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A seminar on

Validation & Qualification of


Dry Powder Mixers, Fluid
Bed Dryer, Tray Dryer
By
ADITI ROY
MPH/10026/18
M.Pharm. (Sem - II)
Dept. of Pharmaceutical sciences & Technology

BIRLA INSTITUTE OF TECHNOLOGY


MESRA, RANCHI

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Contents
 Introduction
 Need of validation
 Powder mixers validation
 Validation of FBD
 FBD control parameters
 Validation of Tray dryer
 Tray dryer control parameters
 Acceptance criteria
 References

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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.

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Parts of Equipment Validation
Design
Design
Qualification
Qualification(DQ)
(DQ)

Performance
Performance Equipment
Equipment Installation
Installation
Qualification
Qualification (PQ)
(PQ) Validation Qualification
Qualification (IQ)
(IQ)
Validation

Operational
Operational
Qualification
Qualification(OQ) 
(OQ) 

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Validation of Dry Powder
Mixer

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Introduction
 Validation of Dry Powder
Mixers

It is defined as documented act


which provide the high degree of
the assurance that Powder Mixer
equipment actually leads to the
desired mixing or blending.

 Why it is essential ?
The mixing of the API and
excipients is the critical step in
the solid dosage form
preparations that affect the
content uniformity at great extent.

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Types of the powder blenders
V cone blenders

Ribbon blenders

Double cone blenders

Conical screw mixer

Tumble blender

Drum mixer
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Variable and monitering

Variables

Monitoring =Blend uniformity

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Installation Qualification (IQ)
Details of the Equipment
 Equipment name, made by & model No. shall be noted down.
 Location for the installation equipment shall be checked.
 Utilities required shall be listed down.
 Any deviation observed while following above procedure
should be informed for corrective action.

Installation Procedure:
 After checking all the specifications as mentioned in the
selection criteria, service engineer shall commission the
equipment.
 Authorized validation team shall carry out installation checks.

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Operational Qualification(OQ)
 After completions of successful installation qualification
initiate the actual operation of to ensure that machine is
operating within specification.

 Check the operation qualification parameters against


their specifications.

 Document the deviation details.

 The Quality head and the department head shall decide


whether deviation is acceptable or not.

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Performance Qualification (PQ)
 Load the materials to be mixed in the mixer.

 Startthe mixer and rotate it for the time as mentioned in


the BMR.

 After completion of mixing switch OFF the mixer and


separate out the drum.

 Collect the sample as per sampling procedure.

 Send the samples to Quality control dept. for content


uniformity, bulk density and sieve analysis.

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Revalidation Criteria
Location of the equipment is changed.

There is change of spare/ parts that have a


direct effect on the performance of the
equipment.

At normal revalidation schedule.

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Validation of fluid bed dryer

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FBD control parameters
Fixed Variable Response
(Monitor) (Test)
Bowl change Inlet/exhaust air Particle size
Porosity of filter temperature distribution
bags Product Densities
Bowl sieve temperature Loss on drying
Drying time Assay
Air volume
Humidity of
incoming air
Humidity of
exhaust air

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Working of FBD

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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.

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Operational Qualification (OQ)
 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’.

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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.
 Critical gauges/indicators provided on the equipment-
calibrated.

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Performance Qualification(PQ)
 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.
 In case of any deviation inform to department head for
necessary action.
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Conti…
Document the deviation details
 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.
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Validation of Tray dryer

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Tray Dryer control parameters
Fixed Variable Response
(monitor) (test)
Trays Inlet/exhaust air Particle size
temperature distribution
Product Densities
temperature Loss on drying
Drying time Assay
Air volume
Humidity of
incoming air
Humidity of
exhaust air

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Working of Tray Dryer

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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.
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.
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Operational Qualification (OQ)
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.

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Acceptance criteria-
 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.

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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.

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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.

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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.

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Bibliography
 http://www.validationonline.net/Mixer.html

(last accessed on 13.09.2018)


 www.askaboutvalidation.com

(last accessed on 10.03.2019)


 Sayed Imtiyaz Haider, ”pharmaceutical master validation
plan”, published by st. Luice press, vol-1 page no 125.
 Jozef H.Timmermans ,”A Report of the Product Quality
Research Institute Workshop on Blend Uniformity”
IJPSR, page-3 .
 Berry I.R., and Nash R.A., ”Pharmaceutical Process
validation” second edition, revised and expanded;
Marcel Dekker series; 83-110.
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Thank you

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