A
Seminar
on
VALIDATION
OF
FLUID BED AND
TRAY DRYER
1
CONTENT:
Why to validate?
 Parts of Equipment Validation
 Who should do Equipment Validation?
 Equipment qualification
 Typical process flow of solid dosage form
 Validation of fluid bed dryer
 Validation of Tray dryer

2
WHY TO VALIDATE?
Equipment validation is Vital for
• Safety
• Fewer interruptions of work
• Lower repair costs
• Elimination of premature replacement
• Less standby equipment
• Identification of high maintenance cost
• Reduction of variation in results
• Greater confidence in the reliability of results
3
PARTS OF EQUIPMENT VALIDATION
Design
Qualification (DQ)
Performance
Qualification (PQ)
Equipment
Validation
Installation
Qualification (IQ)
Operational
Qualification (OQ)
4
WHO SHOULD DO EQUIPMENT VALIDATION?
THE VENDOR OR THE USER?
The user has the ultimate responsibility for
equipment qualification.
 DQ should always be done by the user.
 While IQ for a small and low cost instrument is
usually done by the user, and
IQ for large, complex and high cost instruments
should be done by the vendor.
 OQ can be done by either the user or the vendor.
 PQ should always be done by the user

5
EQUIPMENT QUALIFICATION
Equipment qualification / validation includes
following things :
 Design qualification (DQ)
 Installation qualification (IQ)
 Operational qualification (OQ)
 Performance qualification (PQ)

6
TYPICAL PROCESS FLOW OF
SOLID DOSAGE FORM
Addition of
raw material
-active
excipients
Tableting
-high speed
rotary
Preble
bending
-high speed
mixer
granulator
Granulating
- high speed
mixer
granulator
Blending
-v-blender
Addition of
raw material
-lubricant
-disintegrants
Drying
-fluid bed
dryer
-tray dryer
Sizing
-mill/sieve
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TYPICAL VARIABLE OF DRYING PROCESS
Control variable
Measured responses
Initial temperature
Load size
Drying temperature
program
Air flow program
Drying time
Cooling time


Density
Yield
Moisture content
8
VALIDATION
OF
FLUID BED DRYER
9
FLUID BED DRYER
10
FBD CONTROL PARAMETERS
Fixed
Variable
(monitor)
Response
(Test)
Bowl change
Porosity of
filter bags
Bowl sieve
Inlet/exhaust air
temperature
Product temperature
Drying time
Air volume
Humidity of incoming air
Humidity of exhaust air
Particle size
distribution
Densities
Loss on drying
Assay
11
INSTALLATION QUALIFICATION(IQ)
 Installation
Procedure:
After checking all the specifications as mentioned
in the selection criteria, service engineer of the
manufacturer shall be called for commissioning, if
necessary.
 Authorized validation team shall carry out
installation.
 Department
Head of production, QA &
engineering shall evaluate installation report

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Conti…





Acceptance Criteria For Installation Qualification:
The equipment shall fulfill the selection criteria & its
purpose of Application.
Name of the manufacturer & supplier shall be as
mentioned in the Purchase order
The manufacturer/supplier shall provide complete
equipment manual along with the equipment
All recommended utilities of recommended
capacities are to be provided near the place of
installation
13
Conti…
Revalidation Criteria
 The equipment shall be revalidated if;
 Location of the equipment is changed.
 There is change of spare/parts,major maintenance
or breakdown that have a direct effect on the
performance of the equipment

14
Conti…
Conclusion:
 The equipment shall be considered qualified for
installation provided it meets all the parameters
mentioned in the acceptance criteria.
 After receiving installation report, it shall be
evaluated
&
released
for
operational
qualification, provided installation report is
evaluated & the equipment is found meeting all
parameters of acceptance criteria

15
OPERATIONAL QUALIFICATION (OQ)
Training record
 Before initiating OQ ensure that SOP for
Cleaning and operation of FBD is available.

•
Purpose: To train the qualification team for
performing OQ
16
Conti…
Procedure
 Initiate the actual operation of the FBD to ensure
that machine is operating within specification.
 Check the OQ parameters against their
specifications.
 Observe the functioning of all controls available
on control panel
 Record the observation
 Perform and attach report of heat distribution
study as per ` Heat distribution study procedure’

17
Conti…
Acceptance criteria (Heat Distribution Study:)
 Temperature difference between all thermocouples
and set temperature should not differ by more than
± 5 °C.
 All operating inputs provided on the equipment
when tested shall-successfully comply
-meet tolerance limit
 The equipment should successfully perform when
operated as per SOP

18
Conti…
Critical gauges/indicators provided on the
equipment---calibrated
 The equipment when operated shall not
- produce abnormal sound
- show any discrepancy in its smooth operation.

19
Conti…
Revalidation Criteria:
 The equipment shall be revalidated if;
 Location of the equipment is changed.
 There is change of spare/ parts, major maintenance
or breakdown that have a direct effect on the
performance of the equipment
 Critical gauges shall be replaced or corrected
 At normal revalidation schedule.

20
PERFORMANCE QUALIFICATION(PQ)
To check Heat Distribution by placing 10
thermocouples in geometric pattern with the FBD
Shell and empty Product Container without any
load to ensure heat distribution in the drying
chamber
 Heat distribution study will be performed at 65 ±
5°C for two hour after achieving the temperature
on the controlling sensors to ensure proper heat
distribution.

