This document discusses the qualification of dissolution test apparatus and validation of utility systems. It covers the installation qualification, operational qualification, and performance qualification of dissolution test apparatus. This includes procedures, acceptance criteria, and maintenance schedules for qualifying the apparatus. It also summarizes validation test functions and acceptance criteria for key utility systems like plant steam, pure steam, water for injection, and emergency power generators. The goal is to ensure dissolution testing provides reliable and reproducible results for assessing drug release and bioavailability.

1. Qualification of Dissolution Test
Apparatus and Validation of
Utility System
Presented by : Akshay G. Trivedi
Guided by : Dr. Pintu Prajapati
Enrollment No : 201804103910007
Department of Pharmaceutical Quality Assurance
Maliba Pharmacy College
Uka Tarsadia University

2. Qualification of Dissolution Test
Apparatus
 Contents :
 Introduction & Types
 Installation Qualification
 Operational Qualification
 Performance Qualification
 Maintenance Schedule
 Qualification Protocol
 References

3. Introduction and Types
 Dissolution:
 “The process by which a known amount of drug substance goes into solution
per unit of time under standardized conditions.”
 Dissolution testing is used as a qualitative tool to provide measurements of
the bioavailability of a drug as well as to demonstrate bioequivalence from
batch-to-batch.

4.  Introduction :
 The bioavailability and bioequivalence data obtained can be used to guide the
development of a new formulation and product development processes
toward product optimization, as well as to ensure continuing product quality
and performance of the manufacturing process.
 Requirement for regulatory approval for product marketing.
 Vital component of the overall quality control program.

5. Introduction and Types
Types of Dissolution Test Apparatus
 IP : Paddle, Basket
 BP : Basket, Paddle, Flow through cell
 USP : Basket, Paddle, Reciprocating cylinder, Flow through cell
Paddle over disc, Rotating cylinder, Reciprocating disc

6. Installation Qualification
 Procedure
 Acceptance Criteria
 Conclusion

7. Installation Qualification
 Procedure :
 Details of the Equipment
 Supplier or Manufacturer Name & Address
 Equipment Name, Make & Model No.
 In-house Equipment Code No.
 Location
 Utilities

8. Installation Qualification
 Installation Procedure :
 Site Inspection, Environmental Conditions and Prerequisite
 Parts Identification List
 Validation of Physical Parameter
 SOPs
 Computerized System

9. Installation Qualification
 Acceptance Criteria :
 Fulfill the Selection Criteria & its Purpose of Application
 Material of Construction and Name of the Manufacturer & Supplier shall be as
mentioned in the Purchase order
 Meet pre-selected Design Parameters
 Equipment Manual shall be provided
 Utilities of recommended capacities are to be provided

10. Installation Qualification
 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.

11. Operational Qualification
Procedure :
 Power ON Check
 Lift Movement Check
 Temperature Accuracy
 Accuracy of Shaft Rotation
 Control of Paddle Wobbling

12. Operational Qualification
 Control of Paddle Centering
 Control of Distance of Shaft to Side of Vessel
 For Automated Dissolution Systems :
 Software/Hardware Communication
 Operator Interface Functions
 Stress / Boundary / Challenge Testing

13. Operational Qualification
 Acceptance Criteria :
 All operating inputs provided on the equipment when tested shall successfully
comply to their intended use & meet tolerance limit given by the
manufacturer.
 Perform successfully when operated as per SOP.
 Critical indicators provided on the equipment are calibrated.
 Equipment when operated shall not produce any abnormal sound or show
any discrepancy in its smooth operation.

14. Operational Qualification
 Conclusion :
 The equipment shall be considered qualified for performance qualification
provided it meets the acceptance criteria of operational qualification.
 The operational test reports shall be evaluated & equipment shall be released
for carrying out the performance qualification.

15. Performance Qualification
 Procedure :
 Test must be conducted for each of the combinations of vessels and
apparatus.
 USP Calibrator Tablets are used:
Disintegrating Tablets (Prednisone)
Non-disintegrating Tablets (Salicylic Acid)

16. Performance Qualification
 Effectiveness of dissolution will be qualified by determining drug content in
the solution.
 For the comparison, solution of known concentration of USP Reference
Standard is used.
 Document the deviation details.

17. Performance Qualification
 Acceptance Criteria :
 The result of the suitability test should be as per USP specification.
 The equipment should work smoothly with minimum noise while operating.
 The equipment should produce intended outputs with respect to quality &
quantity consistently.

18. Performance Qualification
 Conclusion :
 The equipment shall be considered qualified for regular usage provided it
should meet the acceptance criteria of performance qualification.
 The performance test reports shall be evaluated & equipment shall be
released for Carrying out the routine process.

