER REVISION NUMBER 0

EFFECTIVE DATE

PROCESS VALIDATION REFERENCE DOCUMENT: VALIDATION

REPORT NO. PRVR-TG-221003 (Refer Module 3:

1. SUMMARY
The purpose of research was to study prospective validation of LamaVet Tick
Grease dosage formulation. Quality cannot be adequately
assured by in-process and finished inspections and testing but it
should be built in to the manufacturing process. These processes
should be controlled in order that the finished product meets all
quality specifications. Therefore, building of quality requires careful
attention to a number of factors, such as the selection of materials, product and process
design, control variables, in process control and finished product testing.

Three initial process validation batches of same size, same equipment,

method, material and validation criteria was taken. The critical process
parameters involved in heating, melting and blending stages were identified and
evaluated as per validation plan. Blending of the jelly was
evaluated for product homogeneity and blending process efficiency. The
temperature, rotor speed and duration of mixing affect the final jelly quality.
Therefore, based on results of process validation batch at each of the stages for the
specified parameters it was summarized and concluded that with the
prospective process validation for the LamaVet Tick Grease produces the
batches with no significant deviation and reported documented evidence, that
process can be effectively produce a product which complies with the present
specification and reproducible quality standards. In addition, the drug content of
jelly product was within the limits of 94% to 106%. All the in-process
variables and finished product characteristics were monitored; the statistical
analysis of data was carried out. The outcome indicated that data obtained by
process validation of three batches provides high degree of assurance that
manufacturing process of LamaVet Tick Grease produces product
meeting its predetermined specifications and quality attributes.

2. INTRODUCTION
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DOCUMENT TITLE PROCESS VALIDATION REPORT

DOCUMENT NO. PRVR-TG-221003 PRODUCT CODE PR-20-22403

PRODUCT NAME LamaVet Tick Grease MANUFACTURER Adherechem (Pvt) Ltd

ISSUE NUMBER REVISION NUMBER 0

EFFECTIVE DATE

The Quality System (QS) regulation defines process validation as establishing

by objective evidence that a process consistently produces a result or
product meeting its predetermined specifications. Process validation is a
key element in assuring that these principles and goals are met.

Validation is one of the important steps in achieving and maintaining

the quality of the final product. If each step of manufacturing process is
validated, we can be assured that the final product is of the best
quality. Validation of the individual steps of the processes is called
the process validation. Here this article concentrates to provide
assurance that the manufacturing procedure is suitable for intended purpose and
consistently meets predetermined specifications and quality attributes,
as per specified master formula record. It also provides documented evidence
for the operation sequence and schedule of
manufacturing process and to determine the critical
parameters and variables in the process of manufacturing of the wettable powder. It
gives a higher degree of assurance that the manufacturing process
consistently meet the pre-determined specifications and quality
products output can be used to increase productivity, its consistent quality
and decreasing the need for processing/market complaints.

3. MATERIALS AND METHODOLOGY

3.1 Validation Procedure:

 Three batches of 200kg batch size to be manufactured as described in the
batch manufacturing record. Current version of standard operating
procedures to be followed.
 Record the observations at mixing and milling stage in the below specified
data sheets.
 Carry out analysis after mixing.

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DOCUMENT TITLE PROCESS VALIDATION REPORT

DOCUMENT NO. PRVR-TG-221003 PRODUCT CODE PR-20-22403

PRODUCT NAME LamaVet Tick Grease MANUFACTURER Adherechem (Pvt) Ltd

ISSUE NUMBER REVISION NUMBER 0

EFFECTIVE DATE

3.2 Batches Studied for Process Validation:

PS-20-100-019 - First batch of LamaVet Tick Grease

PS-20-100-020 - First batch of LamaVet Tick Grease
PS-20-100-021 - First batch of LamaVet Tick Grease

3.3 Manufacturers:
Agricura (Pvt) Ltd

3.4 Label Claim:

Each unit contains:
 Deltamethrin, 0.02% (m/m)
 Chlorfenvinphos, 0.2% (m/m)
 High Boiling Tar Acid (HBTA) 1% (m/m)

