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WORLD JOURNAL OF PHARMACY AND PHARMACEUTICAL SCIENCES

P.Ramasubramaniyan et al.

World Journal of Pharmacy and Pharmaceutical Sciences

Volume 2, Issue 6, 5412-5418.

Research Article

ISSN 2278 4357

EQUIPMENT QUALIFICATION AND VALIDATION OF TABLET


COMPRESSION MACHINE
P.Ramasubramaniyan*, N.Sharanya, Palanichamy.S, T.Srinag, P.Pavani, Solairaj.P
Department of Pharmaceutics, Sankaralingam Bhuvaneswari College of Pharmacy, Sivakasi,
Tamil Nadu, India.

Article Received on
16 August 2013,

ABSTRACT

Revised on 15 Sept 2013,


Accepted on 05 November
2013

undertaken to demonstrate the intended use and performance of the

Qualification an ideal step for equipment validation is the action

utilities and equipment. The individual steps of qualification such as


design, installation, operational and performance qualification were

*Correspondence for

done in order to qualify the equipment. Blue print of equipment

Author:

validation was also included. In this article the compression parameters

* Dr. P. Ramasubramaniyan,

such as compression force, turret rpm and feeder rpm were studied.

Professor, Department of

The process capability of the equipment was studied by observing the

Pharmaceutics, Sankaralingam

weight of 20 tablets, disintegration time, friability, individual weight

Bhuvaneswari College of

variation, thickness and hardness. These parameters were studied at

Pharmacy, Sivakasi, Tamil


Nadu, INDIA.
ramskit@yahoo.com

three different speeds and the best results were obtained at the
optimum speed (40 rpm).
KEYWORDS:

Qualification,

validation,

design,

installation,

operational, performance, compression


INTRODUCTION
Qualification: It refers to activities undertaken to demonstrate that utilities and equipment
are suitable for their intended use and perform properly. The individual qualification steps are
defined as follow:
Design Qualification (DQ): It is the documented verification that the proposed design of the
facilities, systems and equipment is suitable for the intended purpose.

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P.Ramasubramaniyan et al.

World Journal of Pharmacy and Pharmaceutical Sciences

Installation Qualification (IQ): It is documented evidence that the premises, supporting


utilities, the equipment have been built and installed in compliance with design
specifications.
Operational Qualification (OQ): In this phase the process parameters are challenged to
assure that product meets all defined requirements under all anticipated conditions of
manufacturing, i.e., worst case testing.
Performance Qualification (PQ): The performance qualification is carried out to establish
the performance and efficiency of the tablet machine during tablet compression operation.
The key objective of this phase is to demonstrate that the process will produce acceptable
product under normal operating conditions.
A Typical Validation Blueprint of Equipment Validation:
1. Installation qualification
Facilities
Utilities
Equipment
2. Operation qualification
Testing Protocols for Utilities and Equipment
3. Validation
Testing protocols for products and cleaning systems
4. Documentation
5. Validation of the QA testing laboratory
6. SOPs
7. Training of personnel
8. Organization charts, Schedule of events
The main aim and objective of this research is to qualify the equipment based on its
process capability by observing the compression parameters.
METHODOLOGY
Execution of Design Qualification

Documentation and verification of procedures required to fulfill the protocol.

Execution of protocol and data collection, interpretation and review of data for accuracy,
completeness and cGMP compliance.

Approval of original protocol formats, approval for the final summaries and system
qualification statement.

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P.Ramasubramaniyan et al.

World Journal of Pharmacy and Pharmaceutical Sciences

Execution of IQ, OQ and PQ:

It includes the development and approval of an IQ, OQ, PQ protocols followed by the

performance of IQ, OQ, PQ. The further step includes the workout and approval of IQ, OQ,
PQ reports.
Procedure Followed for Performance Qualification:

The blend/dummy material was unloaded into the hoppers on the both sides and the

compression machine was operated at low speed (20RPM) as per operating instructions. Then
the machine was set to run for 20 minutes continuously after adjusting the following
parameters.
1. Individual tablet weight variation
2. Weight of 20 tablets
3. Hardness
4. Thickness
5. Disintegration time, Friability

Then the experiment was repeated at both medium (40RPM) and high speed (60RPM)

with same set of parameters and the parameters were checked at different speeds (low,
medium and high rpm). The results were reported
.
Sampling Plan

Collect 100 tablets for every 05 minutes.

