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 Equipment Installation

Qualification (PQ) Validation 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)

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 TYPICAL PROCESS FLOW OF
SOLID DOSAGE FORM

Addition of Preble
bending Granulating Drying
raw material -fluid bed
-high speed - high speed
-active dryer
mixer mixer
excipients -tray dryer
granulator granulator

Addition of
Tableting Blending raw material Sizing
-high speed -v-blender -lubricant -mill/sieve
rotary -disintegrants

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TYPICAL VARIABLE OF DRYING PROCESS

Control variable Measured responses

Initial temperature Density

Load size Yield
Drying temperature Moisture content
program
Air flow program
Drying time
Cooling time
8
 VALIDATION
OF
FLUID BED DRYER

9
FLUID BED DRYER

10
FBD CONTROL PARAMETERS

Fixed Variable Response

(monitor) (Test)
Bowl change Inlet/exhaust air Particle size
Porosity of temperature distribution
filter bags Product temperature Densities
Bowl sieve Drying time Loss on drying
Air volume Assay
Humidity of incoming air
Humidity of exhaust air

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
12
 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.

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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.

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Validation
of
Tray dryer

28
TRAY DRYER

29
TRAY DRYER CONTROL PARAMETERS

Fixed Variable Response

(monitor) (Test)
Trays Inlet/exhaust air Particle size
temperature distribution
Product temperature Densities
Drying time Loss on drying
Air volume Assay
Humidity of incoming air
Humidity of exhaust air

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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