3.5 Drug Substance Profiles:

(i) Chlorfenvinphos
(a) Description
Chlorfenvinphos is an
organophosphorus insecticide and acaricide used
in the control of flies, fleas, mites and moths in and around agricultural
buildings, pastures, and potato crops.
Chlorfenvinphos is also widely used
in external parasiticide
formulations for use on cattle, sheep, deer, goats, horses and dogs.
Technical chlorfenvinphos (comprised of the sum of
E- and Z-isomers) has a minimum
purity of 900 g/L. Typically, the ratio of isomers Z:E is
8.6:1 in the technical material, with both the cis and the trans isomers
having insecticidal activity. Whilst the potency of the
isomers varies from species to
species, the trans isomer is usually the more active one.
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DOCUMENT TITLE PROCESS VALIDATION REPORT

DOCUMENT NO. PRVR-TG-221003 PRODUCT CODE PR-20-22403

PRODUCT NAME LamaVet Tick Grease MANUFACTURER Adherechem (Pvt) Ltd

ISSUE NUMBER REVISION NUMBER 0

EFFECTIVE DATE

(b) Category: Antihelmintics

Broad spectrum contact, non-systemic
ectoparasiticide: insecticide, acaricide,
tickicide, louisicide, larvicide

(c) Chemical Name:

2-chloro-1-(2,4-dichlorophenyl)vinyl diethyl
phosphate

(d) Trade & Technical Products Names: Birlane, Dermaton,

Sapercon, Steladone, and Supona

(e) Physical & Chemical Properties

Chlorfenvinphos exists in two geometric
isomeric forms: alpha (=cis)
isomer and ß (=trans) isomer. In the ß (=trans) isomer
the vinyl
chlorine atom is opposite to the substituted aryl ring.

The technical material contains not less than 92% of

total isomers; a
typical sample contains 9.7% w/w cis-and 83.8%
trans-isomer. The alpha isomer
is less insecticidally active than the ß isomer.

Physical state: Liquid at 25°C

Colour: Amber
Odour: Mild chemical
Melting point: -19 to -23°C
Boiling point: 167-170°C at 0.5 mm Hg
Vapour pressure: 1.7×10 mm Hg at 25°C
Specific gravity: 1.36 at 15.6°/15.6°C
Refractive index: n25°C : 1.5272
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DOCUMENT TITLE PROCESS VALIDATION REPORT

DOCUMENT NO. PRVR-TG-221003 PRODUCT CODE PR-20-22403

PRODUCT NAME LamaVet Tick Grease MANUFACTURER Adherechem (Pvt) Ltd

ISSUE NUMBER REVISION NUMBER 0

EFFECTIVE DATE

(ii) Deltamethrin
(a) Description
Deltamethrin is a synthetic pyrethroid
insecticide that is largely used in
structural pest control. A potent insecticide, effective by contact and
ingestion against a wide range of pests. Crop
protection uses include: Coleoptera,
Heteroptera, Homoptera, Lepidoptera and Thysanoptera in
cereals, citrus, cotton, grapes, maize, oilseed rape, soya beans, top fruit
and vegetables. It controls Acrididae, and is
recommended against locusts. Soil
surface sprays control Noctuidae. It is used against indoor
crawling and flying insects, and pests of stored grain and timber. Dip
or spray, and pour-on applications give good
control of Muscidae, Tabanidae,
Ixodidae and other Acari on cattle, sheep and pigs, etc.

(b) Category: Antihelmintics

 neurotoxin
 Deltamethrin is effective against insects via ingestion and direct
contact.
 Pyrethroids, in general, interfere with normal production and
conduction of nerve signals in the nervous system. Pyrethroids act
on nerve membranes by delaying the closing of the activation gate
for the sodium ion channel.

(c) Chemical Name:

(S)-α-cyano-3-phenoxybenzyl (1R,3R)-3-
(2,2-
dibromovinyl)-2,2-dimethylcyclopropane
carboxylate

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DOCUMENT TITLE PROCESS VALIDATION REPORT

DOCUMENT NO. PRVR-TG-221003 PRODUCT CODE PR-20-22403

PRODUCT NAME LamaVet Tick Grease MANUFACTURER Adherechem (Pvt) Ltd

ISSUE NUMBER REVISION NUMBER 0

EFFECTIVE DATE

(d) Trade & Technical Products Names: Butox, Butoflin, Cislin,

Crackdown, Decis and K-Othrine.