19. Maintenance Schedule
Frequency Procedure / Parameter
After Each Test Clean up the system
Weekly Inspect:
• Circulating Water Pump
• Bath Water
Monthly Replace Bath Water
Every 6 Months • Check Temperature Calibration
• Calibration of the system
• Inspect- Guide Rods & Spindle Bearings
Annually Inspect:
• Belts
• Idler Pulleys
Every 2 Years Replace the Belts

20. Qualification Protocol
Figure of Equipment :
Fig: Various Equipments used for Qualification

21. Figure of Equipment :
Fig: Temperature Probe – used for measuring
temperature in vessel and in bath
Figure of Equipment :

22. Fig: Tachometer- used for measuring rotation of shaft
Figure of Equipment :

23. Fig: Wobble Gauge (with Basket Rim) – used to check
wobbling of basket rim
Figure of Equipment :

24. Fig: Dissolution Test Apparatus Connected with various
Equipments used for Qualification
Figure of Equipment :

25. Validation of Utility System
 This study provides a summary of the key validation test functions and
acceptance criteria for each utility system. These are provided as a guideline
for those involved in the validation of any pharmaceutical.
 Approval of this master plan neither provides approval of these test functions
and acceptance criteria for does it limit the test functions and acceptance
criteria included in any protocol.
 final approval of test functions and acceptance criteria is made by approval of
the installation, operational, and where applicable, performance qualification
protocols.

26. Plant steam
 Test functions :
 Perform installation qualification of deionizer and distillation equipment,
holding tanks, clean steam generator, and distribution system.
 Complete and document all required pre-start-up maintenance procedures
(including cleaning).
 Perform general operational controls verification testing.
 Verify that the system has adequate steam capacity during peak hours of
operation. Confirm that the steam pressure in within 5 psi of the
recommended operating pressure.
 Record the range of all process or equipment parameters (set points,
pressure, etc). Test the water produced by the system to ensure adequate
conductivity.
 Check that the holding tank water quality does not change adversely during
storage in holding tanks.

27.  Acceptance criteria :
 The system is installed in accordance with design specifications, manufacturer
recommendations, and cGMPs. Instruments are calibrated, identified, and
entered into the calibration program.
 General controls and alarms operate in accordance with design specification.
 The system operates in accordance with design specifications throughout the
operating range or range of intended use.
 System regulators must operate within ± 2 psi of design level.
 The system capacity must be sufficient to operate all system at peak demand
periods.

28. Pure steam
 Test functions :
 Perform installation qualification.
 Perform general operational controls verification testing.
 Verify that clean steam is fed by a purified water system or WFI system.
 Operate the system per applicable SOPs. Perform sampling as per the
sampling procedure and schedule.
 Record the range of all process or equipment parameters (set points,
pressure, etc.) verified during operational and performance qualification
testing.

29.  Acceptance criteria :
 The system is installed in accordance with design specifications, manufacturer
recommendations, and cGMPs. Instruments are calibrated, identified, and
entered into the calibrated program.
 General controls and alarms operate in accordance with design specifications.
 Operate the system per applicable SOPs. Perform sampling over a 1- month
period as per the sampling procedure and schedule.
 Test samples for conformance to current USP water for injection monograph.

30. Water for injection
 Test functions :
 Perform installation qualification. Verify piping, fitting, proper dimensions,
Drawings, wiring, PC software, calibration, and quality of materials.
 Check flow rates, low volume of water supply, excessive pressure drop, and
temperature drop or increase beyond set level.
 Perform general operational controls verification testing. Operate system
throughout the range of intended use.
 System regulators must operate within ± 2 psi of design level.
 Record the range of all process or equipment parameters verified during
operational and performance qualification testing.

31.  Acceptance criteria :
 The system is installed in accordance with design specifications, manufacturer
recommendations, and cGMPs. Instrument are calibrated, identified, and
entered into the calibration program.
 General controls and alarms operate in accordance with design specifications.
 All samples must meet the following criteria :
 Bacteriological purity. All samples must contain no more than 10 cfu/100 ml.
 Physical properties. The temperature of the hot water for injection must be
greater than 80°C.

32. Emergency power(standby generator)
 Test functions :
 Perform installation qualification.
 Perform general operational controls verification testing.
 Operate system throughout the range of opening design specifications or
range of intended use.
 Verify that the emergency power generation system has adequate power to
provide all intended users.
 Record the range of all process or equipment parameters verified during
operational and performance qualifications testing.

33.  Acceptance criteria :
 The system is installed in accordance with design specifications, manufacturer
recommendations, and cGMPs. Instruments are calibrated, identified, and
entered into the calibration program.
 General controls and alarms operate in accordance with design specifications.
 All intended users must operate under normal power source interruption
conditions.

34. References
 Frost S; “Introduction to the Validation of a Dissolution Apparatus”;
Dissolution Technologies; February 2004; 19-21.
 Sigvardson K; “Laboratory Equipment Qualification”; Pharmaceutical
Technologies; October 2011; 102-108.
 United States Pharmacopeial Convention, Inc; United States Pharmacopeia 26;
Rockville, Maryland: United States Pharmacopeial Convention, Inc; 2003.
 United state pharmacopoeia- 2014.