PRELIM: 4 Flashcards
Validation means _________ or ___________.
rectification or confirmation.
Types of Validation (4)
Analytical method validation
Equipment validation
Cleaning validation
Process validation
Methods should be validated when: (3)
- When they are to be established for routine use.
- When the method is to be changed due to change in conditions.
- Whenever the equivalence between new method and the standard are demonstrated
used for a specific test is suitable for which it is to be carried out.
Analytical method validation
is to provide a high level of documented evidence that the equipment and the process confirm to a standard
Equipment validation
can be defined as a procedure that demonstrates that a process under standard conditions is capable of consistently producing a product that meets the established product specifications.
Validation
The _________ of an analytical method refers to the closeness of values obtained from a series of tests.
precision
The ________ of an analytical method refers to the closeness of agreement between the observed value and the value which is either conventionally a true one or reference one.
accuracy
___________ is established when the same sample is estimated repeatedly by the same analyst using same analytical method within the same laboratory using same instrument and performed within a short period of time.
Repeatability
When the test is repeated on different days by different persons or using different instruments within the same laboratory, the variation is expressed in terms of ____________ ___________.
intermediate precision
is the interval between the upper and lower concentration (amounts) of analyte in the sample
Range
a measure of its capacity to remain unaffected by small, but deliberate variations in method parameters and provides an indication of its reliability during normal usage
Robustness
are two important concepts in analytical chemistry used to assess the sensitivity of an analytical method. They both help to determine the lowest concentration of an analyte that can be reliably detected and quantified, respectively.
Limit of Detection (LOD) and Limit of Quantification (LOQ)
Types of equipment validation: (4)
Installation Qualification (IQ)
Operational Qualification (OQ)
Design Qualification (DQ)
Performance Qualification (PQ)
is the lowest concentration of an analyte that can be reliably distinguished from the background noise with a certain level of confidence at which the presence of the
analyte can be detected, but not necessarily quantified accurately
LOD (limit of detection)
is the lowest concentration of an analyte that can be reliably detected and quantified with acceptable accuracy and precision. It ensures that the measured concentration falls within an acceptable range of uncertainty, allowing for accurate quantification
LOQ (limit of quantification)
ensures that there is no cross contamination in a multi-product manufacturing plant and also prevents microbial contamination
Cleaning validation
Types of contamination to be considered in cleaning validation (4)
- Cross contamination
- Microbial contamination
- Contamination by cleaning or sanitizing agent
- Contamination by other agents
It is done to provide a high degree of assurance that the equipment functions as intended.
Operational Qualification (OQ)
It ensures that all major processing and packing equipment and ancillary systems are in conformity with installation specification, equipment manuals ,schematics
Installation Qualification (IQ)
It is a documented review of the design, at an appropriate stage in the project, for conformance to operational and regulatory
expectation.
Design Qualification (DQ)
It is a documented verification that all aspects of a facility, utility or equipment perform as intended in meeting pre- determined acceptance criteria.
Performance Qualification (PQ)
Important Installation Qualification (IQ) considerations:
- Calibration,preventive maintenance
- Safety features
- Software documentation
- Equipment design features
Important Operational Qualification (OQ) considerations:
- Software procedures
- Raw material specification
- Process operation procedures
- Material handling requirements
Important Design Qualification (DQ) considerations are:
- GMP’s and regulatory requirements
- Reliability and efficiency
- Safety and environment impact
- Construct ability and installation of equipment
Important Performance Qualification (PQ) considerations:
- Actual product & process parameters
- Acceptability of the product
- Process repeatability
- Long term process stability
is the means of ensuring & providing documentary evidence that processes are capable of repeatedly & reliably producing a finished product of the required quality.
Process validation
Types of Process validation: (4)
- Prospective validation
- Concurrent validation
- Retrospective validation
- Process re-validation
It is a process where current production batches are used to monitor processing parameters.
Concurrent validation
It is conducted prior to the distribution of either a new product or a product made under a modified production process, where the modifications are significant & may affect the product characteristics.
Prospective validation
This validation may be used for older products which were not validated by the fabricator at the time that they were first marketed.
Retrospective validation
Initial stages of formulation development & process development
Prospective validation
Process with low production volume per batch and market demand
Concurrent validation
is required when there is a change in any of the critical process parameters, formulation, primary packaging components, major equipment or premises
Process re-validation
is only acceptable for well established
detailed processes and will be inappropriate when there have recent changes in the formulation of the products, operating procedures, equipment & facility.
Retrospective validation
Changes in raw materials ( physical properties such as density, viscosity, particle size distribution)
Process re-validation
The number of batches produced are limited
Concurrent validation
Designing of batch records
Prospective validation
Changes in the plant/facility
Process re-validation
Number of lots released per year
Retrospective validation
A previous validated process is being transferred to a third party contract manufacturer or to another site
Concurrent validation
Master manufacturing/packaging documents
Retrospective validation
