1. A Seminar on 1

2.  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

3. 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

4. Equipment Validation Equipment Validation Installation Qualification (IQ) Installation Qualification (IQ) Operational Qualification (OQ) Operational Qualification (OQ) Performance Qualification (PQ) Performance Qualification (PQ) Design Qualification (DQ) Design Qualification (DQ) 4

5.  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

6. EQUIPMENT QUALIFICATION  Equipment qualification / validation includes following things :  Design qualification (DQ)  Installation qualification (IQ)  Operational qualification (OQ)  Performance qualification (PQ) 6

7. Addition of raw material -active excipients Preble bending -high speed mixer granulator Granulating - high speed mixer granulator Drying -fluid bed dryer -tray dryer Tableting -high speed rotary Blending -v-blender Addition of raw material -lubricant -disintegrants Sizing -mill/sieve 7

8. Control variable Initial temperature Load size Drying temperature program Air flow program Drying time Cooling time Measured responses Density Yield Moisture content 8

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11. FixedVariable (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

12. 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

13.  Acceptance Criteria For Installation Qualification: The equipment shall fulfill the selection criteria & its purpose of Application.selection criteria 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

14.  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

15.  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

16. 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

17.  Procedure Initiate the actual operation of the FBD to ensure that machine is operating within specification. Check the OQ parameters against their specifications.OQ parameters 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’ Heat distribution study procedure 17

18.  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

19. 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

20.  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

21. 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

22.  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

23. 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

24.  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

25.  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

26. 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

27.  Sampling Procedure: 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

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30. FixedVariable (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

31. INSTALLATION QUALIFICATION(IQ)  Procedure: Selection criteria shall be defined and based on specific function to be carried out by the machine & its efficiency. Selection criteria Requirement of accessories shall be decided & listed out. Supplier or manufacturer selection 31

32.  Purchase Details: 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

33.  Details of the Equipment 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

34.  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.selection criteria Authorized validation team shall carry out installation Department Head of production, QA & engineering shall evaluate installation report 34

35.  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

36. 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

37.  Procedure Initiate the actual operation of the TD to ensure that machine is operating within specification. Check the OQ parameters against their specifications.OQ parameters Observe the functioning of all controls available on control panel Record the observation 37

38.  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

39. 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. Heat distribution study 39

40.  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

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42. 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

43.  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

44. Berry I.R., and Nash R.A., ”Pharmaceutical Process validation” second edition, revised and expanded; Marcel Dekker series; 83-110. 44

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