(e) Physical & Chemical Properties

Technical grade deltamethrin is an odourless
white powder with a melting point
of 98 - 101 °C and contains more than 98% of the
material. The vapour pressure is 2.0 x 10-6 Pa at 25 °C and it is
practically non-volatile. It is
insoluble in water, but soluble in organic
solvents, such as acetone, cyclohexanone, and xylene. It is stable to
light, heat, and air, but unstable in alkaline media.

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4- Finished Product Specification & Finished Product Analysis and Acceptance Criteria for LamaVet Tick Grease:

Standard (e.g. Ph.Int., BP, USP, House) Professed

Specification Reference Number And Version PS-20-22403
Test Acceptance criteria Acceptance criteria Analytical procedure
(release) (shelf-life) (type/source/version)
Description Jelly, free from invisible impurities Jelly, free from invisible Visual
impurities
Assay Deltamethrin 0.020 – 0.032% (m/m) 94.0-106% of labelled amount 333/WP/M/3, CIPAC Handbook L, p.45, 2006
of Deltamethrin
Chlorfenvinphos 0.210 – 0.320% (m/m) 94.0-106% of labelled amount CIPAC Method 88/1/M/1.3; 1A p. 1131)
of Chlorfenvinphos
Colour Light blue Light blue Visual
Odour Characteristic Characteristic Visual
Drop Point 35 – 45oC 35 – 45oC ASTM D-127
Melting Point 55-65 oC 55-65 oC ASTM D-127
Cone Penetration, 25 oC 160-180 160-180 ASTM D-937

Table 1: Product Specifications & Acceptance Criteria

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5. Raw Materials and Formulation

Following raw materials are used in the manufacturing of sucralfate oral suspension. All the
raw materials were tested in the quality control department and individual certificate of analysis is
generated and it assures that all the materials will complies with specifications.

Component and quality Function Strength (label claim) Batch Size

standard (and grade, if  Deltamethrin, 200kg
applicable) 0.02% (m/m)
 Chlorfenvinphos,
0.2% (m/m)
 High Boiling Tar
Acid (HBTA) 1%
(m/m)
Quant. per Unit, kg %
Deltamethrin Tech. BP, 98% Insecticide API 0.1020 0.041
Chlorfenvinphos Tech., 92% Insecticide API 1.0870 0.435
High Boiling Tar Acid Antiseptic 5.0000 2.000
White Oil Diluent 50.0000 20.000
Petroleum Jelly, BP Carrier 443.8060 177.522
Blue Dye, BP Colour 0.0050 0.002

Total 200.00 100.0000

Table 2: Raw Material & Formulation For 200kg Batch

Figure 1: Manufacturing Process of LamaVet Tick Grease

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6. MANUFACTURING PROCESS

6.1 Narrative description of the Manufacturing Process

(i) Measure Petroleum Jelly into mixing tank.

(ii) Heat to 70oC.
(iii) Slowly mix in tar acid until dissolved.
(iv) Mix in Deltamethrin and Chlorfenvinphos.
(v) Stop heating and allow the solution to cool to about 45oC.
(vi) Mix in Tar Acid.
(vii) Add White Oil and Blue Dye and mix until homogeneous.
(viii) Let cool and take 500ml sample for analysis.

All the APIs along with the excipients were mixed in the SS manufacturing tank and after mixing the
suspension is transferred into #60 mesh in order to ϐilter the suspension. After ϐiltration decartoning,
washing and drying of empty PET bottles were done and the ϐilling and sealing operation were
performed. The steps in the manufacturing are shown in Figure 1 and packing is shown in Figure 2.

Packaging Process LamaVet Tick Grease

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6.2 Details of Equipment’s Used in The Manufacturing of LamaVet

Tick Grease

a) Stainless steel mixing tank

b) Capacity: 500 Litre
c) Structure: Double layer
d) Heating Mode: Electricity heating
e) Agitator Type: High speed mixer
f) Electricals: 24kw, 36rpm, electric heating
g) Sample thief
h) Dropping Point Tester

Details of sampling plan in process validation of sucralfate oral suspension

The process of mixing shall be evaluated for homogeneity of the solution through the sampling of
mixed materials from 5 locations (T1, T2 from Top Layer & M1, M2 from Middle layer & B from
Bottom Layer) after 10 minutes, 15 minutes and after 20 minutes of mixing. Sample shall be collected
from different locations using suitable sampler to conduct Description, pH, identiϐication, Weight/ml
& Assay of the Bulk Solution. The process of ϐiltration shall be evaluated by taking samples from 10,
15- and 20- min intervals and after ϐilling the ϐilled bottles were collected at initial middle and ϐinal
stage of the ϐilling and sealing process.