RESULTS & DISCUSSION


TABLE No. 1:
Speed: Medium (40rpm)
Feeder rpm: LHS: 52, RHS: 56
Turret rpm:40RPM
Compression Force (KN): LHS: Main:16.9, Pre:5.7 RHS: Main:17.1, Pre:6.2
S.
PARAMETER
ACCEPTANCE
TIME INTERVAL (LHS)
No.
CRITERIA
0 min 05
10
15
20 min
min
min
min
1
Weight of 20 tablets
21.28 2%
21.24
21.26 21.26
21.28 21.25
(20.85 21.71g)
2
Disintegration Time
NMT 20 min
10'52" 12'31" 09'59" 11'02" 12'15"
3
Friability
NMT 0.8% w/w
0.34
0.41
0.37
0.33
0.39
The compression parameters such as weight of 20 tablets, disintegration time, friability,
individual weight variation, thickness and hardness are taken in to consideration at slow

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P.Ramasubramaniyan et al.

World Journal of Pharmacy and Pharmaceutical Sciences

(20RPM), medium (40RPM) and high (60RPM) speeds of machine. The results shown here
are the one observed at medium speed (40RPM) which is found to be optimum.
TABLE No. 2
Speed: Medium (40rpm)
Feeder rpm: LHS: 52, RHS: 56
Turret rpm:40RPM
Compression Force (KN): LHS: Main:16.9, Pre:5.7 RHS: Main:17.1, Pre:6.2
S.
PARAMETER
ACCEPTANCE
TIME INTERVAL (RHS)
No.
CRITERIA
0 min 05
10
15
20 min
min
min
min
1
Weight of 20 tablets
21.28 2%
21.28
21.29 21.28
21.24 21.26
(20.85 21.71g)
2
Disintegration Time
NMT 20 min
11'31" 13'03" 10'31" 11'15" 12'52"
3
Friability
NMT 0.8% w/w
0.36
0.44
0.40
0.34
0.41
TABLE No. 3
Time / No. Individual Weight Variation of the tablet : 1.064 5.0% (1.011 1.117 g)
of Tablets Speed: 40rpm
1
2
3
4
5
6
7
8
9
10
0
LHS 1.061 1.060 1.057 1.067 1.070 1.059 1.059 1.062 1.059 1.059
min RHS 1.053 1.064 1.076 1.060 1.058 1.061 1.057 1.064 1.059 1.065
05
LHS 1.054 1.045 1.061 1.067 1.063 1.061 1.060 1.059 1.066 1.055
min RHS 1.063 1.067 1.070 1.059 1.072 1.071 1.075 1.065 1.051 1.055
10
LHS 1.057 1.066 1.053 1.059 1.053 1.071 1.069 1.050 1.070 1.059
min RHS 1.052 1.065 1.067 1.057 1.056 1.064 1.066 1.055 1.067 1.056
15
LHS 1.065 1.066 1.059 1.058 1.063 1.060 1.064 1.047 1.063 1.061
min RHS 1.054 1.064 1.063 1.058 1.055 1.063 1.059 1.057 1.075 1.059
20
LHS 1.042 1.049 1.056 1.056 1.060 1.051 1.064 1.056 1.059 1.056
min RHS 1.054 1.056 1.043 1.043 1.065 1.054 1.056 1.053 1.046 1.058
TABLE No. 4
Time / No.
of Tablets
0
LHS
min RHS
05
LHS
min RHS
10
LHS
min RHS
15
LHS
min RHS

Thickness: 7.1 0.3mm (6.8 7.4mm)