21
Conti…
Procedure
 After completion of OQ initiate the PQ of FBD.
 The effectiveness of drying will be qualified by
determining reduction of % moisture content in
drying process.
 3 batches/ lots of any product will be taken for PQ
of FBD.
 At least 2.0 gm of sample is sampled for % MC
check from the top, middle and bottom trays and
will be reported

22
Conti…
In case of any deviation inform to department
head for necessary action
 Document the deviation details
 Deviation is acceptable or not will be decided
-if yes
-if not

23
Conti…
Acceptance criteria
 The reduction in moisture content after drying
should be as per the specification in the BMR
 % RSD of LOD should not be more than 6 %
 The equipment should produce intended outputs
with respect to quality & quantity consistently

24
Conti…
Revalidation Criteria:
 The equipment shall be revalidated if;
 Location of the equipment is changed.
 There
is change of spare/ parts, major
maintenance or breakdown that have a direct
effect on the performance of the equipment
 At normal revalidation schedule.

25
PROCEDURE FOR DRYING EFFICACY
STUDY IN FLUIDIZED BED DRYER:
Ensure the cleaning of machine
 Load the wet mass in the FBD product container
 Set the process time & outlet temperature and run
the FBD.
 After completion of drying take out FBD bowl and
collect the sample
 At least 2.0 gm of sample is sampled for % MC
check from the top, middle and bottom trays and
will be reported

26
Conti…
Sampling Procedure:
 Ware nose mask, hand gloves before sampling.
 Label the sample bag with details as Product
name, stage, date, time and sign
 Collect app. 2.0 gms of dried material composite
sample in poly bag as per location shown
 Record the details of analysis.

27
Validation
of
Tray dryer
28
TRAY DRYER
29
TRAY DRYER CONTROL PARAMETERS
Fixed
Variable
(monitor)
Response
(Test)
Trays
Inlet/exhaust air
temperature
Product temperature
Drying time
Air volume
Humidity of incoming air
Humidity of exhaust air
Particle size
distribution
Densities
Loss on drying
Assay
30
INSTALLATION QUALIFICATION(IQ)
Procedure:
 Selection criteria shall be defined and based on
specific function to be carried out by the machine
& its efficiency.
 Requirement of accessories shall be decided &
listed out.
 Supplier or manufacturer selection

31
Conti…
Purchase Details:
 The purchase order no. & date shall be checked
 The accessories & their spare parts if any shall be
checked as per purchase order
 The delivery period shall be as per purchase order
 Supplier or manufacturer name & address shall be
checked
 Any deviation observed should be informed to the
supplier or manufacturer

32
Conti…
Details of the Equipment
 Equipment name, make & model no. shall be
noted down
 In-house identification no. shall be allocated
 Location for installation shall be decided
 Utilities required shall be listed down

33
Conti…
Installation Procedure:
 After checking all the specifications as mentioned
in the selection criteria, service engineer of the
manufacturer shall be called for commissioning, if
necessary.
 Authorized validation team shall carry out
installation
 Department Head of production, QA &
engineering shall evaluate installation report

34
Conti…
Acceptance Criteria For IQ
 Fulfill the selection criteria & its purpose of
Application
 The equipment shall be as per purchase order
 Accessories received shall be as per purchase order
 Should meet pre-selected design parameters
 Manufacturer/supplier shall provide complete
equipment manual
 Material of construction shall be as per purchase
order

35
OPERATIONAL QUALIFICATION (OQ)
Training record
 Before initiating OQ ensure that SOP for
Cleaning and operation of Tray dryer is available.


Purpose: To train the qualification team for
performing OQ
36
Conti…
Procedure
 Initiate the actual operation of the TD to ensure
that machine is operating within specification.
 Check the OQ parameters against their
specifications.
 Observe the functioning of all controls available
on control panel
 Record the observation

37
Conti…





Acceptance criteria
All operating inputs provided on the equipment when
tested shall-successfully comply
-meet tolerance limit
The equipment should successfully perform when
operated as per SOP
Critical gauges/indicators provided on the equipment--calibrated
The equipment when operated shall not
- produce abnormal sound
- show any discrepancy in its smooth operation.
38
PERFORMANCE QUALIFICATION(PQ)
To check Heat Distribution by placing 10
thermocouples in geometric pattern with the TD
Shell and empty Product Container without any
load to ensure heat distribution in the drying
chamber
 Heat distribution study will be performed at +45
°C and +105°C for one hour after achieving the
temperature on the controlling sensors to ensure
proper heat distribution.

39
Conti…
Procedure
 After completion of OQ initiate the PQ of TD
 The effectiveness of drying will be qualified by
determining reduction of % moisture content in
drying process.
 3 batches/ lots of any product will be taken for
PQ of TD
 At least 2.0 gm of sample is sampled for % MC
check from the top, middle and bottom trays and
will be reported

40
41
Conti…
In case of any deviation inform to department
head for necessary action
 Document the deviation details
 Deviation is acceptable or not will be decided
-if yes
-if not

42
Conti…
Acceptance criteria
 Temperature difference between all thermocouples
and set temperature should not differ by more than
 5 °C.
 The reduction in moisture content after drying
should be as per the specification in the BMR
 % RSD of LOD should not be more than 6 %
 The equipment should produce intended outputs
with respect to quality & quantity consistently

43
REFERENCES
Berry I.R., and Nash R.A., ”Pharmaceutical
Process validation” second edition, revised and
expanded; Marcel Dekker series; 83-110.
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SEMINAR OPEN FOR DISCUSSION
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