Process Validation Parameters:

Sl No. Parameters Source

1 Appearance
2 Colour
3 Odour
4 Uniformity of Dosage form End Product Testing
5 Drop Point
6 % Assay
7 11 Final Mixing
8 Appearance
9 % Assay
10 Filling In-process Testing
11 Filled Volume
12 Sealed Jars
13 Leak Test

Table 1: Process Control Parameters

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PROCESS OBJECTIVE VARIABLE TEST (RESPONSE)

(MONITOR)
Jelly Preparation To ensure a specified Temperature, Load, Appearance, Assay,
jelly with specified Mixing time, Mixing Colour, Drop Point
drop point and % Speed
assay (specified % of
labelled amount)
Filling To ensure uniformity Filling Ratio Fill volume, % Assay
in filled volume and %
assay

RESULTS AND DISCUSSION

The samples were collected and tested and all the equipment’s used in the manufacturing of sucralfate
oral suspension were qualified.

The critical process variables were tested for the manufacturing of sucralfate oral suspension and
results were shown in theTable 1. All the process parameters were performed and the results were
shown in the Table 2. Sampling locations depicted in Table 3. Environmental monitoring of
manufacturing area was done and the results were shown in the Table 4. Yield statement of bulk
suspension is given in Table 5. The bottle washing details were given in Table 6. Empty bottle
physical appearance test is done and it is free from ϐibred and coloured particles. The parameters at
the ϐilling and sealing operation were determined and results are shown in Table 7. Process veritable
results were shown in Table 8. In-process product analysis during ϐilling and sealing operation were
determined and results were shown in Table 9. Environmental monitoring of ϐilling and sealing area
is monitored and results were given inTable 10. Finished product analysis of sucralfate oral
suspension results were shown in Table 11. Yield statement for ϐinished product is shown in Table
12.

The process validation was started at the qualification of equipment all the equipment was
qualified at the time of process validation. Environmental condition monitoring of
manufacturing area is critical process parameter for process validation. In environmental
monitoring critical parameter like, temperature, relative humidity, and differential pressure,
viable or non-viable particles are generally monitored. The maximum and minimum
temperature was found to be 22.44ºC and 19.21ºC respectively in different processing area.
The maximum and minimum relative humidity% was found 27.50% and 18.23%
respectively in different processing area. The maximum and minimum differential pressure
was found to be 3.4 mm of WC and 1.8 mm of WC respectively depends on different
processing area. The viable particles were not found during observation. The maximum non
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viable particles of ≥0.5µ were found to be 536 and 1645 per m3 respectively in sterile filling
area and area adjacent to sterile area. Similarly, the maximum non viable particles of ≥5.0µ
were found to be 5 and 329 per m3 respectively in sterile filling area and area adjacent to
sterile area. The visible and non visible particulate matter was checked during vial washing,
sterilization and filling stages, the particulate matter was found to be as per acceptance
criteria. During vial filling and stoppering the weight variation and content uniformity of
dosage unit was also calculated / checked. The result was found under acceptance criteria.

Sealing integrity test was performed after vial sealing with the help of sealing integrity test
apparatus no defects was observed in this test. Analytical test and sterility test of finished
product was performed by quality control and microbiology department both test were
complies. All about the calculation the batch yield of three consecutive batches were found
to be 95.14%, 95.67% and 95.53% respectively.

So the data of all three batches were complying with its acceptance criteria. Hence the
product can be successfully manufactured at the commercial scale and the sterile
manufacturing process is validated.

Where the result obtained show significant deviations from those expected, the regulatory
authorities need to be informed immediately. In such cases corrective action should be
proposed and any changes proposed in the manufacturing process should receive prior
regulatory approval by way of variation.

The blending was performed and the samples at the designated locations were drawn after 20, 40 and
60minutes of blending for determination of the API content. The content, appearance, specific
gravity, values and emulsifiability meet the acceptance criteria at the all the 3 blending intervals.
From the analytical results it is clear that the API distribution pattern in the blend is almost
homogeneous.