1
2
3
4
5
6.98
6.96
6.98
6.97
6.94
6.96
6.94
6.94
6.93
6.94
6.98
6.94
6.96
6.98
6.97
6.94
6.98
6.94
6.98
6.97
6.91
6.94
6.98
6.94
6.89
6.97
6.98
6.94
6.98
6.94
6.94
6.92
6.94
6.94
6.97
6.89
6.97
6.98
6.94
6.87

6
6.94
6.98
6.84
6.96
6.88
6.92
7.01
6.94

7
6.93
6.98
6.86
6.94
6.89
6.93
7.0
6.93

8
6.94
7.01
6.89
6.98
6.98
6.94
6.98
6.94

9
6.90
6.96
6.86
6.97
6.93
6.94
6.99
6.93

10
6.92
6.96
6.92
6.87
6.92
7.00
6.94
7.00

20
min

6.99
6.89

6.93
7.0

6.94
6.96

6.98
7.01

6.98
7.0

6.94
6.98

LHS
RHS

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6.89
6.96

6.94
6.98

6.95
6.94

6.98
6.89

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TABLE No. 5
Time / No. Hardness: 10.0 - 16.0 kp
of Tablets
1
2
3
4
12.8
14.0
14.6
0
LHS 13.6
min RHS 12.6
13.1
13.6
12.8

5
15.2
13.4

6
13.7
13.6

7
13.8
12.8

8
14.2
14.6

9
14.6
14.8

10
14.8
13.8

10
min

LHS
RHS
LHS
RHS

14.0
12.8
13.6
13.8

14.6
12.6
13.8
13.8

14.2
12.4
14.1
14.2

13.6
13.8
14.7
14.7

13.8
13.8
13.5
14.9

13.2
14.2
13.4
13.6

12.6
14.4
14.9
13.4

12.2
13.8
15.0
13.4

14.0
14.2
12.8
12.6

14.2
14.6
13.3
12.7

15
min
20
min

LHS
RHS
LHS
RHS

12.7
14.8
14.9
14.8

12.7
14.1
12.9
12.8

13.6
14.6
12.8
12.6

13.5
13.6
14.6
14.6

14.2
13.6
14.7
14.1

14.5
13.2
14.1
14.2

14.6
14.4
14.4
14.5

14.9
14.5
14.4
14.6

14.8
14.3
13.9
13.9

14.8
14.2
13.6
13.8

05
min

SUMMARY & CONCLUSION


The parameters studied under the compression process are such as compression force, turret
rpm and feeder rpm. These are set at three different speeds and analyzed on both sides to
assess the exact parameters.
Turret was set at the speed of 20rpm with Feeder at LHS as 32rpm, at RHS as 36rpm and
Compression Force (KN) Main at LHS as 17.0, at RHS as 16.1 and Pre at LHS as 5.7, at RHS
as 5.3.
Turret was set at the speed of 40rpm with Feeder at LHS as 52rpm, at RHS as 56rpm and
Compression Force (KN) Main at LHS as 16.9, at RHS as 17.1 and Pre at LHS as 5.7, at RHS
as 6.2.
Turret was set at the speed of 60rpm with Feeder at LHS as 70rpm, at RHS as 75rpm and
Compression Force (KN) Main at LHS as 15.8, at RHS as 16.3 and Pre at LHS as 5.6, at RHS
as 6.5.
The samples were collected from both the sides (LHS, RHS) to qualify the two press stations
and the observations made from the results were found to be in specified limits as per the IH
specifications.
From this we conclude that the equipment is successfully qualified and can be used for
production of further batches.

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World Journal of Pharmacy and Pharmaceutical Sciences

ACKNOWLEDGMENT
We express our sincere thanks to our Principal Dr.P.Solairaj and management of
Sankaralingam Bhuvaneswari College of Pharmacy, Sivakasi for providing us the required
facilities. We also like to thank all the members involved in this work for their immense
support and cooperation.
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World Journal of Pharmacy and Pharmaceutical Sciences

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