The distribution of the Deltamethrin and Chlorfenvinphos is well acceptable as per the
predetermined specification at all the intervals of blending as shown by the samples analysed, after
60 minutes results show more closer homogeneity of API distribution with other excipient of
blend.

Critical Process Acceptance Criteria Observation Result

Variable
Capacity 500 Litre 500 Litre Complies
Mixing speed 50RPM 50RPM Complies
Mixing time To be recorded 60 minutes Complies
Process time To be recorded 60 minutes Complies

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Critical Process Variables for The Production of Bulk Suspension

Sr. No. Test After 20 min After 40 min After 60 min

1 Description Complies Complies Complies

Process Parameter Test Results

Sr. No. Batch No. API Content, % 40 minutes 60 minutes

m/m
1 PS-20-100- Deltamethrin 0.021 0.024
019 Chlorfenvinphos 0.195 0.251
Tar Acid 0.96 1.04
2 PS-20-100- Deltamethrin 0.020 0.026
020 Chlorfenvinphos 0.25 0.246
Tar Acid 0.87 1.09
3 PS-20-100- Deltamethrin 0.019 0.024
021 Chlorfenvinphos 0.210 0.265
Tar Acid 0.93 1.03

Assay Results After 40 and 60 minutes

Process Step Equipment Critical Process Acceptance Result

Variable Criteria
Filling Filling machine Process time, To be recorded 6.5 hours
Machine speed, 10 to 20 BPM 15 BPM
Average fill
weight, NLT 500g 502g
Uniformity of fill Min.: 490g
weight Max.: 510g

Process Variable Results for Packaging

Sr. No. Test Acceptance Criteria Results

1 Appearance Jelly, free from invisible impurities Complies
2 Assay Deltamethrin: 0.020 – 0.032% (m/m) 0.024
Chlorfenvinphos: 0.210 – 0.320% 0.251
(m/m)
Tar Acid: 0.95-1.05 (m/m) 1.04
3 Colour Pale Blue Complies
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4 Odour Characteristic Complies

5 Drop Point 35-45 oC 38 oC

Finished Product Analysis: Batch No. PS-20-100-019

Sr. No. Test Acceptance Criteria Results

1 Appearance Jelly, free from invisible impurities Complies
2 Assay Deltamethrin: 0.020 – 0.032% (m/m) 0.026
Chlorfenvinphos: 0.210 – 0.320% 0.246
(m/m)
Tar Acid: 0.95-1.05 (m/m) 1.09
3 Colour Pale Blue Complies
4 Odour Characteristic Complies
5 Drop Point 35-45 oC 38 oC

Finished Product Analysis: Batch No. PS-20-100-020

Sr. No. Test Acceptance Criteria Results

1 Appearance Jelly, free from invisible impurities Complies
2 Assay Deltamethrin: 0.020 – 0.032% (m/m) 0.024
Chlorfenvinphos: 0.210 – 0.320% 0.265
(m/m)
Tar Acid: 0.95-1.05 (m/m) 1.03
3 Colour Pale Blue Complies
4 Odour Characteristic Complies
5 Drop Point 35-45 oC 38 oC

Finished Product Analysis: Batch No. PS-20-100-019

Sr. No. Batch No. Step Theoretical Yield, % Actual, Yield, %

1 PS-20-100-019 Blending 100% 99.86
2 PS-20-100-020 99.82
3 PS-20-100-021 99.88

Yield Statement of Finished Products Finished Product Analysis

CONCLUSIONS
The equipment used in the manufacturing of the LamaVet Tick Grease were checked for their
Installation, Operation and Performance Qualification and verified. Key variables in the preparation
of sucralfate oral suspension were selected and all the critical process variables are were found within
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the limits. The process condition at each unit operation was established. The process parameters in the
preparation of LamaVet Tick Grease were meeting its predetermined specifications. Hence, the
process validation of LamaVet Tick Grease was performed and the process meets its predetermined
specifications and hence the product is maintaining the good quality from the first step to the final
step of validation.

Conflict of Interest
The authors declare that they have no conflict of interest for this study.

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Maryland. pages 2–3. United States Food and Drug Administration, USA.

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